A kind of method utilizing ester solvent to process polystyrene sulfonic acid resin catalyst

A polystyrene sulfonic acid and ester solvent technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, catalyst activation/preparation, etc., can solve the difficulties in the preparation of methyl chloroacetate and sodium methoxide, which are not suitable for large-scale production and other issues to achieve the best reactivity effect

Inactive Publication Date: 2018-08-07
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] But two kinds of raw materials methyl chloroacetate and sodium methylate of this method are difficult to prepare, are not suitable for large-scale production

Method used

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  • A kind of method utilizing ester solvent to process polystyrene sulfonic acid resin catalyst
  • A kind of method utilizing ester solvent to process polystyrene sulfonic acid resin catalyst
  • A kind of method utilizing ester solvent to process polystyrene sulfonic acid resin catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Put 10 grams of NKC-9 sulfonic acid resin catalyst into 100 mL containing ester solvent (methyl formate, ethyl formate, methyl acetate, methyl propionate, ethyl propionate, n-propyl formate, isopropyl formate Esters, ethyl methoxyacetate, methyl benzoate, etc.) in the reactor, in the temperature range of 35-150 ℃ to treat the sulfonic acid resin catalyst for 1-7 h. After the treated catalyst was filtered, it was dried in an oven at 120 °C for 6 h. The evaluation conditions of the catalyst were as follows: Weigh 30 mL of DMM, 30 mL of 1,4-dioxane solvent, and 1 g of the modified sulfonic acid resin catalyst into the reaction kettle respectively, and use N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is less than 0.1 %, pass in 3.0 MPa CO, let it stand for 30 minutes, and use it for leak detection of the reactor to ensure that the device is airtight and then emptied Gas in the kettle. The sti...

Embodiment 2

[0040] Put 10 grams of different types of polystyrene sulfonic acid resin catalysts (D-009B, DA-330, D-006, D-072, Amberlyst-15, NKC-9) into a 100mL reaction kettle containing methyl benzoate solvent , at 100-150°C, 5.0 MPa, and CO atmosphere for 6 h. After the treated catalyst was filtered, it was dried in an oven at 120 °C for 6 h. The evaluation conditions of the catalyst were as follows: Weigh 30 mL of DMM, 30 mL of 1,4-dioxane solvent, and 1 g of the modified sulfonic acid resin catalyst, and add them to the reaction kettle respectively, and use N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is less than 0.1%, pass in 3.0 MPa CO, let it stand for 30 minutes, and use it for leak detection of the reactor to ensure that the device is not leaking and then emptied Gas in the kettle. The stirring speed of the reactor was 500 rpm, 3.0 MPa CO was introduced, the reaction temperature was controlled at...

Embodiment 3

[0045] Put 10 grams of DA-330 catalyst into a 100 mL reaction kettle containing methyl benzoate solvent, and treat it at 110 °C, 5.0 MPa, and CO atmosphere for 0.5-20 h. After the treated catalyst was filtered, it was dried in an oven at 120 °C for 6 h. The evaluation conditions of the catalyst were as follows: Weigh 30 mL of DMM, 30 mL of 1,4-dioxane solvent, and 1 g of the modified sulfonic acid resin catalyst, and add them to the reaction kettle respectively, and use N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is less than 0.1 %, pass in 3.0 MPa CO, let it stand for 30 minutes, and use it for leak detection of the reactor to ensure that the device is airtight and then emptied Gas in the kettle. The stirring speed of the reactor was 500 rpm, 3.0 MPa CO was introduced, the reaction temperature was controlled at 110 °C, and the reaction was carried out for 6 hours. Cool down to room temperature...

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Abstract

A method of utilizing an ester solvent to process a polystyrene sulfonic acid resin catalyst relates to a method for processing a resin catalyst, the method comprising the following steps: adding a polystyrene sulfonic acid resin catalyst to a container containing an ester solvent, Introduce a gas with a pressure of 0.1-20.0 MPa, control the treatment temperature at 35-150°C, and the treatment time at 0.5-20.0 h. The polar organic ester solvent is also used as a water-carrying agent, a pore-enlarging agent and a structural modifier of the sulfonic acid resin. It works; the catalyst is a resin catalyst containing sulfonic acid functional groups, which is one or more mixtures of D-009B, DA-330, NKC-9, D-006, Amberlyst-15, and D-072. The method of the present invention adopts polar organic ester solvent heat treatment polystyrene sulfonic acid resin catalyst, and after the treatment, the sulfonic acid resin catalyst is used for methylal carbonylation reaction, and compared with the sulfonic acid resin catalyst that has not been treated with ester, it shows extremely Excellent reactivity, stability and selectivity to methyl methoxyacetate.

Description

technical field [0001] The invention relates to a method for processing resin catalysts, in particular to a method for processing polystyrene sulfonic acid resin catalysts with ester solvents. Background technique [0002] Methyl methoxyacetate (MMAc) is an important organic chemical raw material, which can be used for the kinetic resolution of chiral amine compounds, the synthesis of vitamin B6 and sulfa-5-pyrimidine, and the catalyst for polymerization reactions; Petroleum route (use cheap and easy-to-obtain methylal as the reaction raw material, synthesize high value-added MMAc through carbonylation reaction) produce the upstream product of ethylene glycol, a bulk chemical raw material, from MMAc (generate ethylene glycol monomethyl ether through hydrogenation reaction , and then generate ethylene glycol through hydrolysis reaction), ethylene glycol is mainly used in polyester fiber, antifreeze, unsaturated polyester resin, lubricant, plasticizer, non-ionic surfactant and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/10C07C67/36C07C69/708
CPCB01J31/10B01J37/0009C07C67/36C07C69/708
Inventor 石磊张婉莹孙东陈飞张晓东
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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