A kind of efficient sulfonic acid resin catalyst modification method

Active Publication Date: 2018-09-11
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 efficient sulfonic acid resin catalyst modification method
  • A kind of efficient sulfonic acid resin catalyst modification method
  • A kind of efficient sulfonic acid resin catalyst modification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Put 10 grams of D-009B sulfonic acid tree catalyst into 100 mL containing different alcohol solvents (methanol, ethanol, propanol, ethylene glycol, 1,3-propanediol, 2-propanol, n-butanol, n-pentanol , isoamyl alcohol, n-hexanol, cyclohexanol, benzyl alcohol, etc.) in the reaction kettle, treat the sulfonic acid resin catalyst in the temperature range of 65-150 ℃ for 1-7 h. The treated catalyst was filtered and 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 stirr...

Embodiment 2

[0043] The polystyrene sulfonic acid resin catalyst (D-009B, DA-330, D-006, D-072, Amberlyst-15, NKC-9) of 10 grams of different models is packed in the reaction kettle that 100mL contains n-hexanol solvent, Treat at 100-150°C, 3.0 MPa, CO atmosphere for 6 h. The treated catalyst was filtered and 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 stirring speed of the reactor was 500 rpm, 3.0 MPa CO was introduced, the reaction temperature was controlled at 110 °C, and the...

Embodiment 3

[0048] Put 10 grams of D-009B catalyst into a 100 mL reaction kettle containing n-hexanol solvent, and treat it at 110 °C, 3.0 MPa, and CO atmosphere for 0.5-20 h. The treated catalyst was filtered and 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 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 after the reaction, filter ...

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Abstract

A high-efficiency sulfonic acid resin catalyst modification method, relates to a catalyst modification method, the method includes the following process: polystyrene sulfonic acid resin catalyst is added to a container equipped with an alcohol solvent, and 0.1-20.0 MPa is passed through Pressure gas, controlled treatment temperature 50-150°C, treatment time 0.5-100.0 h, polar organic alcohol solvent simultaneously acts as water-carrying agent, pore-enlarging agent and structural modifier of sulfonic acid resin. The present invention adopts polar organic alcohol solvent to heat-treat the polystyrene sulfonic acid resin catalyst, and the polar organic alcohol solvent acts together as a water-carrying agent, a pore-enlarging agent and a structural modifier of the sulfonic acid resin, showing excellent performance. The reactivity, stability and selectivity of the product methyl methoxyacetate.

Description

technical field [0001] The invention relates to a catalyst modification method, in particular to a high-efficiency sulfonic acid resin catalyst modification method. 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 explosives, coatings, inks,...

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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