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Tertiary butyl phenol synthesis method by methyl tertiary butyl ether alkylation reaction

A technology of methyl tert-butyl ether and tert-butyl phenol is applied in the field of preparation of tert-butyl phenol series products, which can solve the problems of large loss and industrialized application of MTBE method.

Inactive Publication Date: 2006-03-29
BC P INC CHINA NAT PETROLEUM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

From the technical process, the problem of large loss of MTBE in the reaction process is solved, so that the MTBE method can achieve the purpose of industrial application

Method used

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  • Tertiary butyl phenol synthesis method by methyl tertiary butyl ether alkylation reaction

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Experimental program
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Effect test

Embodiment 1

[0015] Attached figure 1 As shown in the double-tank reaction process, add 100g of phenolic reaction raw material phenol and catalyst to reactor 1 and 2, heat up to 80°C, start adding MTBE dropwise to reactor 1, and reactor 2 absorbs reactor 1. The volatilized trace amount of MTBE and the isobutene generated by the cracking are carried out in an alkylation reaction simultaneously. After dripping, sampling and analysis showed that the content of phenol in the alkylation solution was 0.45%, p-tert-butylphenol 18.24%, o-tert-butylphenol 1.36%, 2.6-di-tert-butylphenol 0.34%, 2.4-di-tert-butylphenol 73.58% %, 2.4.6-tri-tert-butylphenol 6.03%, alternately use one kettle to absorb another kettle reaction, after 5 cycles, the MTBE / phenol feeding (mol ratio) is 2.1 / 1 on average, and the alkylation liquid weighs 200g 1. Methanol weighs 90g, the input material is 197g+100g is 297g, and the material loss before and after is 7g.

Embodiment 2

[0019] Using the same double-tank reaction process as in Example 1, add 110 g of reaction raw material phenol and a catalyst in reactor one and two, control the temperature at 70°C to 160°C, and start to add MTBE dropwise in reactor one. The trace amount of MTBE volatilized in the first absorption reactor and the isobutene generated by the cracking are carried out simultaneously for the alkylation reaction. After dripping, sampling and analysis showed 17.35% phenol content, 4.24% o-tert-butylphenol content, 72.51% p-tert-butylphenol content, 0.58% 2.6-di-tert-butylphenol content, and 5.24% 2.4-di-tert-butylphenol content. Alternately use two kettles as the reaction kettle and the absorption kettle. After 5 cycles, the average MTBE / phenol feeding (mol ratio) is 1 / 1.07, and the average weight of each batch of alkylation liquid is 180g, and the weight of methanol is 38g. Add 220g of material, the loss is only 2g before and after.

Embodiment 3

[0023] Using the same double-tank reaction process as in Example 1, 118 g of p-cresol and a catalyst were respectively added to reactors one and two. Control the temperature at 50-100°C, add MTBE dropwise in one kettle, and absorb it in the other kettle, and do 5 batches of experiments. The average amount of MTBE added dropwise is 262ml. Sampling analysis shows that the average content of the alkylating solution is: p-cresol content 1.35%, 2-tert-butyl-4-methylphenol 35.23%, 2.6-di-tert-butyl-4-methylphenol 63.25%, other 0.17%. Alkylation liquid weighs 220g, methanol is 86g, the amount of material added is 312g, and the loss before and after is 6g.

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Abstract

The invention relates to a process for synthesizing butyl phenol through methyl butyl butyl ether alkanization, wherein a double still style reaction process flow is employed, i.e., a first autoclave is in series connection with an autoclave having the same reacting condition, which absorbs the light constituents volatilized from the first autoclave, the volatile substance is subject to secondary reaction and absorption for solving the problem of deterioration.

Description

technical field [0001] The present invention relates to a kind of preparation method of tert-butylphenol series products, especially a kind of method for synthesizing tert-butylphenol by methyl tert-butyl ether (ie MTBE) alkylation reaction. Background technique [0002] Tert-butylphenol is one of the main raw materials for hindered phenolic antioxidants or synthesized hindered phenolic antioxidants. Since such antioxidants account for a large proportion in applications, the amount of tert-butylphenol is relatively large. Big. Industrially, tert-butylphenol series products are generally prepared by using isobutylene as an alkylating agent and electrophilic substitution on the benzene ring (such as JP02221236, etc.). The use of isobutene as an alkylating agent has the following disadvantages: isobutene is easy to volatilize, is difficult to store, and is easy to cause losses during transportation; isobutene is prone to polymerization during the reaction process, generating i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/06C07C37/06
Inventor 赵义军初荣敏赖燕萍邓廷昌温金萍
Owner BC P INC CHINA NAT PETROLEUM CORP
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