Preparation method for mixture containing tert-butyl hydroperoxide

A technology containing tert-butyl hydroperoxide and tert-butyl hydroperoxide, which is applied in the preparation of peroxy compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problem of not harsh reaction conditions, waste of raw materials, damage to environment and other issues, to achieve the effect of reducing preparation costs, protecting the environment, and saving energy and raw materials

Active Publication Date: 2010-10-13
常熟市滨江化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] It should be said that compared with the isobutane oxidation method, the preparation method of tert-butanol hydrogen peroxide undoubtedly has the advantages of less harsh re...

Method used

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  • Preparation method for mixture containing tert-butyl hydroperoxide
  • Preparation method for mixture containing tert-butyl hydroperoxide
  • Preparation method for mixture containing tert-butyl hydroperoxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A) 870Kg tert-butanol (mass fraction is 85%) is joined in the first reaction device earlier, promptly joins in the esterification reaction kettle, then under stirring state and control temperature is 0~40 ℃ with 370Kg sulfuric acid (mass fraction Fraction is 80%) is added dropwise in described tert-butanol, and dropwise time is 45min, continues to stir 30min after dropwise addition, obtains tert-butyl hydrogensulfate esterified liquid;

[0028] B) Under the condition that the stirring temperature is controlled between 0 and 50°C while stirring, slowly add 515Kg hydrogen peroxide (65% by mass fraction) dropwise to the 3080Kg reuse solution (34.6% by mass fraction containing sulfuric acid, In the second reaction device (the mass fraction containing hydrogen peroxide is 5.4%), that is, in the mixing tank, the dropwise addition time is 30min, and the stirring is continued for 25min after the dropwise addition to obtain a mixed solution;

[0029] C) Under the conditions of s...

Embodiment 2

[0032] A) 350Kg sulfuric acid (mass fraction is 98%) is joined in the first reaction device earlier, promptly joins in the esterification reaction kettle, and then under stirring state and control temperature is 0~40 ℃ with 870Kg tert-butanol (mass fraction Fraction is 85%) dropwise in the described sulfuric acid, dropwise time is 60min, continue to stir 20min after dropwise addition, obtain tert-butyl hydrogensulfate esterified liquid;

[0033] B) Under the condition of stirring while controlling the stirring temperature between 0 and 50°C, slowly add 2380Kg of recycled liquid (containing 35.3% sulfuric acid by mass fraction and 5.2% hydrogen peroxide by mass fraction) into the container In the second reaction device of 650Kg hydrogen peroxide (mass fraction is 50%), i.e. in the mixing tank, the dropwise addition time is 55min, and after the dropwise addition, continue to stir for 10min to obtain a mixed solution;

[0034]C) Under the conditions of stirring and controlling th...

Embodiment 3

[0037] A) Under the condition of stirring and controlling the reaction temperature between 0 and 40°C, slowly add 270Kg sulfuric acid (90% by mass fraction) and 820Kg tert-butanol (90% by mass fraction) to the first reaction simultaneously. In the device, it is added to the esterification reaction kettle, the dropwise addition time is 30min, and the stirring is continued for 50min after the dropwise addition is completed, to obtain the tert-butyl hydrogen sulfate esterification solution;

[0038] B) under the condition of stirring while controlling the stirring temperature between 0~50°C, mix 490Kg hydrogen peroxide (mass fraction is 70%) with 3780Kg reuse liquid (the mass fraction containing sulfuric acid is 35.5%, the mass fraction containing hydrogen peroxide is 8.8%) was slowly added dropwise into the second reaction device, that is, the mixing tank, and the dropwise addition time was 40 minutes, and the stirring was continued for 30 minutes after the dropwise addition to o...

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Abstract

The invention relates to a preparation method for a mixture containing tert-butyl hydroperoxide, which belongs to the technical field of organic peroxide preparation. The method includes the following steps that: (A) tert-butyl alcohol and sulfuric acid are added into a first reactor and stirred for reaction and the reaction temperature is controlled, so that tert-butyl hydrogen sulfate esterified solution is obtained; (B) hydrogen peroxide and recycled mother solution are added into a second reactor and stirred and the stirring temperature is controlled, so that mixed solution is obtained; (C) the tert-butyl hydrogen sulfate esterified solution and the mixed solution are added into a third reactor and stirred for reaction and the reaction temperature is controlled, so that reaction product is obtained; (D) the reaction product is led into a liquid-separating tank to separate liquid, so that upper oleic-phase mixture containing the tert-butyl hydroperoxide and lower aqueous-phase mother solution containing sulfuric acid and hydrogen peroxide are obtained, moreover, the lower aqueous-phase mother solution containing the sulfuric acid and the hydrogen peroxide returns to the step B and is mixed with the hydrogen peroxide, and the upper oleic phase is the mixture containing the tert-butyl hydroperoxide. The invention prevents the discharge of industrial sewage, so that the environment is protected, and energy and materials are saved, so that the preparation cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of preparation of organic peroxides, and in particular relates to a preparation method of a mixture containing tert-butyl hydroperoxide. Background technique [0002] The English name of tert-butyl hydroperoxide is: tert-Butyl hydroperoxide (TBHP for short). Its molecular formula is: C 4 h 10 o 2 ; Molecular weight: 90.12; Structural formula: [0003] [0004] TBHP is one of the most commonly used tertiary alkyl hydroperoxides, which can be used directly or in a mixture with one or more reactants or with other compounds as an initiator for the polymerization of vinyl monomers and thermosetting polymers. Ester resin curing agent can also be widely used as a synthetic raw material for other organic peroxides as a tert-butyl peroxide introducing agent. [0005] According to patents CN200410038310.9 (Notice No. CN1286808C), CN200710099851.6 (Publication No. CN101314583A), CN 200810061607.5 (Publication N...

Claims

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Application Information

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IPC IPC(8): C07C409/04C07C407/00
Inventor 应立曹俊锋陈国华
Owner 常熟市滨江化工有限公司
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