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Cationic resin catalyst, preparation method thereof and catalytic application thereof in preparation of glycolic acid by methyl glycolate hydrolysis method

A technology of cationic resin and methyl glycolate, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of increased separation cost and conversion of methyl glycolate Low efficiency and other problems, to achieve the effect of increasing conversion rate, promoting complete hydrolysis, and shortening the process flow

Pending Publication Date: 2019-04-12
丹东明珠特种树脂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the hydrolysis of methyl glycolate is a reversible reaction, restricted by chemical balance, a large amount of unhydrolyzed methyl glycolate in the reaction system needs to be recovered, resulting in increased separation costs, and there is also a technical problem that the conversion rate of methyl glycolate is too low. At present, there is no relevant report on the industrial scale application of this method.

Method used

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  • Cationic resin catalyst, preparation method thereof and catalytic application thereof in preparation of glycolic acid by methyl glycolate hydrolysis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1 Catalyst A

[0020] Suspension copolymerization system: mix 100g of styrene with 7g of divinylbenzene, wash twice with NaOH solution with a concentration of 1mol / l, and then wash twice with water to remove the polymerization inhibitor in the raw material; the porogen is cyclohexane, Initiator is cumene hydroperoxide, is 1:0.1:0.005 with the mass ratio of styrene and porogen, initiator, adds porogen and initiator in the mixture of styrene and divinylbenzene, waits After the initiator is dissolved, the whole is poured into a stirred tank that has been equipped with a dispersant of a 0.5% polyvinyl alcohol aqueous solution. The quality of the polyvinyl alcohol aqueous solution is the total mass of styrene, divinylbenzene, porogen and initiator. 3 times;

[0021] Copolymerization reaction: the rotation speed is 80r / min, first raise the temperature to 60°C, hold for 2h, then raise the temperature to 70°C, hold for 3h, finally raise the temperature to 90°C, hold fo...

Embodiment 2

[0024] Example 2 Catalyst B

[0025] Suspension copolymerization system: mix 100g of styrene with 7g of divinylbenzene, wash twice with NaOH solution with a concentration of 1mol / l, and then wash twice with water to remove the polymerization inhibitor in the raw material; the porogen is benzene, the initiator Be azobisisoheptanonitrile, the mass ratio of styrene and porogen, initiator is 1:0.1:0.005, add porogen and initiator in the mixture of styrene and divinylbenzene, treat initiator After dissolving, the whole is poured into a stirred tank with a concentration of 1.0% methylcellulose aqueous solution dispersant, the quality of methylcellulose aqueous solution is the total mass of styrene, divinylbenzene, porogen and initiator 4 times;

[0026] Copolymerization reaction: the rotation speed is 120r / min, first raise the temperature to 60°C, hold for 4h, then raise the temperature to 70°C, hold for 6h, finally raise the temperature to 90°C, hold for 1h, then cool and filter t...

Embodiment 3

[0029] Example 3 Catalyst C

[0030] Suspension copolymerization system: mix 100g of styrene with 7g of divinylbenzene, wash twice with NaOH solution with a concentration of 1mol / l, and then wash twice with water to remove the polymerization inhibitor in the raw material; the porogen is benzene, the initiator For benzoyl peroxide, the mass ratio of styrene to porogen and initiator is 1:0.05:0.02, add porogen and initiator to the mixture of styrene and divinylbenzene, and wait for the initiator to dissolve Finally, the whole is poured into the stirred tank that has been equipped with the dispersant of 0.5% sodium dodecylbenzenesulfonate aqueous solution, the quality of sodium dodecylbenzenesulfonate aqueous solution is styrene, divinylbenzene, 3 times the total mass of porogen and initiator;

[0031] Copolymerization reaction: the rotation speed is 80r / min, first raise the temperature to 60°C, hold for 2h, then raise the temperature to 70°C, hold for 3h, finally raise the temp...

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Abstract

The invention provides a cationic resin catalyst, a preparation method thereof and a catalytic application of thereof in preparation of glycolic acid by a methyl glycolate hydrolysis method. The cationic resin catalyst is prepared from styrene as a monomer and divinylbenzene as a cross-linking agent, the styrene and the divinylbenzene are copolymerized with a pore-forming agent, an initiator and adispersing agent to prepare copolymer white balls, the copolymer white balls are subjected to pore purification and sulfonation to prepare the cationic resin catalyst, wherein the mass ratio of the styrene to the divinylbenzene is 100:7, the mass ratio of the pore-forming agent to the initiator is 1: (0.05-0.3) : (0.005-0.03), and the ratio of the total mass of the styrene, divinylbenzene, pore-forming agent and initiator to the weight of the dispersing agent is 1: (3-4). The catalytic application of the methyl glycolate hydrolysis method for preparing glycolic acid in a catalytic distillation tower has the advantages of short process flow, complete hydrolysis of the methyl glycolate, improvement of the conversion rate of the methyl glycolate, overcoming the technical problem of reverse decomposition of the glycolic acid, long service life of the catalyst and low energy consumption.

Description

technical field [0001] This patent application relates to a cationic resin catalyst, its preparation method and its catalytic application, and its characteristics relate to a catalyst that can ensure the industrial application of glycolic acid produced by hydrolysis of methyl glycolate, its preparation method and its industrial production of ethanol by hydrolysis of methyl glycolate Catalyzed reactions of acids. Background technique [0002] Glycolic acid, also known as glycolic acid, contains both carboxyl and hydroxyl groups in its molecule, and has dual properties of organic acid and alcohol. Under certain reaction conditions, glycolic acid can undergo oxidation reaction, hydrogenation reaction, polymerization reaction, and esterification reaction. Etc. Therefore, glycolic acid is an important chemical product and an intermediate product of organic synthesis. In daily life and industrial production of products, glycolic acid also has a wide range of application value and ...

Claims

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Application Information

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IPC IPC(8): B01J31/10C07C59/06C07C51/09
CPCC07C51/09B01J31/10C07C59/06Y02P20/10
Inventor 吕晓东王义成冷东斌张伟段宏毅管秀明彭慧敏刘晓林何罡
Owner 丹东明珠特种树脂有限公司
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