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Copolymer ligand rhodium-lithium bimetal catalyst and its manufacturing method and application

A bimetallic catalyst and copolymer technology, applied in organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, carbon monoxide reaction to prepare carboxylic acid, etc., can solve the problem of increasing the corrosion of reaction equipment and no industrial application Value, material requirements and other issues, to achieve the effect of avoiding water gas reaction, excellent stability, high selectivity

Inactive Publication Date: 2004-08-04
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This greatly increases the corrosiveness of the reaction equipment, the material requirements for the reaction process become more stringent, and it also brings certain unfavorable factors such as water gas side reactions
[0006] In 1987, people such as Shogo Shimazu (Appl.Cat., 1987 (35): 279) studied polyethylamine type chelating resin and RhCl 3 Forming a polymer complex as a catalyst for methanol carbonylation reaction has certain activity, but the catalytic space-time yield is low and has no industrial application value

Method used

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  • Copolymer ligand rhodium-lithium bimetal catalyst and its manufacturing method and application
  • Copolymer ligand rhodium-lithium bimetal catalyst and its manufacturing method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 0.3mol of purified 2-vinylpyridine and 0.7mol of methyl acrylate to 6mmol of azobisisobutyronitrile, mix well and add to 2mol of benzene, heat to 60°C for 24 hours, precipitate with ether, filter, Wash and dry to obtain the copolymer.

[0035] Add the copolymer into 400ml aqueous solution containing 10wt% sodium hydroxide, reflux and stir for 1h, adjust the pH to 6 with hydrochloric acid, stir and precipitate with ether after cooling, continue to wash the precipitate with water, salt out, filter and dry, then add Put it into an aqueous solution containing 0.47 mol of lithium hydroxide, heat it at 60°C and stir for 2 hours, precipitate it with ether after cooling, dissolve it in methanol, precipitate it with ether, and dry it to obtain a copolymer lithium salt ligand.

[0036]Dissolve the copolymer lithium salt ligand in 1.5mol methanol solution, stir at 30°C for 10min, add dropwise methanol solution containing 13mmol rhodium acetate, react for 30min, and after the s...

Embodiment 2

[0038] Weigh 0.5mol of purified 4-vinylpyridine and 0.5mol of maleic anhydride monomer, add 4mmol of benzoyl peroxide as an initiator, react in 2.5mol of benzene at 60°C for 20h, precipitate with ether, and filter , washing and drying to obtain the copolymer.

[0039] The copolymer was refluxed and hydrolyzed with 500ml aqueous solution containing 5wt% potassium hydroxide for 2 hours, adjusted the solution to pH 5 with hydrochloric acid, stirred and precipitated with ether after cooling, continued to wash the precipitate with water, salted out, filtered and dried, and then added to a solution containing 0.3 In an aqueous solution of mol lithium hydroxide, react at 70°C for 2 hours, precipitate with ether, dissolve in methanol, precipitate with ether and dry to obtain the ligand of the copolymer lithium salt.

[0040] Dissolve the copolymer lithium salt ligand in a mixture of 1.5mol methanol and 0.5mol acetic acid, stir at 20°C for 20min, add an aqueous solution containing 39mm...

Embodiment 3

[0042] Mix 0.3 mol of purified 2-vinylpyridine, 0.5 mol of methyl acrylate and 0.2 mol of methacrylate diester monomer, add 10 mmol of azobisisobutyronitrile initiator, then add 60 ml of kerosene, and mix well , added to the filled with 10wt% Na 2 SO 4 In the reaction flask of the aqueous solution, Na 2 SO 4 The volume of the aqueous solution is 400ml, the temperature is raised to 70°C, the rotation speed is 400 rpm, the amount of bentonite is 50g, and the amount of bentonite is 50g. After stirring for 1 hour, reduce to 200 rpm, stop after 24 hours of continuous reaction, and filter After washing with water, extract with acetone and dry to obtain high molecular polymer.

[0043] Add the polymer to an aqueous solution of sodium hydroxide and react at 100°C for 2 hours, adjust to an acidic pH of 5.5 with hydrochloric acid, stir and precipitate with ether after cooling, continue to wash the precipitate with water, salt out, filter and dry, and then add to a solution containing...

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Abstract

A bimetal Rh-Li catalyst for the hydroxylation reaction of methanol to obtain acetic acid or the carbonylating reaction of methyl acetate to obtain ethylanhydride is disclosed, which has 3 basic structures and features high activity, selectivity and stability. Its preparing process includes such steps as copolymerization of 2-vinylpyridine or 4-vinylpyridine on acrylic acid, acrylate, or maleic acid anhydride, hydrolzying by strong alkali, acting on lithium hydroxide to obtain ligand, reacting on Rh compound and coordination.

Description

technical field [0001] The invention relates to a copolymer ligand rhodium-lithium bimetallic catalyst. [0002] The present invention also relates to a method for preparing the above-mentioned catalyst. [0003] The present invention also relates to the application of the above-mentioned catalyst in the carbonylation of methanol to prepare acetic acid and the carbonylation of methyl acetate to prepare acetic anhydride. Background technique [0004] The production of acetic acid or acetic anhydride by carbon monoxide, methanol and methyl acetate under the action of soluble rhodium is a new type of catalytic process invented and developed by the American Monsanto Company since the 1970s. It has remarkable advantages such as high activity, low temperature and low pressure. Advantages, so the industrialization of this process marks a major breakthrough in the acetic acid industry. (Roth, J.F.; Craddock, J.H. Chem. Tech., 1971, 600) [0005] In the carbonylation reaction of m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/16C07C51/12C07C53/08
Inventor 邹瑾袁国卿
Owner INST OF CHEM CHINESE ACAD OF SCI
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