With Pretreatment Process Patents (Class 536/70)
  • Patent number: 11566372
    Abstract: A method for defibrating a fiber body includes: a supply step of supplying a liquid to a fiber body containing fibers; and a defibrating step of defibrating the fiber body to which the liquid is supplied, and in the supply step, the liquid is supplied to the fiber body so that a rate in tensile strength of the fiber body immediately before defibrated in the defibrating step to the fiber body before the liquid is supplied thereto is 60.0% or less.
    Type: Grant
    Filed: December 2, 2019
    Date of Patent: January 31, 2023
    Assignee: SEIKO EPSON CORPORATION
    Inventors: Tetsuya Aoyama, Shinichi Kato, Shigemi Wakabayashi, Yoshihiro Ueno, Shunichi Seki, Takumi Sago, Hiroki Kurata
  • Patent number: 11091564
    Abstract: The invention relates to the separation of manure in fractions and the treatment of said fractions in order to retrieve useful components to produce manure-derived bioplastic and other manure-derived bioproducts. The invention further relates to a method for producing composite (bio)plastic, and to a method for producing fibre from regenerated manure-derived cellulose. The methods include the steps of: flocculation treatment and a filtration treatment; pulping the manure-derived solid fractions; acetylation of the manure-derived dissolving-grade cellulose pulp with acetic anhydride and a catalyst; extracting fermentable components from the different fractions of the manure to produce monocarboxylic acids for use in the monocarboxylic acid carrier solution. Furthermore methods are disclosed for forming composite bioplastics with resin binding agents; and for spinning yarn from cellulose pulp.
    Type: Grant
    Filed: May 17, 2017
    Date of Patent: August 17, 2021
    Inventor: Jalila Essaidi
  • Publication number: 20150141639
    Abstract: A process for producing a cellulose derivative, including reacting a reactant and a cellulose or a derivative thereof in a solid-liquid heterogeneous system to form a cellulose derivative containing a long-chain organic group having 5 or more carbon atoms introduced therein, in a swollen state, and performing solid-liquid separation to obtain the cellulose derivative containing a long-chain organic group introduced therein.
    Type: Application
    Filed: May 31, 2013
    Publication date: May 21, 2015
    Inventors: Kiyohiko Toyama, Massatoshi Iji, Shukichi Tanaka
  • Patent number: 8993747
    Abstract: The present invention relates to a process for the production of alkali cellulose for the production of alkali cellulose and, optionally, cellulose ethers from cellulose in the presence of alkali and, if applicable, with alkylating and/or hydroxyalkylating agent(s) comprising the reaction of a cellulose with an alkali metal hydroxide, wherein the alkali metal hydroxide is mixed with cellulose in a mixing apparatus, the mixing apparatus (1) having an upper region (20, 102a, 202a) with a first cross-section and a lower region (21, 102b, 202b) with a second cross-section, the second cross-section being the same as or smaller than the first cross-section and comprising at least one non-horizontally oriented mixing device (23, 27, 121, 221, 224).
    Type: Grant
    Filed: January 8, 2010
    Date of Patent: March 31, 2015
    Assignee: Dow Global Technologies LLC
    Inventors: Matthias Sprehe, Bettina Hoelzer
  • Publication number: 20140212670
    Abstract: Provided is a process for obtaining solid cellulose, such as a cellulose solidified article or cellulose shaped article, from a cellulose solution without causing discharge of large amounts of waste liquids and environmental issues such as large energy consumption. The process produces solid cellulose through the steps of (A) dissolving cellulose in a solvent (s1) to give a cellulose solution, where the solvent (s1) includes at least one onium hydroxide in a content of from 45 to 85 percent by weight and water in a content of from 15 to 55 percent by weight, and the at least one onium hydroxide is selected from the group consisting of quaternary phosphonium hydroxides and quaternary ammonium hydroxides; (B) bringing the cellulose solution into contact with a poor solvent (s2) to precipitate cellulose as a cellulose solidified article; and (C) separating and collecting the cellulose solidified article.
    Type: Application
    Filed: December 23, 2013
    Publication date: July 31, 2014
    Applicant: DAICEL CORPORATION
    Inventors: Shu SHIMAMOTO, Hiroyuki OHNO
  • Publication number: 20130115654
    Abstract: A method for utilizing agricultural biomass components, namely cellulose, hemicellose, and lignin, and converting them to value-added biobased chemical products is described herein. The present method provides treatments to obtain a plurality of component streams from agricultural biomass for producing derivative products while minimizing waste products.
    Type: Application
    Filed: November 9, 2011
    Publication date: May 9, 2013
    Applicant: Thesis Chemistry, LLC
    Inventors: John R. Peterson, Christopher M. Yost, Jian Wu
  • Publication number: 20130115653
    Abstract: A method for utilizing woody biomass components, namely cellulose, hemicellose, and lignin, and converting them to value-added biobased chemical products is described herein. The present method provides treatments to obtain a plurality of component streams from woody biomass for producing derivative products while minimizing waste products.
    Type: Application
    Filed: November 9, 2011
    Publication date: May 9, 2013
    Applicant: Thesis Chemistry, LLC
    Inventors: John R. Peterson, Christopher M. Yost, Jian Wu
  • Publication number: 20120121830
    Abstract: This invention relates a cellulose solution comprising cellulose and at least one tetraalkylammonium alkylphosphate and processes to produce the cellulose solution. Another aspect of this invention relates to shaped articles prepared from a cellulose solution comprising cellulose and at least one tetraalkylammonium alkylphosphate. Another embodiment of this invention relates to compositions comprising derivatives of cellulose prepared from a cellulose solution comprising at least one tetraalkylammonium alkylphosphate. Another embodiment of this invention relates to compositions comprising regioselectively substituted cellulose esters prepared from a cellulose solution comprising cellulose and at least one tetraalkylammonium alkylphosphate. In another embodiment of the invention, the cellulose esters of the present invention are used as protective and compensation films for liquid crystalline displays.
    Type: Application
    Filed: January 25, 2012
    Publication date: May 17, 2012
    Applicant: Eastman Chemical Company
    Inventors: Charles Michael Buchanan, Norma Lindsey Buchanan, Elizabeth Guzman-Morales
  • Publication number: 20110230655
    Abstract: A process is disclosed for regenerating or derivatizing cellulose. The process comprises the steps of providing a source of unrefined cellulose, and dissolving the unrefined cellulose in a molten inorganic salt. The source of unrefined cellulose may be a biomass, such as wood. The process permits the regeneration or derivatization of cellulose having a high degree of polymerization.
    Type: Application
    Filed: February 18, 2011
    Publication date: September 22, 2011
    Inventors: Jacob A. MOULIJN, Sjoerd Daamen, Paul O'Connor, Rob Van Der Meij
  • Publication number: 20070249824
    Abstract: The present invention relates to a method of manufacturing cellulose acetate by use of a high temperature steam reactor vessel and a superheated steam generator. According to this method, a material to which solid catalyst added is subject to a steaming process so as to cause cellulose content to be separated from the material, followed by carrying out an acetylating process of the separated cellulose content together with solid acid in the state of being pressurized so as to obtain cellulose acetate. The high temperature steam reactor vessel employs a system that there is arranged in a reactor vessel body 1 a cartridge 2 filled with collective chips 100, whereby enabling the material subjected to the process to be readily handled and processed, and also resulting in that there is no need to carry out in a later process separation between useful content and residue produced in hydrolysis with high temperature steam.
    Type: Application
    Filed: August 28, 2006
    Publication date: October 25, 2007
    Applicant: ITEF INC.
    Inventor: Teruyuki Shikata
  • Patent number: 6835828
    Abstract: Disclosed is a process for producing reactive cellulose for use in the manufacture of cellulose acetate having superior clarity by mercerizing hardwood cellulosic material and reacting it with an hydroxyalkylating agent to a degree of molar substitution ranging from 0.04 to 0.15 per anhydroglucose unit in cellulose.
    Type: Grant
    Filed: July 8, 2003
    Date of Patent: December 28, 2004
    Assignee: Rayonier Inc.
    Inventors: Karl D. Sears, Wendy Hendricks
  • Patent number: 6683174
    Abstract: The present invention provides a cellulose triacetate which exhibits a satisfactory filtration performance Thus, the present invention provides a cellulose triacetate whose occlusion constant (K) determined by the following method is 70 or less. Method: the cellulose triacetate is dissolved in a solvent mixture of methylene chloride/methanol (9/1 w/w) to form a 16% by weight (as a solid concentration) solution, which is then filtered under a constant pressure at the filtration pressure of 3 kg/cm2 and the temperature of 25° C. using a muslin filter to determine a filtered volume with the lapse of time, from which the slope of a linear curve represented by t/V−t (wherein t is a filtration time (sec) and V is a filtered volume (ml)) is calculated to obtain an occlusion constant (K) where K=slope×2×104.
    Type: Grant
    Filed: May 8, 2001
    Date of Patent: January 27, 2004
    Assignee: Daicel Chemical Industries, Ltd.
    Inventors: Toru Ozaki, Hiroshi Ogawa, Hirofumi Sasai
  • Publication number: 20040002598
    Abstract: The invention provides a process for manufacturing at low cost cellulose acetate, which is useful as a biodegradable plastic, using corncob meal which has hitherto been thrown away as a raw material. More specifically, the invention provides a process for manufacturing cellulose acetate, which comprises the steps of: steaming corncob meal at a temperature of 150 to 250° C. and a pressure of 20 to 29 MPa; filtering the steamed corncob meal to obtain a solid product; and dehydrating and acetylating by adding acetic anhydride and sulfuric acid to the solid product. The steaming is preferably carried out by using a pressure vessel and the filtering is preferably carried out by using a filtering device.
    Type: Application
    Filed: May 16, 2003
    Publication date: January 1, 2004
    Inventors: Shunichi Matsuo, Takatsugu Takamura
  • Publication number: 20030050472
    Abstract: Disclosed is a process for producing reactive cellulose for use in the manufacture of cellulose acetate having superior clarity by mercerizing hardwood cellulosic material and reacting it with an hydroxyalkylating agent to a degree of molar substitution ranging from 0.04 to 0.15 per anhydroglucose unit in cellulose.
    Type: Application
    Filed: August 31, 2001
    Publication date: March 13, 2003
    Applicant: Rayonier Inc.
    Inventors: Karl D. Sears, Wendy Hendricks
  • Patent number: 6407224
    Abstract: A catalytic system for cellulose acylation includes an adduct of sulfuric acid with N,N-dimethylacetamide, free sulfuric acid or free N,N-dimethylacetamide with the following mole ratio of the components: adduct:1.0; free sulfuric acid, max:0.49; or free N,N-dimethylacetamide, max:0.4. A process for producing such a catalytic system is based upon reacting sulfuric acid with N,N-dimethylacetamide in an anhydrous medium at a temperature of 0° C.-25° C. with the following mole weight ratio of the components: sulfuric acid:1.0; N,N-dimethylacetamide, max:1.4. A process for cellulose acylation in the presence of this catalytic system incorporates cellulose treatment with acetic acid followed by treatment of the resultant activated cellulose with a lower fatty acid anhydride at a temperature of 10° C.-90° C. in the presence of this catalytic system taken in an amount of 1.5-30.0 wt.
    Type: Grant
    Filed: July 16, 1999
    Date of Patent: June 18, 2002
    Assignee: Nauchno-prozvodstvennaya firma “Efiry Tselljulosy”
    Inventors: Dmitry Petrovich Mironov, Anatoly Ivanovich Shamolin, Eduard Pavlovich Grishin, Valentin Ananievich Bondar
  • Publication number: 20010011132
    Abstract: A process for producing cellullose acetate by acetylation reaction with cellulose as a raw material, wherein acetate is used as an acetylating agent.
    Type: Application
    Filed: February 1, 2001
    Publication date: August 2, 2001
    Inventors: Katsuyoshi Yamakawa, Koushin Matsuoka, Tadahisa Sato
  • Patent number: 6103891
    Abstract: The present invention presents novel methods for recovery of phosphoramidites from the waste products of oligonucleotide synthesis. The methods include reacting a trihalophenoxydihalophosphorane with a H-phosphonate in the presence of an amine.
    Type: Grant
    Filed: February 12, 1999
    Date of Patent: August 15, 2000
    Assignee: Isis Pharmaceuticals, Inc.
    Inventors: Richard H. Griffey, Douglas L. Cole, Vasulinga T. Ravikumar
  • Patent number: 6083498
    Abstract: Compositions and lures are described which provide vapor blends of acetic acid and one or more compounds selected from the group consisting of isobutanol, racemic 2-methyl-1-butanol, S-(-)-2-methyl-1-butanol, 2-methyl-2-propanol, heptyl butyrate, and butyl butyrate which function as highly effective attractants for yellowjacket wasps and paper wasps. By attracting wasps to traps or baits, the chemical attractants provide a means for detecting, surveying, monitoring, and controlling the wasps.
    Type: Grant
    Filed: March 10, 1998
    Date of Patent: July 4, 2000
    Assignee: The United States of America as represented by the Secretary of Agriculture
    Inventor: Peter J. Landolt
  • Patent number: 5990304
    Abstract: An object of the invention is to obtain cellulose acetate with improved physical properties, particularly film strength arid improved flexibility of the molded product. Cellulose acetate wherein average degree of acetylation is not less than 59%, viscosity average degree of polymerization (DP) is not less than 290, and concentrated solution viscosity (.eta.) according to the falling ball viscosity method for viscosity average degree of polymerization (DP) is expressed by the following formula (1): 2.814.times.ln(DP)-11.753.ltoreq.ln(.eta.).ltoreq.7.28.times.ln(DP)-37.059 (1) and a process for production thereof.
    Type: Grant
    Filed: October 9, 1998
    Date of Patent: November 23, 1999
    Assignees: Daicel Chemical Industries, Ltd., Fuji Photo Film Co., Ltd.
    Inventors: Atsunobu Kiyose, Shu Shimamoto, Yuichiro Shuto, Hiroki Taniguchi
  • Patent number: 5962677
    Abstract: Cellulose acetate having a high moldability and low solution viscosity in spite of having a high average degree of polymerization is obtained. The low molecular weight components of cellulose acetate (e.g., CTA having average degree of acetylation of 59.0 to 62.5%) are eluted with a washing solvent to produce a cellulose acetate having a molecular weight distribution Mw/Mn of 1 to 1.7. As the washing solvent, those swell or partially dissolve the cellulose acetate, for example, those which dissolve 0.1 to 30% by weight of cellulose acetate can be used. This solvent includes, for example, a solvent having a solubility parameter .delta. of 7 to 12.5 (ketones, ethers, organic acid, esters, etc.).
    Type: Grant
    Filed: October 9, 1998
    Date of Patent: October 5, 1999
    Assignees: Daicel Chemical Industries, LTD., Fuji Photo Film Co., LTD.
    Inventors: Ko Murakami, Toshinori Okano, Hiroki Taniguchi, Atsunobu Kiyose, Shu Shimamoto
  • Patent number: 5928613
    Abstract: In a production process of a cellulose acetate which comprises (a) a reduced pressure-acetylation step of acetylating a cellulose under a reduced pressure in the presence of sulfuric acid or other acidic catalyst, with distilling off a gaseous phase component of the reaction system out of the system, and (b) a post-acetylation step of allowing the acetylation to further proceed by increasing the pressure as compared with the pressure of the reduced pressure-acetylation step by means of release of the pressure reduction of the reaction system or the like, the shift operation from the reduced pressure-acetylation step to the post-acetylation step is conducted by taking a distilling rate of a distillate in the reduced pressure-acetylation step as an index to control the reaction temperature of the post-acetylation step.
    Type: Grant
    Filed: June 8, 1998
    Date of Patent: July 27, 1999
    Assignee: Daicel Chemical Industries, Ltd.
    Inventor: Mitsuru Yamashita
  • Patent number: 5929229
    Abstract: The present invention relates to a process for preparing cellulose esters having a total DS/AGU of 0.1 to 3.0, said process consisting of contacting the following:(i) a cellulose material,(ii) a solubilizing amount of a solvent system comprising a carboxamide diluent or a urea-based diluent,(iii) an acylating reagent, and(iv) a titanium-containing compound.
    Type: Grant
    Filed: March 6, 1998
    Date of Patent: July 27, 1999
    Assignee: Eastman Chemical Company
    Inventors: Kevin J. Edgar, Richard T. Bogan
  • Patent number: 5914397
    Abstract: An object of the invention is to obtain cellulose acetate having improved physical properties, particularly film strength and improved flexibility of the molded product. Cellulose acetate having an average degree of acetylation of not less than 59%, viscosity average degree of polymerization (DP) of not less than 290. and concentrated solution viscosity (.eta.) according to falling ball viscosity method for viscosity average degree of polymerization (DP) expressed by the following formula (1):2.814.times.ln(DP)-11.753.ltoreq.ln(.eta.).ltoreq.7.28.times.ln(DP)-37.059( 1)and a process for the production thereof.
    Type: Grant
    Filed: November 21, 1996
    Date of Patent: June 22, 1999
    Assignee: Daicel Chemical Industries, Ltd.
    Inventors: Atsunobu Kiyose, Shu Shimamoto, Yuichiro Shuto, Hiroki Taniguchi
  • Patent number: 5869646
    Abstract: In a production process of a cellulose acetate which comprises (a) a reduced pressure-acetylation step of acetylating a cellulose under a reduced pressure in the presence of sulfuric acid or other acidic catalyst, with distilling off a gaseous phase component of the reaction system out of the system, and (b) a post-acetylation step of allowing the acetylation to further proceed by increasing the pressure as compared with the pressure of the reduced pressure-acetylation step by means of release of the pressure reduction of the reaction system or the like, the shift operation from the reduced pressure-acetylation step to the post-acetylation step is conducted by taking a distilling rate of a distillate in the reduced pressure-acetylation step as an index to control the reaction temperature of the post-acetylation step.
    Type: Grant
    Filed: January 22, 1997
    Date of Patent: February 9, 1999
    Assignee: Daicel Chemical Industries, Ltd.
    Inventor: Mitsuru Yamashita
  • Patent number: 5821359
    Abstract: The invention relates to a process for acetylation of lignocellulosic fibres (LF) using an acetylating agent comprising acetic anhydride at a temperature of above 140.degree. C. and a pressure of 100-150 kPa wherein raw or substantially raw LFs are treated with a superheated acetylating agent comprising at least 20 % w/w acetic anhydride for a duration of at least 1.5 minutes in an acetylation reactor (3), the treatment with superheated acetylating agent also ensuring that the acetylated LFs are substantially free from occluded, adsorbed or absorbed acetylating agent, the amounts of which are less than 5 % w/w of the acetylated LFs recovered from the base of a circulation cyclone (5), so as to substantially acetylate the LFs to achieve a weight gain of at least 2 %. The LFs may optionally be pre-treated, prior to being treated with the superheated acetylating agent, preferably by spraying, for a very short period of time.
    Type: Grant
    Filed: August 20, 1997
    Date of Patent: October 13, 1998
    Assignee: A-Cell Acetyl Cellulosics AB
    Inventors: Helen Louise Nelson, David Ian Richards
  • Patent number: 5770726
    Abstract: The present invention relates to a process for preparing a substituted cellulose acetoacetate alkanoate without using a carboxamide/lithium chloride solvent system. The process involves contacting cellulose in a carboxylic acid diluent with an acetylating compound selected from the group consisting of a carboxylic acid anhydride and an acid chloride, an acetoacetylating compound selected from the group consisting of diketene, an alkyl acetoacetate and 2,2,6-trimethyl-4H-1,3-dioxin-4-one, and a mineral acid catalyst under conditions and in a molar ratio sufficient to cause the cellulose, acetylating compound and acetoacetylating compound to react to produce a substituted cellulose acetoacetate alkanoate.
    Type: Grant
    Filed: March 10, 1997
    Date of Patent: June 23, 1998
    Assignee: Eastman Chemical Company
    Inventors: Chung Ming Kuo, Kevin Joseph Edgar
  • Patent number: 5750677
    Abstract: The present invention relates to a process for preparing cellulose esters having a total DS/AGU of 0.1 to 3.0, said process comprising contacting the following:(i) a cellulose material,(ii) a solubilizing amount of a solvent system comprising a carboxamide diluent or a urea-based diluent,(iii) an acylating reagent, and(iv) a titanium-containing compound.
    Type: Grant
    Filed: December 30, 1994
    Date of Patent: May 12, 1998
    Assignee: Eastman Chemical Company
    Inventors: Kevin J. Edgar, Richard T. Bogan
  • Patent number: 5723600
    Abstract: A method for treating cellulose with cellulose ester for use in various paper products involves reacting cellulose and an acid anhydride to form a cellulose ester-carboxylic acid solution. Acetic anhydride may be used as the acid anhydride, and a cellulose acetate-acetic acid solution may formed as the resulting cellulose ester-acetic acid solution. The cellulose acetate-acetic acid solution is diluted in a mixer, with additional acetic acid. Bulk cellulose is milled into cellulose fibers, and the diluted cellulose acetate-acetic acid solution diluted is combined with the cellulose fibers to achieve a treated fiber. Excess cellulose acetate-acetic acid solution is removed from the treated fiber and recycled to the mixer used in dilution. The treated fiber is water washed followed by removing water from the washed treated fiber. This product can then be used in paper making to produce a sheet for circuit boards, laminated products, and various paper products.
    Type: Grant
    Filed: September 23, 1996
    Date of Patent: March 3, 1998
    Assignee: Eastman Chemical Company
    Inventor: Griffin Ivan Johnson
  • Patent number: 5674999
    Abstract: An improved process for surface treating water soluble cellulosic polymers with crosslinking agents to provide products which are more readily dispersible in cold water, and have longer viscosity delay times than can be achieved with polymers treated in low intensity mixers, such as ribbon blenders, comprising distributing the crosslinking agent using a continuous, high intensity mixer, followed by heating to facilitate surface crosslinking. This process also allows for a reduced level of crosslinking chemicals to be used.
    Type: Grant
    Filed: December 18, 1995
    Date of Patent: October 7, 1997
    Assignee: The Dow Chemical Company
    Inventors: Michael R. Smith, Gary J. Schulz, Kenneth C. Reibert
  • Patent number: 5608050
    Abstract: The specification discloses a process for the manufacture of cellulose acetate. The process reacts, at a temperature suitable for acetylation, an acetic acid activated pretreated cellulose raw material containing 100 parts cellulose by dry weight, and 0.5 to 40 parts of a bisulfate catalyst by dry weight of the cellulose. The bisulfate catalyst is selected from lithium bisulfate, sodium bisulfate, and potassium bisulfate. To enhance mixing with the activated and pretreated cellulose, the catalyst may be mixed with 2 to 4 parts of acetic anhydride by dry weight of the cellulose, and 4 to 6 parts of acetic acid by dry weight of the cellulose. In a further embodiment, 0.05 to 10 parts of a strong Bronsted acid by weight of the dry cellulose may be added as a co-catalyst.
    Type: Grant
    Filed: December 18, 1995
    Date of Patent: March 4, 1997
    Assignee: Eastman Chemical Company
    Inventors: Chung M. Kuo, Richard T. Bogan
  • Patent number: 5451672
    Abstract: A process for producing cellulose acetate from a hard, low-grade pulp sheet having a high sheet density on an industrial scale without impairing the acetylation reactivity of the pulp, characterized in that a pulp sheet having a sheet density of at least 0.5 g/cm.sup.3 is used as the cellulose material and the pulp sheet is disintegrated while feeding less than 40 parts by weight, based on 100 parts by weight (in terms of oven-dry weight) of the pulp sheet, of water into the disintegrating section of a disintegrator in the step of disintegrating the material. The present process is economically advantageous because the drying and humidity controlling steps are simplified due to the quantity of water to be fed being small.
    Type: Grant
    Filed: October 12, 1993
    Date of Patent: September 19, 1995
    Assignee: Daicel Chemical Industries, Ltd.
    Inventors: Hiroki Taniguchi, Yoshiaki Kaino, Ryota Iwata
  • Patent number: 5378828
    Abstract: The present invention provides a process for the preparation of water soluble alkali metal salts of cellulose sulfate having a degree of substitution ranging from 1 to 3 and viscosity of 1 percent aqueous solution in excess of 20 centipoises (cps). The process involves the use of chlorosulfuric acid as a sulfonating agent in the presence of pyridine used as a solvent in reaction. The important steps of the process for preparation of the water soluble salts include presoaking of the cellulose in pyridine followed by washing the pyridine salt with an alcohol such as methanol and reacting saturated alkali metal bicarbonate or carbonate solutions with the sulfonated cellulose.
    Type: Grant
    Filed: September 2, 1993
    Date of Patent: January 3, 1995
    Assignee: Dextran Products Limited
    Inventors: Thomas C. Usher, Natu Patel, Chhagan G. Tele
  • Patent number: 5371207
    Abstract: A novel method has been discovered for the pretreatment of cellulose with acetic acid and acetic anhydride under pressure, resulting in uniformly activated cellulose fibers. The improved process for producing cellulose diacetate comprises the steps of: (1) pretreating and activating the fluffed cellulose fibers in a solution of glacial acetic acid and acetic anhydride at room temperature and elevated pressure for a specific time; (2) mixing the activated cellulose containing acetic acid and anhydride further with a mixture of glacial acetic acid, acetic anhydride and sulphuric acid catalyst and acetylating the cellulose at specific initial and end temperatures to form primary cellulose acetate; and (3) partially neutralizing the sulphuric acid catalyst and destroying the excess acetic anhydride by adding an aqueous solution of magnesium acetate with dilute acetic acid to provide an excess of water in the reaction dope for hydrolysis at elevated temperature and pressure conditions.
    Type: Grant
    Filed: February 12, 1993
    Date of Patent: December 6, 1994
    Assignee: Arbokem Inc.
    Inventor: J. Ming Zhuang
  • Patent number: 5294703
    Abstract: Provided is a novel improved process for the preparation of .alpha.-D-cellobiose octaacetate via the acetylative degradation of cellulose or cellulose acetate. The title compound is provided in high yield and quality in a facile one-pot process, amenable to large-scale synthesis.
    Type: Grant
    Filed: April 7, 1993
    Date of Patent: March 15, 1994
    Assignee: Eastman Kodak Company
    Inventors: John A. Hyatt, Tony L. Sander, D. Mark Naylor, Bobby L. Bernard
  • Patent number: 5244945
    Abstract: A method is provided for preparing a cellulose ester plastic composition from waste paper (e.g. recycled paper) and/or sugar cane bagasse. The paper or bagasse is reacted with an acid anhydride in the presence of a catalyst to esterify some of the hydroxy groups on the cellulose. The resulting cellulose ester product is combined with various additives such as acetins, agricultural fillers, and carbon particles.
    Type: Grant
    Filed: July 20, 1992
    Date of Patent: September 14, 1993
    Assignee: International Communications & Energy
    Inventor: Glenn R. Elion
  • Patent number: 5150721
    Abstract: Disclosed is a novel process of preparing tobacco smoke filter material, wherein an acidic compound such as citric acid is dissolved in a cellulose acetate spinning solution prior to spinning the filaments of the filter material.
    Type: Grant
    Filed: October 10, 1990
    Date of Patent: September 29, 1992
    Inventors: Benedict M. Lee, James E. Harris
  • Patent number: 5150723
    Abstract: Disclosed is a novel tobacco smoke filter material comprising a filter element such as cellulose acetate crimped tow having at least about 1 weight percent of micro acicular crystals of a compound such as sodium carbonate present on the surfaces of the filter element. Also disclosed is a process for preparation of such tobacco smoke filter material comprising immersing the filter element in a solution of the compound capable of forming the micro acicular crystals, followed by removing the filter element from the solution and removing residual liquid, thereby forming the novel tobacco smoke filter material.
    Type: Grant
    Filed: June 8, 1990
    Date of Patent: September 29, 1992
    Assignee: Eastman Kodak Company
    Inventors: Benedict M. Lee, James E. Harris
  • Patent number: 5141006
    Abstract: Disclosed is a novel process of preparing tobacco smoke filter material, wherein an acidic compound such as citric acid is dissolved in a cellulose acetate spinning solution (dope) prior to spinning the filaments of the filter material.
    Type: Grant
    Filed: February 28, 1990
    Date of Patent: August 25, 1992
    Assignee: Eastman Kodak Company
    Inventors: Benedict M. Lee, James E. Harris
  • Patent number: 5124278
    Abstract: The present invention addresses the use of metalorganic amines as metallic donor source compounds in reactive deposition applications. More specifically, the present invention addresses the use of the amino-substituted metallic donor source compounds M(NR.sub.2).sub.3-x H.sub.x, where R is organic, alkyl or fluoroalkyl, and x is less than or equal to 2, and M=As, Sb or P, in processes requiring deposition of the corresponding element. These uses include a number of different processes; the metalorganic vapor phase epitaxy of compound semiconductor material such as GaAs, InP, AlGaAs, etc.; doping of SiO.sub.2 or borosilicate based glasses to enhance the reflow properties of the glass; in-situ n-type doping of silicon epitaxial material; sourcing of arsenic or phosphorus for ion implantation; chemical beam epitaxy (or MOMBE); and diffusion doping into electronic materials such as silicon dioxide, silicon and polycrystalline silcon.
    Type: Grant
    Filed: September 21, 1990
    Date of Patent: June 23, 1992
    Assignee: Air Products and Chemicals, Inc.
    Inventors: David A. Bohling, Gregory T. Muhr, Sherri L. Bassner
  • Patent number: 5114535
    Abstract: A process for making cellulose acetate from wood pulp takes wet wood pulp and instead of converting it into dry pulp sheet which is the usual feedstock for acetate, dries and mechanically separates the pulp into a cellulose flock using a pin mill through which a hot drying gas is passed. Deactivation of the cellulose is avoided by control of the drying gas exit temperature to 80.degree. C. to 95.degree. C. and of the moisture content of the cellulose flock to 4 to 15% by weight. The flock produced may be acetylated directly without any need for reactivation treatments additional to the normal activation with acetic acid.
    Type: Grant
    Filed: March 19, 1991
    Date of Patent: May 19, 1992
    Assignee: Courtaulds PLC
    Inventors: Richard Burley, Patrick Roche
  • Patent number: 5036900
    Abstract: Cellulosic sheet material is processed in preparation for esterification for example acetylation to produce cellulose acetate, by treating the sheet material with water and then feeding the wetted material into a machine that simultaneously shreds and dries the material. The conditions in the machine are carefully controlled (outlet temperature not in excess of 110.degree. C. and moisture content 4-15% by weight) to ensure that the cellulosic material does not become deactivated towards esterification. The method enables low alpha content cellulosic material supplied in the form of high density sheet to be acetylated to produce high quality cellulose acetate flake.
    Type: Grant
    Filed: October 17, 1990
    Date of Patent: August 6, 1991
    Assignee: Courtaulds PLC
    Inventors: Richard Burley, Lucjan S. Slota
  • Patent number: 4480090
    Abstract: The present invention relates to a method of preparing lower fatty acid esters of cellulose which comprises esterifying at a temperature of between about 75.degree. C. and about 110.degree. C. a cellulose compound having esterifiable hydroxyl groups with an esterifying bath comprising an organic acid anhydride, a diluent, and a catalyst comprising from 0.2 to 2.0 parts phosphoric acid, from 0.1 to 1.2 parts sulfuric acid, and from 0.05 to 0.6 parts of a hindered aliphatic alcohol by weight per 100 parts of the cellulose to be esterified.
    Type: Grant
    Filed: October 21, 1983
    Date of Patent: October 30, 1984
    Assignee: Eastman Kodak Company
    Inventors: Chung-Ming Kuo, Alan P. Leonard
  • Patent number: 4399275
    Abstract: Highly reactive cellulose is prepared by mercerizing cellulosic material and reacting it with an hydroxyalkylating agent to a degree of substitution ranging from 0.05 to 0.3, said degree of substitution being short of rendering the cellulose appreciably soluble in water. The highly reactive cellulose is particularly useful for the preparation of such cellulose derivatives as cellulose acetate at considerably improved production levels.
    Type: Grant
    Filed: January 6, 1982
    Date of Patent: August 16, 1983
    Assignee: ITT Corporation
    Inventor: Karl D. Sears
  • Patent number: 4385172
    Abstract: Heat treatment of never-dried dissolving pulps prior to drying prevents or retards the hornification and consequent decrease in esterification reactivity which normally occurs on drying of untreated pulps.
    Type: Grant
    Filed: March 24, 1980
    Date of Patent: May 24, 1983
    Assignee: International Paper Company
    Inventors: V. M. Yasnovsky, Donald M. MacDonald
  • Patent number: 4336370
    Abstract: Treatment of dissolving pulp derived from wood with small quantities of C.sub.2 -C.sub.18 carboxylic acids and subsequent storage of the treated pulp, under conditions where little acid evaporation can occur, for periods of about two hours or more results in a product which has more uniform reactivity toward standard activation techniques in subsequent esterification reactions which produce known cellulose esters. At certain concentrations conventional activation techniques may be dispensed with.
    Type: Grant
    Filed: March 24, 1980
    Date of Patent: June 22, 1982
    Assignee: International Paper Company
    Inventors: V. M. Yasnovsky, Donald M. MacDonald
  • Patent number: 4162359
    Abstract: Cellulose acetate is produced by subjecting highly purified cellulosic dissolving pulp to a bleaching sequence including at least one alkaline extraction stage and acetylating the bleached pulp to convert the pulp to cellulose acetate. The yellowness index of the cellulose acetate is reduced by carrying out the alkaline extraction stage in the presence of from 0.2 to 3.3%, based on dry pulp weight, of sodium or hydrogen peroxide.
    Type: Grant
    Filed: March 13, 1978
    Date of Patent: July 24, 1979
    Assignee: International Telephone and Telegraph Corporation
    Inventors: Phyllis C. Leithem, Romeo Conca