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Method for synthesizing 2, 6-di-tert-butylphenol by using environment-friendly heterogeneous catalyst

A technology of di-tert-butylphenol and heterogeneous catalysts, applied in chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve problems such as complex operation, unstable pressure, and difficult separation. Achieve the effects of simple preparation process, stable reaction pressure, and improved economic benefits

Inactive Publication Date: 2021-03-30
南京晶典抗氧化技术研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Existing 2,6-di-tert-butylphenol is widely used in industry, and there are many kinds of preparation technology research about 2,6-di-tert-butylphenol, as patent CN1935764A discloses a kind of 2,6-di-tert-butylphenol The preparation method of butylphenol alkylation liquid uses aluminum powder as a catalyst to catalyze the reaction of phenol and isobutylene. The conversion rate of phenol in this method is above 85%, and the product yield can reach 80%. However, the reaction system is a high-pressure reaction, and the reaction In the process, the pressure is unstable, the process operation difficulty coefficient is relatively large, and the reaction waste liquid treatment is difficult, and the environmental protection cost is high; the patent CN 108503513A discloses a preparation method of 2,6-di-tert-butylphenol, which uses triisobutylaluminum With aluminum trichloride as a catalyst, it catalyzes the reaction of phenol with isobutylene or isobutylamine, and the final product yield can reach 98.5%.
The preparation method has mild reaction conditions, high product yield, and low possibility of forming by-products, but the reaction needs to undergo multi-step temperature rise and fall, the process is cumbersome, the operation is complicated, and waste water containing metal ions is generated at the same time, which has a greater pollution effect on the environment; Patent CN 102906059B discloses a method for producing 2,6-di-tert-butylphenol, using alumina as a catalyst, phenol and C4 raffinate stream containing isobutene and 1-butene or 2-butene in the 70°C-130°C, under the reaction conditions of normal pressure, the source of the reaction raw material is easy to obtain, but the reaction conversion rate is not high, the composition of the reaction solution is complicated, and the subsequent separation is difficult; patent CN 1844071A This patent provides the preparation of high selectivity 2 , a new method for 6-di-tert-butylphenol, the reaction of phenols with isobutene in the presence of triphenoxyaluminum catalyst
The reaction is performed under high temperature and high pressure, and the reaction yield can reach more than 80%. The reaction has good selectivity, but the catalyst is easily soluble in the reaction solution, and the follow-up treatment costs are high, and metal ion wastewater is easily generated, and the environmental protection cost is high.

Method used

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  • Method for synthesizing 2, 6-di-tert-butylphenol by using environment-friendly heterogeneous catalyst
  • Method for synthesizing 2, 6-di-tert-butylphenol by using environment-friendly heterogeneous catalyst
  • Method for synthesizing 2, 6-di-tert-butylphenol by using environment-friendly heterogeneous catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Such as figure 2 In the process flow shown, take 4kg CD650 resin catalyst and spread it in the No. 1 reactor. The raw material of tert-butanol enters the No. 1 reactor and heats up to 100°C. After catalysis, the reacted liquid enters the cooler and cools The liquid enters the first-stage packing rectification tower, the height of the first-stage packing rectification tower is about 2.5m, the tower diameter is 0.2m, the reflux ratio is 3, the main packing is Raschig ring, and the tert-butanol from the top of the tower is refluxed into No. reactor. The gaseous state in the cooler enters the secondary packing rectification tower, the height of the secondary packing rectification tower is about 2m, the tower diameter is 0.2m, the reflux ratio is 3, the main packing is Raschig ring, and the isobutene product comes out from the top of the tower, the purity reaches 99.99%; about 5kg of ZGC-111 resin solid acid catalyst is laid in the fixed bed reactor, and the isobutene and ...

Embodiment 2

[0045] Such as figure 2 In the process flow shown, take 4kg CD650 resin catalyst and spread it in the No. 1 reactor. The raw material of tert-butanol enters the No. 1 reactor and heats up to 100°C. After catalysis, the reacted liquid enters the cooler and cools The liquid enters the first-stage packing rectification tower, the height of the first-stage packing rectification tower is about 2.5m, the tower diameter is 0.2m, the reflux ratio is 3, the main packing is Raschig ring, and the tert-butanol from the top of the tower is refluxed into No. reactor. The gaseous state in the cooler enters the secondary packing rectification tower, the height of the secondary packing rectification tower is about 2m, the tower diameter is 0.2m, the reflux ratio is 3, the main packing is Raschig ring, and the isobutene product comes out from the top of the tower, the purity reaches 99.99%; about 5kg of CS-N-001 solid acid catalyst is laid in the fixed bed reactor, and the isobutene and pheno...

Embodiment 3

[0047] Such as figure 2In the process flow shown, take 4kg CD550 type resin catalyst and lay it in the No. 1 reactor. The tert-butanol raw material enters the No. 1 reactor. After catalysis, the reacted reaction liquid enters the cooler, and the cooling liquid enters the primary packing. In the rectification tower, the height of the primary packing rectification tower is about 2.5m, the tower diameter is 0.2m, the reflux ratio is 3, the main filler is Raschig ring, and the tert-butanol is refluxed into the No. 1 reactor from the top of the tower. The gaseous state in the cooler enters the secondary packing rectification tower, the height of the secondary packing rectification tower is about 2m, the tower diameter is 0.2m, the reflux ratio is 3, the main packing is Raschig ring, and the isobutene product comes out from the top of the tower, the purity reaches 99.99%; about 5kg of CS-001 resin solid acid catalyst is laid in the fixed bed reactor, and the isobutene and phenol de...

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Abstract

The embodiment of the invention discloses a method for synthesizing 2, 6-di-tert-butylphenol by using an environment-friendly heterogeneous catalyst in the technical field of chemical synthesis, whichcomprises the following steps: S1, introducing a reaction raw material tert-butyl alcohol from a feed port at the top end of a reactor I through a feed pump, adding a solid acid catalyst into the reactor I, and carrying out dehydration reaction to generate an isobutene solution; s2, conveying the reaction liquid into a cooler from a discharge port in the top end of the reactor for cooling, and conveying the obtained cooling liquid into a primary rectifying tower for rectification; the preparation process is simple, the reaction pressure is stable, a heterogeneous catalyst reaction system is introduced, a novel heterogeneous catalyst is used for replacing an L acid or aluminum salt homogeneous catalyst in an original production process, According to the characteristics of the novel heterogeneous catalyst, a 2, 6-di-tert-butylphenol synthesis reaction unit and a separation unit are subjected to process optimization design, so that the yield of 2, 6-di-tert-butylphenol is improved. The purposes of simplifying the process, saving energy and protecting the environment are achieved, economic benefits are improved, and the requirement for large-scale industrial green production is met.

Description

technical field [0001] The embodiment of the present invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing 2,6-di-tert-butylphenol with an environment-friendly heterogeneous catalyst. Background technique [0002] 2,6-Di-tert-butylphenol, English name 2DTBP, molecular formula C14H22O, soluble in caustic lye and common organic solvents such as ethanol. 2,6-Di-tert-butylphenol is used to prepare hindered phenolic antioxidants, rubber anti-aging agents, cresol-formaldehyde resins and plasticizers. It can be used as a disinfectant in medicine and also used as a surfactant to manufacture many An excellent antioxidant and light stabilizer, it can also be used in the manufacture of natural rubber and synthetic plastic antioxidants, fuel stabilizers, ultraviolet absorbers, pesticides, dye intermediates, etc. [0003] Existing 2,6-di-tert-butylphenol is widely used in industry, and there are many kinds of preparation technology re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/06C07C37/14C07C37/74C07C11/09C07C1/24C07C7/04B01J31/06
CPCC07C37/14C07C37/74C07C1/24C07C7/04B01J31/06B01J2231/32C07C11/09C07C39/06Y02P20/10
Inventor 刘定华马江涛居海军郑鑫
Owner 南京晶典抗氧化技术研究院有限公司
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