Purification Or Recovery Patents (Class 568/958)
  • Patent number: 9040758
    Abstract: A method of removing alkalinity and salt from a nitroaromatic product downstream of water washing to remove mineral acids and alkaline washing to remove salts of organic acids, comprises washing the product stream with an acidic aqueous solution, prior to the step of removing excess organic reactant, by steam stripping or distillation. Acid removed from the stripper or column is recycled back for use in the acidic washing. The acidic washing is done instead of the neutral washing step of the prior art. It removes residual salt and decreases the level of entrained colloidal water in the nitroaromatic product.
    Type: Grant
    Filed: August 18, 2009
    Date of Patent: May 26, 2015
    Assignee: NORAM INTERNATIONAL LIMITED
    Inventor: Sergio Berretta
  • Patent number: 9012701
    Abstract: A method of removing alkalinity and salt from a nitroaromatic product downstream of water washing to remove mineral acids and alkaline washing to remove salts of organic acids, comprises washing the product stream with an acidic aqueous solution, prior to the step of removing excess organic reactant, by steam stripping or distillation. Acid removed from the stripper or column is recycled back for use in the acidic washing. The acidic washing is done instead of the neutral washing step of the prior art. It removes residual salt and decreases the level of entrained colloidal water in the nitroaromatic product.
    Type: Grant
    Filed: August 18, 2009
    Date of Patent: April 21, 2015
    Assignee: Noram International Limited
    Inventor: Sergio Berretta
  • Patent number: 8907144
    Abstract: A process for continuous adiabatic nitration of toluene to mononitrotoluene (MNT). The process yields a product quality of MNT that is comparable to that obtained by isothermal production. The process uses excess toluene, with the reaction rate being controlled to maintain a residual of 0.003-0.102 wt % nitric acid in the spent acid and an orange to red color of the spent acid. Further process conditions include re-concentrated sulfuric acid at 83 to 99 degrees C. with a concentration of sulfuric acid from 66 to 70.5 wt %. This is mixed with nitric acid to generate a mixed acid with 1.0 to 3.8 wt % nitric acid and toluene is added at a rate of 1.1 to 1.71 moles toluene/mole nitric acid. The reactants are mixed in a reactor with an overall average mixing intensity of 5.8 to 19 W/kg of contained solution.
    Type: Grant
    Filed: March 22, 2012
    Date of Patent: December 9, 2014
    Assignee: NORAM International Limited
    Inventor: Michael Gattrell
  • Patent number: 8207382
    Abstract: A method for stabilizing nitro compounds against discoloration. The method comprises reacting nitro compounds containing color-forming impurities with nitric acid, neutralizing and washing the product, and distilling therefrom purified nitro compounds.
    Type: Grant
    Filed: April 8, 2009
    Date of Patent: June 26, 2012
    Inventors: Daniel M. Trauth, Edward L. Little, Richard L. James, John D. Gummere, Morteza Mokhtarzadeh, Li Wang
  • Patent number: 5221440
    Abstract: A process for removing organic compounds, including nitro-hydroxy-aromatic compounds and amines, from alkaline wastewater, and in particular from wastewater generated in the production of nitrobenzene, dinitrobenzene, nitrotoluene and dinitrotoluene. The process involves distilling the alkaline wastewater steam at or near atmospheric pressure until it is concentrated five to twenty-five fold. The distillate includes water, which may be discharged to the environment, subjected to biological treatment, or recycled for use in the production process; and volatile organics, which are phase separated from the aqueous portion of the distillate and which may be recycled to the crude product stream. The concentrated residue from the distillation may be incinerated or subjected to biological treatment.
    Type: Grant
    Filed: April 20, 1992
    Date of Patent: June 22, 1993
    Assignee: Rubicon Inc.
    Inventors: Aki Miyagi, Walter Kraushaar, John B. Wilcoxon, Toby Gerhold
  • Patent number: 5180859
    Abstract: A process for the preparation of halonitroalkanes, e.g. bromonitromethane, is disclosed in which a nitroalkane is reacted with an alkali metal base or an alkaline earth metal base, and the resulting nitroalkane salt is halogenated to form the halonitroalkane in a reaction mixture. The process is improved by acidifying the reaction mixture, preferably to pH=0-4, and thereafter recovering the halonitroalkane by azeotropic distillation of the reaction mixture. The acidification step increases the amount of halonitroalkane recovered, as compared to prior art processes in which the reaction mixture is distilled without prior acidification.
    Type: Grant
    Filed: July 7, 1992
    Date of Patent: January 19, 1993
    Assignee: Great Lakes Chemical Corporation
    Inventors: Larry D. Timberlake, James L. Brennan
  • Patent number: 5151190
    Abstract: A method for separating water by pervaporation from a liquid mixture comprising isopropanol and water, which comprises (a) heating the liquid mixture, then supplying the heated mixture to a pervaporation membrane module unit using a polyimide-type separating membrane to conduct separation of the liquid mixture, recycling a part or whole of the liquid not permeated through the membrane to a feed liquid mixture, supplying a fresh feed liquid mixture to an optional place in the circulation route, and withdrawing the liquid mixture from an optional place in the circulation route, (b) controlling the amount of the liquid to be recycled among the liquid not permeated through the membrane to a level of at least 10 times by volume the amount of the fresh feed liquid mixture, and (c) controlling the difference between the liquid temperature at the inlet of the membrane module unit and the liquid temperature at the outlet of the membrane module unit to a level of at most 20.degree. C.
    Type: Grant
    Filed: December 27, 1991
    Date of Patent: September 29, 1992
    Assignees: Ryoka Techno Engineering & Construction Co., Mitsubishi Kasei Corporation
    Inventor: Furuto Seiryo