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Green and efficient heterogeneous catalyst for compounding 2,4-di-tert-butylphenol

A di-tert-butylphenol and heterogeneous catalyst technology, applied in the chemical industry, can solve the problems of high corrosion, easy pollution, high reaction temperature, etc., and achieve the effects of reducing operating costs, simplifying the production process, and stabilizing catalytic performance

Inactive Publication Date: 2017-07-25
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, sulfuric acid, perchloric acid, and p-toluenesulfonic acid in the above-mentioned catalysts are highly corrosive to equipment and dangerous to use; in the catalytic reaction of anhydrous aluminum trichloride, the selectivity of 2,4-di-tert-butylphenol is not good. High; the reaction temperature required in the γ-alumina catalytic reaction is high, which is not conducive to operation; the activated clay catalyst cannot be recycled, and a large amount of waste is generated. The separation process is time-consuming and laborious and easily causes pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment １

[0017] 40wt% styrene monomer, 7wt% dipropenylbenzene copolymerized crosslinking monomer, 3wt% azobisisobutyronitrile initiator, 8wt% acetone esterified modified nano-CaCO 3 Materials, 12wt% toluene porogen and 30wt% petroleum ether solvent are formulated into oil phase solution A; pure water, Arabic dispersant and iron oxide dispersant are formulated into water phase solution B at a mass ratio of 100:2:1.8. Then the oil phase solution A and the water phase solution B were mixed according to the mass ratio of 1:2.4, vigorously stirred at 80°C for 6 hours, filtered and washed to obtain polymer microspheres containing modified porous nanomaterials; then steam distillation was used The porogen and residual monomers were removed at 95°C, and the obtained porous resin bulk white ball was stirred in 2% hydrochloric acid at 50°C for 5 h, washed with water, filtered, and dried to obtain the bulk resin microspheres containing nanopores. ball.

[0018] According to the mass ratio of 100...

Embodiment ２

[0020] After preheating at 78°C, 2000 kg of phenol was fed into the tank reactor in the form of fluid, and 30 kg of the solid acid resin catalyst obtained in Example 1 was added, and stirred for 20 min. 1790 kg of isobutylene was introduced at a rate of 800 kg / h, and the temperature of the reaction system was set at 95°C. When the temperature was higher than 95°C, high-speed circulating cooling water was used to cool down. After the isobutene was completely introduced, the reaction system was kept warm for 60 min. After the reaction was completed, the catalyst was kept in the reactor, and then the 2,4-di-tert-butylphenol was alkylated and squeezed out, and the content of 2,4-di-tert-butylphenol was analyzed to be 70.65%.

Embodiment ３

[0022] After preheating at 78°C, 3000 kg of phenol was fed into the tank reactor in the form of fluid, and 45 kg of the solid acid resin catalyst obtained in Example 1 was added, and stirred for 20 min. 3040 kg of isobutylene was introduced at a rate of 800 kg / h, and the temperature of the reaction system was set at 97°C. When the temperature was higher than 97°C, high-speed circulating cooling water was used to cool down. After isobutene was completely introduced, the reaction system was kept warm for 30 min. After the reaction was completed, the catalyst was kept in the reactor, and then the 2,4-di-tert-butylphenol was alkylated and squeezed out, and the content of 2,4-di-tert-butylphenol was analyzed to be 72.58%.

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Abstract

The invention relates to a green and efficient heterogeneous catalyst for compounding 2,4-di-tert-butylphenol. The catalyst is a porous solid acid resin catalyst with high specific surface area. Phenol and isobutene are taken as reaction raw materials for producing 2,4-di-tert-butylphenol under a catalytic effect of the nontoxic harmless green solid acid resin catalyst. The catalyst provided by the invention is used for replacing a carclazyte catalyst in the present production, can be repeatedly reused, has the characteristics of long service life, is capable of greatly reducing the production cost of the catalyst, is capable of greatly reducing the solid waste generated by disposable use of the carclazyte catalyst and can realize the greening of the production process. Meanwhile, the heterogeneous catalyst for compounding 2,4-di-tert-butylphenol provided by the invention is simply separated, recycled and reused, the separating time of the present carclazyte catalyst is greatly shortened and the production efficiency is obviously increased.

Description

technical field [0001] The invention relates to a green and efficient heterogeneous catalyst for synthesizing 2,4-di-tert-butylphenol, which belongs to the field of chemical industry. Background technique [0002] 2,4-Di-tert-butylphenol is an important chemical intermediate, widely used in the preparation of natural rubber, plastic antioxidant, synthetic rubber antioxidant, fuel stabilizer and dye intermediates. At present, the catalysts used to catalyze the reaction of phenol with isobutanol or isobutene to produce 2,4-di-tert-butylphenol mainly include sulfuric acid, perchloric acid, p-toluenesulfonic acid, anhydrous aluminum trichloride, γ- Alumina, activated clay, etc. For example, Chinese Patent Publication No. CN1935763A, date of publication is March 28, 2007, and the name of the invention is a preparation method of 2,4-di-tert-butylphenol alkylation liquid. The invention uses montmorillonite (including attapulgite) ) as a catalyst, 2,4-di-tert-butylphenol alkylatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C37/14C07C39/06
CPCC07C37/14B01J31/06B01J35/615B01J35/635C07C39/06Y02P20/52Y02P20/584
Inventor 朱志荣赵国庆
Owner TONGJI UNIV
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