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Method for preparing tert-butyl acetate

A technology of tert-butyl acetate and acetic acid, which is applied in the field of preparing tert-butyl acetate, can solve the difficulties of separation and purification of tert-butyl acetate, and does not involve olefin polymerization inhibition, etc., and achieves selectivity improvement, self-polymerization inhibition, and extreme solution The effect of easy polymerization

Inactive Publication Date: 2012-03-14
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantage of this method is that the polymerization of olefins will occur in the reaction process, and its dimer will increase the difficulty of separation and purification of tert-butyl acetate
The patent does not deal with the inhibition of olefin polymerization

Method used

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  • Method for preparing tert-butyl acetate
  • Method for preparing tert-butyl acetate
  • Method for preparing tert-butyl acetate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1 does not use a polymerization inhibitor, and embodiments 2 to 4 use different single polymerization inhibitors. 90g acetic acid, 9g strong acid type ion exchange resin catalyst and 0.08g polymerization inhibitor join in the 500ml stainless steel autoclave that has cooling coil pipe, after sealing, pressurize to 1.0MPa with nitrogen and blow several times, to remove air, then in Heat the mixture to 60°C with stirring, and pressurize with nitrogen to make 166gC 4 The liquid phase feed was added to the kettle, and the pressure was increased to 1.4MPa with nitrogen, and the reaction time was 1h. Table 1 is the mixed raw material C used 4 composition, and the results are shown in Table 2.

[0023] Table 1 Raw Material C 4 composition

[0024]

[0025] Table 2 Effect of using a single polymerization inhibitor

[0026]

[0027] As can be seen from Table 2, in acetic acid and containing isobutylene C 4 In the process of synthesizing tert-butyl acetate, ...

Embodiment 5～8

[0029] Embodiments 5-8 use compounded polymerization inhibitors, which are respectively hydroquinone, benzoquinone, phenothiazine, 2,6-dinitro-p-cresol (DNPC) and piperidinol compound zj01 in a ratio of 3:1 Composite, other reaction conditions such as polymerization inhibitor adding total amount are the same as embodiment 1~4. The results are shown in Table 3.

[0030] Table 3 The use effect of compound polymerization inhibitor

[0031]

[0032] As can be seen from Table 3, in acetic acid and containing isobutylene C 4 In the process of synthesizing tert-butyl acetate, the effect of using the compounded polymerization inhibitor (Example 6) of benzoquinone and piperidinol compound zj01 is obviously better than that of using hydroquinone, phenothiazine, DNPC and piperidinol compound zj01 complex polymerization inhibitor (embodiment 5, 7 or 8).

Embodiment 9～11

[0034] Use benzoquinone and zj01 (2,2,6,6-tetramethyl-4-hydroxyl-piperidinyl oxygen free radical) composite polymerization inhibitor to compare the use effects of different proportions, and other reaction conditions are the same as in Example 1~ 4. The results are shown in Table 4.

[0035] Table 4 The effect of using different proportions of compound inhibitors

[0036]

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Abstract

The invention relates to a method for preparing tert-butyl acetate, and in particular relates to a method for preparing tert-butyl acetate based on acetic acid and isobutene-containing C4 as raw materials. The method is characterized by adding a polymerization inhibitor in a reaction process, wherein the polymerization inhibitor is a component A or a component B or a mixture of the components A and B, wherein the component A is selected from phenols, diphenols, benzoquinone and derivatives thereof or phenothiazine compounds, and the component B is a hydroxylamine compound or piperidine derivative. By adopting the method provided by the invention, the self-polymerization reaction of isobutene can be well inhibited, the selectivity of tert-butyl acetate is greatly improved, and separation process is simplified.

Description

technical field [0001] The invention relates to a method for preparing tert-butyl acetate, in particular to a method for preparing tert-butyl acetate with acetic acid and isobutylene-containing C 4 Process for the preparation of tert-butyl acetate as a starting material. Background technique [0002] Tert-butyl acetate is an excellent gasoline anti-shock agent, and can also be used as a solvent for nitrocellulose, etc. [0003] The traditional methods for producing tert-butyl acetate mainly include acid / alcohol method and acid / ene method. Compared with the acid / alcohol method, the acid / alkene method can reduce the cost of raw materials, and at the same time reduce the problems of difficult water separation and high energy consumption in the acid / alcohol process, which belongs to the green chemical process. However, the disadvantage of this method is that the polymerization of olefins will occur in the reaction process, and its dimer will increase the difficulty of separati...

Claims

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Application Information

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IPC IPC(8): C07C69/14C07C67/04C07C67/62
Inventor 王申军菅秀君潘清李玉田彭光辉
Owner CHINA PETROLEUM & CHEM CORP
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