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A novel solid catalyst and its application in the preparation of 2,4-dimethyl-6-tert-butylphenol

A solid catalyst and a new type of technology, applied in catalytic reactions, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve the problems of insufficient consideration of the proportioning relationship, difficult recycling, difficult processing, etc., and achieve enhanced adhesion. The effect of focusing force and adhesion, excellent chemical stability, improving catalytic performance

Active Publication Date: 2022-07-15
浙江赛迅环保科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, heteropolyacid compounds are prone to partial dissolution after reaction, and are not easy to recycle; cation exchange resins have swelled and broken during the catalytic organic reaction process; zeolite molecular sieves have disadvantages such as limited acid strength and acid content.
[0004] CN101631614A discloses a solid acid alkylation catalyst, the solid acid catalyst includes a multi-metal component that performs a hydrogenation function, and is used to regenerate the catalyst in the presence of hydrogen, but the multi-metal includes noble metals such as palladium, platinum, etc. It adopts cheap precious metals to alleviate the cost pressure, but the precious metals platinum and palladium are still necessary components, and the ratio relationship of various cheap metals is not considered too much; CN106179468B discloses a solid acid catalyst, using two A non-precious metal is matched in a specific ratio to completely replace the precious metal. When it is applied to the alkylation reaction, it can approach or even reach the reaction performance of a fresh alkylation catalyst covered with a precious metal, and it has a cost advantage. And processing requirements are strict, it is difficult to apply to industrial production
[0005] Polytetrafluoroethylene (PTFE) is a highly crystalline polymer of tetrafluoroethylene (TFE) monomer. It is a white waxy thermoplastic. In PTFE, due to the replacement of hydrogen atoms by fluorine atoms, carbon-carbon The chain is gradually reversed from the planar, fully stretched zigzag conformation of polyethylene to the helical conformation of PTFE, which makes the main chain of the polymer free from any external reagents, and makes PTFE have solvent resistance and chemical stability unmatched by other materials. properties, low cohesive energy density, thermal stability, and low intermolecular attraction and surface energy of PTFE, so that PTFE has a very low surface friction coefficient and good ductility at low temperature. These characteristics make PTFE a It is an ideal material for solid acid catalyst carrier; but at the same time, PTFE has poor creep resistance, is prone to cold flow phenomenon, and has high crystallinity, making it difficult to process. This is also the reason why there are few studies on PTFE as a solid acid catalyst. one

Method used

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  • A novel solid catalyst and its application in the preparation of 2,4-dimethyl-6-tert-butylphenol
  • A novel solid catalyst and its application in the preparation of 2,4-dimethyl-6-tert-butylphenol
  • A novel solid catalyst and its application in the preparation of 2,4-dimethyl-6-tert-butylphenol

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Experimental program
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Effect test

Embodiment 1

[0025] A preparation method of 2,4-dimethyl-6-tert-butylphenol, using 2,4-dimethylphenol and isobutylene as raw materials, catalyzed by a solid acid catalyst, to prepare 2,4-dimethyl-6-tert-butyl phenol.

[0026] The preparation method of the solid acid catalyst is as follows:

[0027] (1) Disperse 5g of graphite powder in 100ml of N-methylpyrrolidone (NMP), ultrasonically disperse it in a low-power ultrasonic device for 8h, and then centrifuge the obtained dispersion at 4000r / min for 10min to remove the unexfoliated graphite powder , to obtain graphene / N-methylpyrrolidone dispersion;

[0028] (2) Take 50ml, 0.5mg / ml of graphene / N-methylpyrrolidone dispersion, add styrene, ultrasonically disperse under low power for 3h, then add azobisisobutyronitrile, azobisisobutyronitrile and benzene The mass ratio of ethylene is 1:200, and the heating reaction is carried out for 40h under nitrogen atmosphere and mechanical stirring conditions;

[0029] (3) The product obtained after the...

Embodiment 2

[0037] A preparation method of 2,4-dimethyl-6-tert-butylphenol, using 2,4-dimethylphenol and isobutylene as raw materials, catalyzed by a solid acid catalyst, to prepare 2,4-dimethyl-6-tert-butyl phenol.

[0038] The preparation method of the solid acid catalyst is as follows:

[0039] (1) Disperse 5g of graphite powder in 100ml of N-methylpyrrolidone (NMP), ultrasonically disperse it in a low-power ultrasonic device for 8h, and then centrifuge the obtained dispersion at 4000r / min for 10min to remove the unexfoliated graphite powder , to obtain graphene / N-methylpyrrolidone dispersion;

[0040] (2) Take 80ml, 0.5mg / ml graphene / N-methylpyrrolidone dispersion, add NDZ-401 with a concentration of 1.0wt%, ultrasonically disperse for 3h under low power, then add azobisisobutyronitrile, The mass ratio of azobisisobutyronitrile to NDZ-401 is 1:200, and the heating reaction is carried out for 40h under nitrogen atmosphere and mechanical stirring conditions;

[0041] (3) The product ...

Embodiment 3

[0048] A preparation method of 2,4-dimethyl-6-tert-butylphenol, using 2,4-dimethylphenol and isobutylene as raw materials, catalyzed by a solid acid catalyst, to prepare 2,4-dimethyl-6-tert-butyl phenol.

[0049] The preparation method of the solid acid catalyst is as follows:

[0050] (1) Disperse 10g of graphite powder in 150ml of N-methylpyrrolidone (NMP), ultrasonically disperse it in a low-power ultrasonic device for 12h, and then centrifuge the obtained dispersion for 10min at 4200r / min to remove the unexfoliated graphite powder , to obtain graphene / N-methylpyrrolidone dispersion;

[0051] (2) Take 100ml, 0.5mg / ml of graphene / N-methylpyrrolidone dispersion, add KH560, ultrasonically disperse for 3h under low power, then add azobisisobutyronitrile, the mixture of azobisisobutyronitrile and KH560. The mass ratio is 1:200, and the heating reaction is carried out for 40h under the condition of nitrogen atmosphere and mechanical stirring;

[0052] (3) The product obtained ...

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Abstract

A novel solid catalyst comprises a polytetrafluoroethylene composite carrier modified by styrene grafting and a catalytic active center with a sulfonic acid group as an acid center supported on the carrier. The solid catalyst prepared by the method is applied to In the reaction of catalyzing 2,4 dimethyl-6 tert-butylphenol, because the prepared solid catalyst itself has stable performance and strong catalytic activity, the reaction conversion rate of preparing 2,4 dimethyl-6 tert-butylphenol is high, and the reaction The time is short and the reaction temperature requirement is relatively low, which is favorable for the preparation of 2,4-dimethyl-6-tert-butylphenol.

Description

technical field [0001] The invention belongs to the technical field of chemical reagent synthesis, in particular to a novel solid catalyst and its application in preparing 2,4-dimethyl-6-tert-butylphenol. Background technique [0002] 2,4-Dimethyl-6-tert-butylphenol is a substance that can quickly react with free radicals to terminate the chain reaction. It is a new type of high temperature resistant aviation fuel antioxidant, acrylic acid polymerization inhibitor, also known as stabilizer. , is an intermediate of a variety of polymer antioxidants, but also a very important pharmaceutical intermediate. The alkylating reagents for the production of tert-butylphenol at home and abroad mainly include isobutylene, tert-butyl alcohol and methyl tert-butyl ether. Among them, tert-butyl alcohol as a reagent will generate a large amount of waste water, and methyl tert-butyl ether is the next step product of isobutylene. In terms of reaction effect, isobutene is used as an alkylatin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/10B01J35/10C07C37/14C07C39/06
CPCB01J31/10C07C37/14B01J2231/32B01J35/61C07C39/06
Inventor 徐志梁罗良罗文春施亦斐
Owner 浙江赛迅环保科技有限公司
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