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High-efficiency modification method of sulfonic acid resin catalyst

A high-efficiency sulfonic acid, catalyst technology, applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve problems such as being unsuitable for large-scale production, difficult to prepare methyl chloroacetate and sodium methoxide, and the like, Achieving the effect of good reactivity and extreme reactivity

Active 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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  • High-efficiency modification method of sulfonic acid resin catalyst
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  • High-efficiency modification method of sulfonic acid resin catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The mass of 10 grams of D-009B sulfonic acid tree catalyst was charged into 100 mL containing non-alcoholic solvents (methanol, ethanol, propanol, ethylene glycol, 1,3-propanediol, 2-propanol, n-butanol, n-pentanol). , isoamyl alcohol, n-hexanol, cyclohexanol, benzyl alcohol, etc.), the sulfonic acid resin catalyst was treated in the temperature range of 65-150 °C 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, respectively, and put them into the reaction kettle. 2 The air in the kettle was replaced three times under the condition of 1.0 MPa, so that the remaining air content in the kettle was less than 0.1 %, 3.0 MPa CO was introduced, and it was allowed to stand for 30 min for leak detection of the reaction kettle, and the device was emptied after ensuring that there was ...

Embodiment 2

[0043] 10 grams of different models of polystyrene sulfonic acid resin catalysts (D-009B, DA-330, D-006, D-072, Amberlyst-15, NKC-9) were loaded into a 100 mL reaction kettle containing n-hexanol solvent, Treated 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, respectively, and put them into the reaction kettle. 2 The air in the kettle was replaced three times under the condition of 1.0 MPa, so that the remaining air content in the kettle was less than 0.1 %, 3.0 MPa CO was introduced, and it was allowed to stand for 30 min for leak detection of the reaction kettle, and the device was emptied after ensuring that there was no air leakage. gas in the kettle. The stirring speed of the reaction kettle was 500 rpm, 3.0 MPa CO was introduced, and th...

Embodiment 3

[0048] Put 10 grams of D-009B catalyst into a 100 mL reaction kettle containing n-hexanol solvent, and treat 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, respectively, and put them into the reaction kettle. 2 The air in the kettle was replaced three times under the condition of 1.0 MPa, so that the remaining air content in the kettle was less than 0.1 %, 3.0 MPa CO was introduced, and it was allowed to stand for 30 min for leak detection of the reaction kettle, and the device was emptied after ensuring that there was no air leakage. gas in the kettle. The stirring speed of the reaction kettle was 500 rpm, 3.0 MPa CO was introduced, and the reaction temperature was controlled to be 110 °C, and the reaction was carried out for 6 hours. A...

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Abstract

The invention provides a high-efficiency modification method of a sulfonic acid resin catalyst, and relates to a modification method of a catalyst. The method comprises adding sulfonated polystyrene resin catalyst into a container having alcoholic solvent, introducing the gas with pressure of 0.1-20.0 MPa, and controlling the processing temperature at 50-150 DEG C and the processing time of 0.5-100.0 hours. The polar organic alcohol solvent used as a water-carrying agent and a pore-enlarging agent works together with a structural modifier of sulfonic acid resin. The method uses the polar organic alcohol solvent to heat the sulfonated polystyrene resin catalyst, and the polar organic alcohol solvent used as the water-carrying agent and the pore-enlarging agent works together with the structural modifier of sulfonic acid resin. The polar organic alcohol solvent shows good reaction activity, stability and selectivity of product methyl methoxyacetate.

Description

technical field [0001] The invention relates to a catalyst modification method, in particular to a catalyst modification method of a high-efficiency sulfonic acid resin. 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 sulfonamide-5-pyrimidine, and the catalyst for polymerization reactions. Petroleum route (from cheap and easy-to-obtain methylal as the reaction raw material, through carbonylation to synthesize high value-added MMAc) from MMAc to produce the upstream products of bulk chemical raw material ethylene glycol (through hydrogenation to generate ethylene glycol monomethyl ether) , and then through the hydrolysis reaction to generate ethylene glycol), ethylene glycol is mainly used in polyester fibers, antifreeze, unsaturated polyester resins, lubricants, plasticizers, non-ionic surfactants and explosives, co...

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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