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Method for treating polystyrene sulfonic acid resin catalyst by using ester solvent

A polystyrene sulfonic acid and catalyst technology, applied in 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, etc. problems, to achieve the best reactivity, extremely reactivity effect

Inactive Publication Date: 2016-08-10
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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  • Method for treating polystyrene sulfonic acid resin catalyst by using ester solvent
  • Method for treating polystyrene sulfonic acid resin catalyst by using ester solvent
  • Method for treating polystyrene sulfonic acid resin catalyst by using ester solvent

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Put 10 grams of NKC-9 sulfonic acid resin catalyst into 100 mL containing insoluble ester solvent (methyl formate, ethyl formate, methyl acetate, methyl propionate, ethyl propionate, n-propyl formate, isoformate Propyl ester, ethyl methoxyacetate, methyl benzoate, etc.) in the reaction kettle, treat the sulfonic acid resin catalyst in the temperature range of 35-150 ℃ 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 ke...

Embodiment 2

[0043] 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

[0048] 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

The invention provides a method for treating a polystyrene sulfonic acid resin catalyst by using an ester solvent, and relates to a method for treating resin catalyst. The method includes the following steps: adding polystyrene sulfonic acid resin catalyst into a container containing ester solvent, introducing gas with the pressure of 0.1-20.0 MPa, and controlling the processing temperature at 35-150 DEG C and the processing time for 0.5-20.0 h. The polar organic ester solvent is used as a water-carrying agent and a pore-enlarging agent works together with a structural modifier of sulfonic acid resin, and the catalyst is a resin-type catalyst containing sulfonic acid functional group which is one or mixing multiple of D-009B, DA-330, NKC-9, D-006, Amberlyst-15, and D-072. The method uses polar organic ester solvent to heat the polystyrene sulfonic acid resin catalyst, and the treated sulfonic acid resin catalyst is used for methylal carbonylation reaction. Compared with the sulfonic acid resin catalyst untreated by the ester, the treated catalyst has good reaction activity, stability and selectivity of the products methoxyacetic acid methyl ester.

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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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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