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Preparation method of solid-acid catalyst

A technology of solid acid catalyst and compound, which is applied in the field of preparation of solid acid catalyst, can solve the problems of thermal instability and high price, and achieve the effects of high thermal stability, low cost and wide application prospects

Inactive Publication Date: 2010-07-28
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

[0025] Embodiment 1, the synthesis of novel carbon-based solid acid:

[0026] The 1st step, the synthetic reaction of novel carbon-based solid acid: in the 100mL three-neck bottle that is equipped with electromagnetic stirring, thermometer, reflux condenser, water trap, add 0.05mol2,3-dimercaptoethylthiopropanethiol ( 0.15mol mercapto) and 0.05mol toluene diisocyanate (0.10mol NCO) were heated and stirred, and condensation reaction was carried out at 100°C for 24 hours to obtain a light yellow solid;

[0027] Step 2, synthesis of solid acid catalyst: mix polythiourea resin and 5% hydrogen peroxide solution according to the ratio of hydrogen peroxide and free mercapto to 2, stir at room temperature for 24 hours, and filter until the filtrate After clarification, until there is no sulfuric acid test, the catalyst is dried in an oven at 120° C. for 1 day, and the acid value of the catalyst is 2.0 mmol / g.

Embodiment 2-4

[0029] Except for the following differences, the rest are the same as in Example 1, heated and stirred at 0.05mol2,3-dimercaptoethylthiopropanethiol (0.15molmercapto), and condensed toluene diisocyanate at 100°C according to the ratio in Table 1 Dosage, reaction 24h.

[0030] Table 1

[0031] Example

Embodiment 5-12

[0033] Except following difference, all the other are with embodiment 1, and the influence result of different reactants is shown in Table 2.

[0034] Table 2

[0035] Example

[0036] Example

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PUM

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Abstract

The invention discloses a preparation method of a solid-acid catalyst, belonging to the technical field of chemosynthesis. The method comprises the following steps: selecting a polythiol compound to react with a polyisocyanates compound to obtain polythiocarbamide resin with free sulfhydryl; oxidizing the polythiocarbamide resin by hydrogen peroxide; and converting the sulfhydryl into a sulfo group so as to obtain sulfo group functionalized polythiourea resin, i.e. the novel solid-acid catalyst. The solid-acid catalyst has the advantages that the thermostability is high, and the thermal decomposition temperature is above 150 DEG C; the acid value is high, wherein the acid value is more than 1-6mmol / g; the synthetic cost is low; the catalytic effect is good; the solid-acid catalyst has high catalytic activity in common acid catalyzed reactions such as esterification, condensation, alkylate, etherification, ester exchange and the like; and the solid-acid catalyst can be reused for many times.

Description

technical field [0001] The invention relates to a preparation method of a solid acid catalyst, which belongs to the technical field of organic chemical synthesis. 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 amount of energy is consumed in the above neutralization and sal...

Claims

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Application Information

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IPC IPC(8): B01J31/10B01J35/02C07C69/704C07C67/08C07D317/72C07C39/08C07C37/16C07C43/205C07C41/09C11C3/10
Inventor 齐陈泽肖慧泉杜轶君沈永淼
Owner SHAOXING UNIVERSITY
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