Recycling Monomer Patents (Class 526/68)
  • Patent number: 4360650
    Abstract: The invention concerns a process for the production of copolymers of propylene and but-1-ene which can be used for the production of hollow bodies or heat-sealable films and wherein the proportion by weight of units derived from but-1-ene is from 10 to 40% and wherein the proportion of isolated ethyl branches is at least equal to the square of the proportion of units derived from propylene contained in said polymers. The process is characterized in that a gaseous mixture of propylene and but-1-ene is brought into contact, in the absence of liquid diluent, with a catalytic system which is stereospecific in the polymerization of propylene alone.
    Type: Grant
    Filed: July 28, 1980
    Date of Patent: November 23, 1982
    Assignee: Naphtachimie Societe Anonyme
    Inventors: Bernard Desvignes, Jean C. Bailly, Pierre Mangin
  • Patent number: 4356339
    Abstract: A process for isolating and recovering butene-1 of high purity at a high yield is provided. The process comprises the steps of continuously passing a butane-butene fraction containing 0.1 to 15 wt % of isobutylene and 10 to 50 wt % of butene-1 through a first reactor packed with a strongly acidic cation exchange resin having an average particle size of from 0.2 to 10 mm at a temperature of from 30.degree. to 100.degree. C. and at a space velocity of liquid of from 0.1 to 50 hr.sup.-1 under a pressure of from 1 to 50 atm., dividing the output mixture flowing out of said first reactor into two flows at a division ratio in flow rate of 1.about.15:1, recirculating the first flow having the flow rate of 1.about.
    Type: Grant
    Filed: December 7, 1981
    Date of Patent: October 26, 1982
    Assignee: Nippon Oil Company, Limited
    Inventors: Masao Imaizumi, Tetsuya Takezono, Takaaki Amari, Yutaka Oguchi
  • Patent number: 4343926
    Abstract: The invention concerns a process for the production of elastomeric terpolymers of ethylene, propylene and dienes by the direct polymerization of the monomeric olefins in the gaseous state, in contact with a catalytic system comprising one or more solid compounds of titanium. The resulting terpolymers which are produced in the form of powders can be used without intermediate transformation for the production of molded or extruded articles.
    Type: Grant
    Filed: July 2, 1980
    Date of Patent: August 10, 1982
    Assignee: NAOHTACHIMIE Societe Anonyme
    Inventors: Francois Caumartin, Jean L. Vidal, Pierre Mangin
  • Patent number: 4342853
    Abstract: The energy efficiency of a high pressure, high temperature continuous process for the production of polyethylene is improved and residual gases are more completely removed from the product without detriment to product quality by employing an intermediate separator between the first and second separators. The intermediate separator is maintained at a pressure between about 10 and 70 bars, and the second separator is maintained at a pressure between about 1 and 1.5 bars.
    Type: Grant
    Filed: July 2, 1980
    Date of Patent: August 3, 1982
    Assignee: Societe Chimique des Charbonnages--CdF Chimie
    Inventors: Pierre Durand, Pierre Gloriod
  • Patent number: 4341891
    Abstract: An improved process for polymerizing olefins in the presence of a catalyst employing hydrogen for molecular weight control is disclosed wherein the improvement resides in adding additional hydrogen to the polymer slurry produced in the reactor system so as to eliminate or reduce the formation of gels in articles fabricated from the resultant polymer.
    Type: Grant
    Filed: December 29, 1980
    Date of Patent: July 27, 1982
    Assignee: The Dow Chemical Company
    Inventors: Donald E. Gessell, David M. Courter
  • Patent number: 4340701
    Abstract: A solid particulate olefin polymer containing monomer(s) dissolved therein is vigorously agitated mechanically to raise the temperature of the polymer to at least 90.degree. C. This vigorous agitation is effected in the absence of any purge gas and the unpolymerized olefin monomer desorbed from the polymer by the increase in temperature can readily be recovered and recycled to the polymerization vessel. The technique can form part of the work-up process in which the polymer is removed from the polymerization vessel and separated from unconverted monomer(s) prior to isolation. By this technique, propylene is removed from polypropylene without using a purge stream of nitrogen which makes recovery of the propylene difficult and expensive. The technique additionally heats up the polymer which can be advantageous for subsequent processing. Apparatus for effecting the process includes an agitation vessel which is connected, preferably through an intermediate separation vessel, to an olefin polymerization vessel.
    Type: Grant
    Filed: June 27, 1980
    Date of Patent: July 20, 1982
    Assignee: Imperial Chemical Industries Limited
    Inventors: Bruce A. E. Willmore, Jeffrey C. Greaves
  • Patent number: 4331791
    Abstract: Active polymerization catalyst is deactivated using a high molecular weight epoxide.
    Type: Grant
    Filed: August 15, 1980
    Date of Patent: May 25, 1982
    Assignee: Phillips Petroleum Company
    Inventors: Raymond G. Rohlfing, Melvin B. Welch, Richard E. Dietz
  • Patent number: 4330645
    Abstract: A process for the preparation of propylene homopolymers or copolymers by polymerizing the monomer or monomers in the gas phase in a centric stirred bed of finely divided polymer, with removal of the heat of polymerization by evaporative cooling, the temperature in the polymerization zone being regulated by measuring the temperature continuously and causing any change therein to trigger a change in the amount of liquid monomer, evaporating in the reaction zone, which is introduced per unit time, in which process(1) the radius and height of the centric stirred bed are in a particular ratio to one another, (2) the finely divided polymer in the centric stirred bed is caused to move upward in the peripheral zone of the bed and downward in the central zone of the bed, (3) the temperature in the polymerization zone is regulated by simultaneously measuring it at (3.1) one or more points of the inner part of the stirred bed and (3.
    Type: Grant
    Filed: March 31, 1981
    Date of Patent: May 18, 1982
    Assignee: BASF Aktiengesellschaft
    Inventors: Dirk Juza, Dieter Stein
  • Patent number: 4327208
    Abstract: A process for the production of polyamide-6 or corresponding copolyamides by hydrolytic polymerization wherein the low molecular weight secondary reaction products and the unreacted .epsilon.-caprolactam are separated off from the polyamide melt and directly condensed on the .epsilon.-caprolactam melt to be polymerized.
    Type: Grant
    Filed: July 9, 1980
    Date of Patent: April 27, 1982
    Assignee: Bayer Aktiengesellschaft
    Inventors: Gunter Lehr, Uwe Hucks, Hugo Vernaleken, Werner Nielinger, Erhard Tresper
  • Patent number: 4326048
    Abstract: In a gas phase olefin polymerization using a transition metal compound/aluminum alkyl catalyst system, polymerization can be terminated rapidly by injecting an amount of carbon oxide and then restarting efficiently by addition of an amount of aluminum alkyl.
    Type: Grant
    Filed: May 27, 1980
    Date of Patent: April 20, 1982
    Assignee: Standard Oil Company (Indiana)
    Inventors: Jack F. Stevens, Kwok-fu Lee, Philip M. Rose, David R. Kreider, Chi-Hung Lin
  • Patent number: 4310659
    Abstract: A two-stage hydrolysis process for polymerizing epsilon-caprolactam is disclosed comprising a first stage from a temperature of about 180.degree. C.-260.degree. C., a pressure of 20 to 150 psig, for a period of about 0.5 to 4 hours, then before equilibrium conditions are reached a second stage at a temperature of about 200.degree. C.-260.degree. C., a pressure of about 100-900 Torr for a period of about 2 to 15 hours, while continuously removing most of the water so that water is removed both during hydrolyzation and during the subsequent polycondensation, whereby the cyclic dimer content of the shaped polymer article is below 0.2 percent by weight.
    Type: Grant
    Filed: April 21, 1980
    Date of Patent: January 12, 1982
    Assignee: Allied Corporation
    Inventors: Samuel L. Yates, Charles J. Cole, Albert H. Wiesner, John W. Wagner
  • Patent number: 4301263
    Abstract: Disclosed is a pre-copolymer containing diallyl phthalate units and triallyl isocyanurate units.
    Type: Grant
    Filed: November 8, 1979
    Date of Patent: November 17, 1981
    Assignee: Nippon Kasei Chemical Co., Ltd.
    Inventors: Akinori Kameyama, Hiroyasu Saito, Jihei Inomata
  • Patent number: 4291132
    Abstract: A polymerization process is carried out in at least two zones, wherein in one zone polymerization is effected in the presence of a liquid phase which is at least one liquid olefine monomer and in a subsequent zone polymerization is effected by contacting the solid polymer with a gaseous olefine monomer, the product from the first zone being subjected to a concentration stage to remove some of the liquid olefine monomer before the concentrated polymer mixture is passed to the subsequent zone for polymerization with the gaseous olefine monomer. The monomer in each case may be the same, for example liquid propylene in one zone and gaseous propylene in a subsequent zone. The concentration stage may be effected using a hydrocyclone.
    Type: Grant
    Filed: August 22, 1979
    Date of Patent: September 22, 1981
    Assignee: Imperial Chemical Industries Limited
    Inventor: Michael L. Clifford
  • Patent number: 4282342
    Abstract: Terpolymers which have Fikentscher K-values of from 8 to 100 and comprise 50 mole percent of maleic anhydride units, from 35 to 45 mole percent of 2,4,4'-trimethylpent-1-ene units and from 5 to 15 mole percent of 2,4,4'-trimethylpent-2-ene units, and processes for their preparation by polymerizing 50 parts by weight of maleic anhydride, from 35 to 180 parts by weight of 2,4,4'-trimethylpent-1-ene and from 0.6 to 6 parts by weight of 2,4,4'-trimethylpent-2-ene per part by weight of 2,4,4'-trimethylpent-1-ene employed, in the presence of a free-radical initiator at from 60.degree. to 200.degree. C. and a pressure of from 1 to 20 bar, and separating the terpolymers from the unconverted monomers.
    Type: Grant
    Filed: September 6, 1979
    Date of Patent: August 4, 1981
    Assignee: BASF Aktiengesellschaft
    Inventors: Walter Denzinger, Claus Cordes
  • Patent number: 4282339
    Abstract: Ethylene is polymerized in a dual reactor system in which two reactors are connected in series with a heat exchanger, or intercooler, disposed therebetween. The reaction stream from the first reactor at elevated pressure and temperature is passed through the heat exchanger to effect cooling of the stream. Following passage through the heat exchanger, the pressure of the cooled reaction stream is reduced through a pressure let-down valve and the stream is thereafter introduced into the second reactor wherein further polymerization takes place. The reactors can both be of the autoclave type although one of the reactors can be of the tubular variety.
    Type: Grant
    Filed: December 17, 1979
    Date of Patent: August 4, 1981
    Assignee: National Distillers and Chemical Corp.
    Inventors: Charles R. Donaldson, Claude J. Stiles
  • Patent number: 4276398
    Abstract: In a method of recovering energy in the manufacture of high-pressure polyethylene from ethylene gas, the ethylene gas is compressed and partially converted into polyethylene in a reactor by polymerization. For the purpose of energy recovery, the polymer-gas mixture being discharged from the reactor is accelerated and decompressed in a nozzle system of an energy exchange unit, mixed and compressed with an almost polymer-free working stream. The polymer-free gas is then separated in a separation. The working stream flows through a decompression turbine, and is subsequently conveyed together with the polymer-gas mixture from the reactor into the nozzle system of the energy exchange unit and is continuously re-compressed in the energy exchange unit by the gas stream from the decompression turbine.
    Type: Grant
    Filed: September 18, 1979
    Date of Patent: June 30, 1981
    Inventor: Jacques G. Kempf
  • Patent number: 4269948
    Abstract: A process and apparatus for widening the molecular distribution of ethylene polymers produced at high pressure and at high temperature by polymerizing ethylene at a pressure between 600 and 3,000 bars and at a temperature between 160.degree. C. and 320.degree. C., in two reactors operating in parallel. In the first reactor, the reaction takes place in the presence of less than 0.1% of hydrogen for the purpose of producing a polymer of high molecular weight. In the second reactor, the reaction takes place in the presence of 0.2 to 5% of hydrogen for the purpose of fabricating a polymer of low molecular weight. The effluents from these two reactors are expanded and then moved to a set of two separators interconnected so as to efficiently mix the polymers produced in the two reactors by recycling the least possible amount of hydrogen into the supply circuit of the first reactor in such manner that the proportion of hydrogen in the first reactor remains less than 0.1% in moles.
    Type: Grant
    Filed: December 28, 1979
    Date of Patent: May 26, 1981
    Assignee: Societe Chimique des Charbonnages - CdF CHIMIE
    Inventor: Adrien Nicco
  • Patent number: 4260722
    Abstract: A process for the continuous production of an ethylene copolymer by compressing a mixture of ethylene and comonomer in a pre-compressor and a post-compressor, copolymerizing the mixture in a polymerization zone at a high temperature and high pressure, transferring the reaction mixture into a high pressure product isolation zone, from there into a low pressure product isolation zone and thereafter into a discharge extruder, and recycling the greater part of the unconverted monomer into the polymerization process and passing a small part of the unconverted gas into a low temperature isolation zone, in which process a small part of the gas recycled from the high pressure product isolation zone is passed into the low temperature isolation zone, which is preferably under a pressure of from 10 to 30 bar and at from -10.degree. to -50.degree. C., and all the gas taken off the low pressure product isolation zone is fed to the pre-compressor.
    Type: Grant
    Filed: November 27, 1979
    Date of Patent: April 7, 1981
    Assignee: BASF Aktiengesellschaft
    Inventors: Klaus Pfleger, Wieland Zacher, Klaus Boettcher, Ronald Skorczyk, Oskar Buechner, Franz G. Mietzner
  • Patent number: 4258158
    Abstract: A process for the continuous manufacture of ethylene polymers by catalytic polymerization of the monomer at an elevated temperature and elevated partial pressures of ethylene in a hydrocarbon which is a solvent for the monomer but a non-solvent for the polymer formed, the polymer being isolated by (a) discharging a mixture of polymer, hydrocarbon and monomer from the polymerization chamber, (b) bringing the mixture from stage (a) to a pressure and temperature such that a gaseous phase consisting of the monomer and hydrocarbon and a solid phase consisting of the polymer, with adhering hydrocarbon, is formed, and (c) flushing the solid phase from stage (b) with an inert gas, so as to form a solid phase consisting of polymer and a gaseous phase consisting of hydrocarbon and inert gas, wherein, as additional measures (d), the gaseous phase from stage (c) is brought to a pressure and temperature such that a gaseous phase consisting of inert gas and a liquid phase consisting of hydrocarbon are formed and (e) the li
    Type: Grant
    Filed: August 1, 1978
    Date of Patent: March 24, 1981
    Assignee: BASF Aktiengesellschaft
    Inventor: Erich Pfeiffer
  • Patent number: 4255542
    Abstract: A continuous low pressure gas phase process for the production of solid particulate polymers during an exothermic polymerization reaction in a uniform diameter vertical fluidized bed reactor system which comprises feeding a polymerization catalyst and a gaseous stream containing at least one polymerizable monomer to a fluidized bed of polymer particles and removing the exothermic heat of reaction by indirect cooling means in the reactor and removing dry particulate polymer. Also, apparatus for the polymerization process is described.
    Type: Grant
    Filed: November 30, 1978
    Date of Patent: March 10, 1981
    Assignee: Union Carbide Corporation
    Inventors: Gary L. Brown, David F. Warner, Jae H. Byon
  • Patent number: 4254246
    Abstract: A new process for use with continuously operated plants for the production of polyester polymers suitable for producing fibers, bottles and film, by reacting ethylene glycol and terephthalic acid in the presence of a catalyst so that the vapour by-products from the esterification, prepolycondensation and polycondensation stages are continuously rectified in two in-line columns yielding ethylene glycol of high purity (99.85%) which is returned to the process, waste water with 400 ppm ethylene glycol, and a heavy fraction containing oligomers, diethylene glycol, etc.Moreover, an improvement in the quality of the esterified product is attained as it contains less than 0.6% diethylene glycol without the use of diisopropylamine, a poisonous additive.
    Type: Grant
    Filed: March 26, 1979
    Date of Patent: March 3, 1981
    Assignee: Davy International AG
    Inventors: Ovidiu Dicoi, Hans Wewer
  • Patent number: 4243781
    Abstract: A process is disclosed for the preparation of styrene and acrylonitrile containing polymers wherein styrene and acrylonitrile in a predetermined ratio are introduced continuously into a recirculating polymerization zone of generally constant composition wherein a portion of the styrene and acrylonitrile is polymerized, material is removed from the polymerization zone at a rate equal to the addition of styrene and acrylonitrile on removal from the polymerization zone the monomer being separated from the resulting polymer, the improvement being maintaining a level of oxygen in the styrene and acrylonitrile not greater than 20 parts per million by weight based on the weight of the styrene and acrylonitrile. The resultant polymer is generally colorless.
    Type: Grant
    Filed: June 25, 1979
    Date of Patent: January 6, 1981
    Assignee: The Dow Chemical Company
    Inventor: Raymond W. Kent, Jr
  • Patent number: 4235983
    Abstract: Disclosed is a process for the polymerization of olefins wherein olefinic compounds are separated from mixtures containing them with resulting improved utilization of olefinic compounds. Such olefinic compounds are separated by use of membrane separation units and can be recycled to a polymerization zone.
    Type: Grant
    Filed: October 4, 1978
    Date of Patent: November 25, 1980
    Assignee: Standard Oil Company (Indiana)
    Inventors: Edward F. Steigelmann, Robert L. Yahnke, Alistair S. Couper, Chand Deepak
  • Patent number: 4217431
    Abstract: A continuous process for the manufacture of ethylene copolymers under high pressure and at high temperature in a polymerization zone, with transfer of the reaction mixture into a high pressure product isolation zone and from there into a low pressure product isolation zone, and recycling of the unconverted gas from the high pressure product isolation zone into the polymerization zone and from the low pressure product isolation zone into a low temperature separator, from where the comonomer separated off is recycled to the polymerization process, while the ethylene is discharged as off-gas. The gas taken off the low pressure product isolation zone is preferably compressed to from 10 to 20 bar and cooled to from -10.degree. to -30.degree. C. before it is fed into the low temperature separator. There is a substantial improvement in the efficiency of separating off the comonomer.
    Type: Grant
    Filed: January 10, 1979
    Date of Patent: August 12, 1980
    Assignee: BASF Aktiengesellschaft
    Inventors: Wieland Zacher, Klaus Pfleger, Klaus Boettcher, Ronald Skorczyk, Oskar Buechner
  • Patent number: 4215207
    Abstract: Process and device for cooling a mixture of polymer and monomer from a reactor in which ethylene is polymerized or copolymerized at a pressure greater than 1,000 bars between a pressure-reduction valve located downstream of the reactor and a medium pressure separator. The cooling is achieved by injecting monomer at a pressure below that of the separator using a device with a nozzle cross-section S.sub.1 through which the mixture from the reactor passes, a convergent mixing zone in which the mixture is mixed with the monomer injected, which is supplied at a flow rate q, and a diffuser of throat cross-section S.sub.3, which makes it possible to bring the mixture to the pressure of the separator. The dimensions of the device are such that the ratio Q/S.sub.1 is between 0.20 and 1.35 t/hr.mm2 and the ratio (q+Q/S.sub.3 is between 0.1 and 0.3 t/hr.mm2.
    Type: Grant
    Filed: June 3, 1976
    Date of Patent: July 29, 1980
    Assignee: Societe Chimique des Charbonnages-CdF Chimie
    Inventors: Pierre Durand, Pierre Charlon, Guy Jouffroy
  • Patent number: 4214063
    Abstract: A process for the polymerization of propylene or copolymers of propylene and other olefins is described wherein monomer is contacted with a catalyst in a reaction zone having both a liquid and a vapor phase followed by subjecting a polymer slurry withdrawn from the reaction zone to a degassing step and a wash step in a liquid phase wash zone using propylene as the wash liquid.
    Type: Grant
    Filed: January 11, 1979
    Date of Patent: July 22, 1980
    Assignee: Exxon Research & Engineering Co.
    Inventor: Edwin D. Luallin
  • Patent number: 4209599
    Abstract: A process for the continuous mass polymerization of olefinically unsaturated monomers in the presence of a polymerization initiator. The polymerization is carried out in one or more tubular reactors provided with internal static mixing elements. A portion of the reaction mass produced in the reactor is recirculated back to the reactor as feed.
    Type: Grant
    Filed: January 13, 1978
    Date of Patent: June 24, 1980
    Assignee: Synres International B.V.
    Inventors: John W. Brady, Pieter Eijsberg, Johan D. Logemann
  • Patent number: 4200714
    Abstract: Disclosed is a process for the removal of hydrogen from streams comprising olefinic compounds, such as streams from a polymerization reactor. At least a portion of the olefinic compounds are saturated with a substantial portion of the hydrogen present so as to effectively remove hydrogen from the stream. The saturated material formed can be then separated from unreacted olefinic compounds by use of a membrane separator and the olefinic compounds recycled to a polymerization zone for reaction.
    Type: Grant
    Filed: October 4, 1978
    Date of Patent: April 29, 1980
    Assignee: Standard Oil Company (Indiana)
    Inventors: John A. Mahoney, Clifton G. Frye
  • Patent number: 4200713
    Abstract: This invention relates to a process for producing a homopolymer or co-polymer of an aromatic vinyl monomer by anionically polymerizing a monomer mixture in the absence of oxygen in a tubular coil evaporator.
    Type: Grant
    Filed: May 22, 1978
    Date of Patent: April 29, 1980
    Assignee: Bayer Aktiengesellschaft
    Inventors: Frank Wingler, Clemens Casper, Lothar Liebig
  • Patent number: 4188470
    Abstract: Ethylene is polymerized in a gaseous phase and in contact with a Ziegler/Natta type solid catalyst capable of producing polyethylene in the form of granules having an easily controllable and homogeneous granulometric size, the polymerization being conducted in a tubular reactor in which the catalyst and the polymer granules which are formed are carried along the reactor by the flow of the gas.
    Type: Grant
    Filed: January 11, 1978
    Date of Patent: February 12, 1980
    Assignee: Montedison S.p.A.
    Inventors: Amilcare Collina, Arrigo Soverini, Francesco Rosati
  • Patent number: 4187278
    Abstract: A polymerization process is carried out in at least two zones, wherein in one zone polymerization is effected in the presence of a liquid phase which is at least one liquid olefine monomer and in a subsequent zone polymerization is effected by contacting the solid polymer with a gaseous olefine monomer, the product from the first zone being subjected to a concentration stage to remove some of the liquid olefine monomer before the concentrated polymer mixture is passed to the subsequent zone for polymerization with the gaseous olefine monomer. The monomer in each case may be the same, for example liquid propylene in one zone and gaseous propylene in a subsequent zone. The concentration stage may be effected using a hydrocyclone.
    Type: Grant
    Filed: April 12, 1976
    Date of Patent: February 5, 1980
    Assignee: Imperial Chemical Industries Limited
    Inventor: Michael L. Clifford
  • Patent number: 4184027
    Abstract: A system for controlling the percent of polymer in a reactor in a process in which the reactor effluent, comprising a mixture of polymer, unreacted materials and, possibly, by-products, goes through a separator to remove from such effluent unreacted materials and by-products. The system is especially useful with variable fillage, horizontal continuous stirred tank reactors.
    Type: Grant
    Filed: March 18, 1974
    Date of Patent: January 15, 1980
    Assignee: Monsanto Company
    Inventor: Byrd Hopkins
  • Patent number: 4182801
    Abstract: In the catalytic polymerization of olefins from liquid olefin monomer under positive pressure, the use of a fuel gas, required in any event for providing energy elsewhere in the system, as a regenerative drying gas to regenerate the beds of a molecular sieve dryer used to dry the liquid olefin to be polymerized.
    Type: Grant
    Filed: January 17, 1978
    Date of Patent: January 8, 1980
    Assignee: The Badger Company, Inc.
    Inventors: Constantine D. Miserlis, Peter J. Lewis
  • Patent number: 4181788
    Abstract: A process for the production of thermoplastically processible moulding materials based on vinyl polymers of high chemical and molecular uniformity and having residual monomer contents of less than 0.1 mol % which comprises the steps of:(i) mass homogeneous phase polymerization of at least one vinyl monomer in a stirred continuously charged tank reactor to a conversion of from 25 to 60 mol %;(ii) directly concentrating the syrup consisting of residual monomers and vinyl polymer dissolved therein obtained from step (i) in a spiral tube evaporator at a temperature of from 60.degree. to 250.degree. C. and at a pressure of 100 m bar to 35 bar to obtain a solid content of vinyl polymer of from 40 to 90 mol %;(iii) directly charging the concentrate obtained from step (ii) to the inlet zone of a screw evaporator which consists of at least two sequential zones in order to effect further concentration, in which a first zone at a pressure of from 10 to 300 m bar and at a temperature of from 100.degree. to 250.degree. C.
    Type: Grant
    Filed: May 23, 1978
    Date of Patent: January 1, 1980
    Assignee: Bayer Aktiengesellschaft
    Inventors: Frank Wingler, Lothar Liebig, Gerd Wassmuth, Martin Ullrich, Manfred Hederich
  • Patent number: 4180635
    Abstract: An economical and environmentally advantageous process for the continuous manufacture of unsaturated polyesters, wherein the vapors formed during the polycondensation are purified, in a two-part distillation column, to a degree where the residual content of organic starting materials is less than 1.5 percent by weight, based on the total weight of the effluent, and the unconverted starting materials are recycled to the process.
    Type: Grant
    Filed: March 29, 1978
    Date of Patent: December 25, 1979
    Assignee: BASF Aktiengesellschaft
    Inventors: Hermann Fischer, Richard Thoma, Hanshelmut Kaeppel, Ernst Kochendoerfer, Werner Lagaly
  • Patent number: 4168356
    Abstract: A process and apparatus for the polymerization of ethylene in at least one multizone reactor at a pressure of 300 to 2500 bars and at a temperature of 150 to 350.degree. C. The reaction mixture is passed from the reactor to a separator at a pressure of 50 to 500 bars in which the polymer separates from the gas. The polymer is then passed to a hopper at a pressure of 1 to 20 bars in which the major part of the gas remaining dissolved in the polymer is removed. The gas from the separator is recompressed and is returned only to the first zone of the reactor.
    Type: Grant
    Filed: March 29, 1978
    Date of Patent: September 18, 1979
    Assignee: Societe Chimique des Charbonnages-CdF Chimie
    Inventors: Bernard Levresse, Robert Fonmartin
  • Patent number: 4146729
    Abstract: A continuous process is disclosed for direct esterification of terephthalic acid with ethylene glycol to form low molecular weight polyester with recovery of excess glycol from reaction off-gases. The terephthalic acid is mixed with an excess of glycol, the mixture is reacted at 280.degree.-315.degree. C. in reaction product circulated from a reactor through an external heater and back to the reactor, and reaction product is withdrawn from the reactor for polymerization to high molecular weight polyester. Vapors formed in the reactor are fed into the bottom of a rectification column where the excess glycol is recovered for direct reuse. The vapor feed is sprayed with condensate at 140.degree.-195.degree. C. in the bottom of the column to remove solids and maintain conditions suitable for obtaining less than 0.05 percent glycol in overhead distillate and 0.3 to 10 percent water in glycol condensate.
    Type: Grant
    Filed: April 7, 1977
    Date of Patent: March 27, 1979
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: George R. Goodley, Donald A. Shiffler
  • Patent number: 4146691
    Abstract: A process for producing a cyclopentadiene resin by heat copolymerizing a cyclopentadiene monomer and a comonomer copolymerizable therewith, which comprises(a) using a vinyl monomer containing an ester linkage or a hydroxyl group as the comonomer, and(2) feeding the polymerizable ingredients and optionally an inert solvent from a material-preparing zone to a polymerization zone to polymerize the polymerizable ingredients, feeding the polymer solution formed in the polymerization zone into a separating zone to separate a low-boiling mixture consisting of the unreacted monomers, a by-product oil and optionally the inert solvent from the resulting cyclopentadiene resin, and recycling at least a part of the separated low-boiling mixture to the material-preparing zone for use as a polymerizable ingredient.
    Type: Grant
    Filed: November 28, 1977
    Date of Patent: March 27, 1979
    Assignee: Nippon Zeon Co., Ltd.
    Inventors: Akira Wada, Takao Okuda, Risoh Iwata
  • Patent number: 4146693
    Abstract: Improved continuous process for synthesis of cis-1,4 poly(isoprene). In the commercial process for synthesis of cis-1,4 poly(isoprene) only a portion of the monomer charged is polymerized. The polymer, thus obtained, is separated from the unreacted monomer which in turn is recycled with solvent back into the system for conversion to additional polymer. Fresh monomer must be added from a separate feed to this recycle stream in sufficient quantity to replace or "make-up" for that which was converted to polymer. In the improved process of this invention, this "make-up" isoprene monomer is dried and then is introduced into the process subsequent to the initiation of polymerization of the isoprene monomer already present within the system, but prior to deactivation of the polymerization catalyst. Dehydration of "make-up" isoprene prior to its introduction into the process stream at the above juncture avoids deactivation of the still active catalyst with water.
    Type: Grant
    Filed: December 2, 1977
    Date of Patent: March 27, 1979
    Assignee: The B. F. Goodrich Company
    Inventor: Robert E. Beauregard
  • Patent number: 4138421
    Abstract: Allyl halides are polymerized by a catalyst, silicic or silicoformic acids, to produce poly(allyl halide) polymer and poly(allyl alcohol) polymer.
    Type: Grant
    Filed: November 9, 1977
    Date of Patent: February 6, 1979
    Inventor: David H. Blount
  • Patent number: 4137220
    Abstract: A Novolak epoxy resin is prepared by adding an aqueous solution of alkali metal hydroxide to a solution of Novolak phenolic resin in epichlorohydrin, distilling off water during said addition in the form of an azeotrope with epichlorohydrin and recycling the latter, while maintaining the reaction medium at 60-80.degree. C and at a pH between 7 and 8 and a water content of from 0.5 to 2.5 wt.% in said medium.The thermosetting resin thus obtained can be used in applications requiring resins with low chlorine contents, low viscosity and high epoxy value.
    Type: Grant
    Filed: December 6, 1976
    Date of Patent: January 30, 1979
    Assignee: Societa' Italiana Resine S.I.R. S.p.A.
    Inventors: Giorgio Lazzerini, Silvio Vargiu, Mario Pitzalis
  • Patent number: 4132718
    Abstract: A liquid epoxy resin is produced by gradually feeding an aqueous solution of alkali metal hydroxide into a solution of bisphenol-A in epichlorohydrin, while maintaining the reaction medium at boiling point, distilling off water in the form of an azeotrope with epichlorohydrin and recycling the latter, and maintaining a water content of from 0.1 to 0.7 wt.% and a pH value between 7 and 9 in said reaction medium. The liquid epoxy resins thus obtained have low values of the viscosity, epoxy equivalent and hydrolyzable chlorine content.
    Type: Grant
    Filed: December 7, 1976
    Date of Patent: January 2, 1979
    Assignee: Societa' Italiana Resine S.I.R. S.p.A.
    Inventors: Silvio Vargiu, Mario Pitzalis, Giancarlo Crespolini, Gino Giuliani
  • Patent number: 4129701
    Abstract: Apparatus and process is herein disclosed by which a polymerizable monomer or mixture thereof can be economically and efficiently converted to polymeric substances with a high yield catalyst and, optionally, co-catalyst by a vapor phase, essentially isobaric, polymerization process using a horizontal, stirred-bed, quench-cooled, essentially total reactor off-gas recycle reactor.
    Type: Grant
    Filed: December 19, 1975
    Date of Patent: December 12, 1978
    Assignee: Standard Oil Company (Indiana)
    Inventors: James L. Jezl, Edwin F. Peters
  • Patent number: 4121029
    Abstract: A method and apparatus are provided in a pipeloop reactor system for recovery of soluble catalyst components from polymer slurry effluent into the pipe-loop reactor. The polymer slurry is collected in a wash column attached to the upper run of the loop reactor; the slurry is allowed to settle through a countercurrent flow of wash liquid, the liquid used for wash, being one in which catalyst components are soluble; the washed slurry is collected in a settling leg attached to the wash column; and wash liquid containing catalyst components is overflowed into the reactor loop. In peferred embodiments of the invention the wash liquid is subjected to auto-refrigeration before being admitted into the wash column. In another preferred embodiment unreacted monomer feed is recovered from the polymer slurry, purified, and recycled as wash liquid. In still another embodiment of the invention the flow of polymer from the reactor loop into the wash column is mechanically restricted.
    Type: Grant
    Filed: December 6, 1976
    Date of Patent: October 17, 1978
    Assignee: Phillips Petroleum Company
    Inventors: Howard B. Irvin, Fred T. Sherk
  • Patent number: 4110316
    Abstract: A continuous process is disclosed for direct esterification of terephthalic acid with ethylene glycol, followed by low-pressure polymerization in a continuous polymerizer and in a finisher polymerizer to produce polyester suitable for melt-spinning into yarn for textile uses. Vapors from the polymerizers are condensed in spray condensers to recover glycol liquid, which is recycled to the direct esterification reaction. Efficient operation of the spray condensers at absolute pressures of less than 60 millimeters of mercury is achieved by addition of substantially dry ethylene glycol to lower the water content of condensate used in the sprays.
    Type: Grant
    Filed: April 14, 1977
    Date of Patent: August 29, 1978
    Assignee: E. I. Du Pont de Nemours and Company
    Inventors: Robert R. Edging, Lien-Mow Lee
  • Patent number: 4100142
    Abstract: A continuous process for producing high molecular weight polyester of fiber-forming quality is described. The process includes the direct esterification of a dicarboxylic acid with a glycol to yield a prepolymer mixture of ester and low molecular weight polyester condensable under conditions of elevated temperature and vacuum into polymer of high intrinsic viscosity.
    Type: Grant
    Filed: October 20, 1976
    Date of Patent: July 11, 1978
    Assignee: Fiber Industries, Inc.
    Inventors: Peter Schaefer, Peter Alan Mason, William Harold Yates
  • Patent number: 4094942
    Abstract: A method for removing unreacted monomer (or monomers) from an ethylene homopolymer or a copolymer of ethylene and at least one monomer copolymerizable with ethylene during the course of pelletization by use of an extruder, said polymer having been formed by high-pressure polymerization by use of a radiation or a radical initiator, discharged from the reactor by way of a separator, and fed to said extruder to be pelletized, which method comprises injecting into said extruder 0.1 to 10% by weight (based on said polymer) of water or steam intermixing the polymer and the water or steam in the mixing section of the extruder screw, and subjecting the resulting mix to a subatmospheric pressure of 500 mmHg (absolute) or less in the venting zone provided in the extruder. This method permits efficient removal of the unreacted ethylene or the unreacted ethylene and comonomer contained in a homopolymer or copolymer of ethylene.
    Type: Grant
    Filed: January 19, 1976
    Date of Patent: June 13, 1978
    Assignees: Sumitomo Chemical Company, Limited, The Japan Steel Works, Ltd.
    Inventors: Setsuo Nakai, Hiroshi Ochi
  • Patent number: 4091200
    Abstract: In the production of ethylene-vinyl acetate copolymers in a free radical catalyst initiated high pressure process, explosive decomposition is prevented by contacting the reactor effluent downstream of the reactor outlet with small amounts of a hindered phenolic compound, separating unreacted monomer from the mixture of copolymer, unreacted monomer and scavenger in a separation zone and recycling the separated monomer to the reactor.
    Type: Grant
    Filed: March 23, 1977
    Date of Patent: May 23, 1978
    Assignee: Dart Industries Inc.
    Inventor: Jan Edmond Vandegaer
  • Patent number: 4075287
    Abstract: A stream containing at least one noncondensible, under ordinary pressure and temperature, component and at least two components which are condensible under ordinary pressure and temperature are separated by subjecting said stream to successive fractional distillation conditions to successively remove highest boiling components. An overhead produced in one fractional distillation zone is introduced as a feed into the next fractional distillation zone. The penultimate overhead comprising only the noncondensible and a lowest boiling condensible component is partially condensed. The liquid phase is introduced onto the top tray of a last fractionation zone and the vapor phase is introduced below the top tray. A vapor stream containing a single condensible component and at least one noncondensible can be separated in the same manner as the penultimate overhead of a multi-component mixture.
    Type: Grant
    Filed: October 27, 1976
    Date of Patent: February 21, 1978
    Assignee: Phillips Petroleum Company
    Inventor: Jack S. Scoggin
  • Patent number: RE30148
    Abstract: A melt finish process is disclosed herein for working up solid, particulate polymer from a vapor state polymerization reactor, which reactor employs high yield catalysts, whereby the polymer is moved out of the reactor and into a post polymerization zone characterized by essentially adiabatic polymerization and the heat of such polymerization is used in raising the temperature of and melting said solid, particulate polymer to form molten polymer for further processing.
    Type: Grant
    Filed: July 17, 1978
    Date of Patent: November 13, 1979
    Assignee: Standard Oil Company (Indiana)
    Inventors: James L. Jezl, Edwin F. Peters