Preparation method of solid acid material with carboxylic acid group and sulfonic acid group

A sulfonic acid group, solid acid technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of high price, thermal instability, etc., achieve easy recovery, high catalytic activity, catalytic good effect

Inactive Publication Date: 2012-08-01
SHAOXING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is a problem that it is unstable to heat and the price is too high for industrial use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation of the 1st step, monoester compound:

[0028] Weigh the hydroxysulfonic acid compound and dissolve it in ethyl acetate, the amount of ethyl acetate is 30 times the mass of the hydroxysulfonic acid compound, and the ethyl acetate solution with a mass fraction of maleic anhydride of 10% is added dropwise to the above solution, the maleic anhydride The ratio of the amount of acid anhydride to the hydroxysulfonic acid compound is 1:1, and the ethyl acetate is distilled off after being stirred for 8 hours at room temperature to obtain a monoester compound containing an ethylenic bond, a sulfonic acid group and a carboxyl group;

[0029] Step 2, the synthesis of solid acid materials with both carboxylic acid groups and sulfonic acid groups:

[0030] Dissolve the monoester compound prepared in step 1 in ethanol, the amount of ethanol is 20 times the mass of the monoester compound, add an azoisobutyronitrile initiator, the amount of the initiator is 0.5% of the ...

Embodiment 2-4

[0032] The preparation method is the same as in Example 1, the difference is that the ratio of monoester to divinylbenzene is adjusted, and the prepared solid acid material having both carboxylic acid groups and sulfonic acid groups is shown in Table 1.

[0033] Table 1: Performance comparison of solid acid materials with both carboxylic acid groups and sulfonic acid groups prepared with different ratios of monoester and divinylbenzene.

[0034] Example n(monoester) / n(divinylbenzene) Acid value / mmol / g Thermal decomposition temperature / ℃ 2 1:0.8 3.2 203 3 1:1.2 2.4 190 4 1:1.8 2.1 208

[0035] .

[0036] 2. Application examples.

[0037] The solid acid material having both carboxylic acid groups and sulfonic acid groups prepared in Example 1 was used to catalyze esterification reaction, condensation reaction, alkylation reaction and etherification reaction respectively, and the following examples were obtained.

Embodiment 5

[0038] Embodiment 5, catalytic esterification reaction:

[0039] Add 0.1mol citric acid and 0.45mol n-butanol to a 100mL three-necked bottle equipped with electromagnetic stirring, a thermometer, a reflux condenser, and a water separator for heating and stirring. After the citric acid is completely dissolved, take a sample to measure the acidity, and then add the 1 Prepared catalyst 0.25g, heated to reflux and stirred, the water produced by the reaction was separated from the water separator, reacted for 4 hours, and the calculated yield was 98.6%.

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Abstract

The invention discloses a preparation method of a solid acid material with carboxylic acid group and sulfonic acid group and belongs to the technical field of organic chemosynthesis. The preparation method is characterized in that a hydroxy sulfonate compound reacts with maleic anhydride to obtain a monoester compound containing olefinic link, sulfonic acid group and carboxyl group; the monoester compound is self-polymerized to form an oligomer; and then the oligomer is co-polymerized with divinyl benzene to form the solid acid material with the carboxylic acid group and the sulfonic acid group. The solid acid material with the carboxylic acid group and the sulfonic acid group, prepared by the invention has the advantages that the thermal stability is high, the catalysis effect is good, and accelerant can be used repeatedly.

Description

Technical field: [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for preparing a solid acid material having both carboxylic acid groups and sulfonic acid groups. Background technique: [0002] In today's crisis of energy problems and environmental problems, it has become the goal of modern chemical industry to efficiently generate target products with a small amount of energy without producing unnecessary by-products. Acid catalysts are indispensable in the modern chemical industry and are widely used in the manufacture of various products such as pharmaceuticals, petrochemical products, and polymer products. However, most of the currently used liquid acid catalysts are hydrochloric acid and sulfuric acid. . The liquid catalyst used in the production process needs to be neutralized by alkali, and separated and recovered from the product by removing the salt generated by neutralization. However, a considerable amo...

Claims

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Application Information

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IPC IPC(8): C08F212/36C08F220/38B01J31/06C07C69/704C07C67/08C07C43/20C07C41/09C07C39/08C07C37/16
Inventor 梁学正
Owner SHAOXING UNIVERSITY
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