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Preparation of tert-butyl hydrogen peroxide and di-tert-butyl peroxide

A technology of di-tert-butyl peroxide and tert-butyl hydroperoxide, applied in the direction of organic chemistry, can solve the problems of high production cost, low yield, long process route, etc., and achieve environmental protection, high yield, The effect of reducing production costs

Active Publication Date: 2008-11-05
ZHEJIANG JINKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Among the production methods of large-scale industrial production of tert-butyl peroxide at present, the hydrogen peroxide reaction method is in the majority, but this method has a long process route, high production cost and low yield

Method used

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  • Preparation of tert-butyl hydrogen peroxide and di-tert-butyl peroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Mix 100g of 35% hydrogen peroxide, 30g of 98% sulfuric acid, 0.5g of phosphotungstic acid, 2g of ethylenediaminetetramethylenephosphonic acid, and 2g of hydroxyethylidenediphosphonic acid at 15°C to prepare a mixed solution.

[0040] Pour the above mixed solution into a three-neck flask, then add 75 g of tert-butanol while stirring, raise the temperature to 60° C., and keep the temperature for 30 minutes to obtain a crude product.

[0041] The crude product was separated with a separatory funnel to obtain 88.9 g of an oil phase. Through chromatographic analysis, it is detected that the content of tert-butyl hydroperoxide in the oil phase is 45.2%, the content of di-tert-butyl peroxide is 54.60%, and the others are 0.2%.

[0042] The above-mentioned oil phase is subjected to vacuum rectification at an absolute pressure of 2.5 to 10Kpa and a temperature of 20 to 50°C. The product at the top of the tower is condensed and weighs 40.2g. Chromatographic analysis shows that th...

Embodiment 2

[0044] Mix 100g of 35% hydrogen peroxide, 30g of 98% sulfuric acid, 0.5g of phosphotungstic acid, 2g of ethylenediaminetetramethylenephosphonic acid, and 2g of hydroxyethylidenediphosphonic acid at 15°C to prepare a mixed solution.

[0045] Pour 75 g of tert-butanol into a three-neck flask, then add the above mixed solution while stirring, raise the temperature to 60° C., and keep it warm for 30 minutes to obtain a crude product.

[0046]The crude product was separated to obtain 86 g of oil phase, and the oil phase was analyzed by chromatography, and it was detected that the content of tert-butyl hydroperoxide was 31.6%, the content of di-tert-butyl peroxide was 67.60%, and the others were 0.8%.

[0047] The above oil phase is subjected to vacuum rectification at an absolute pressure of 2.5 to 10Kpa and a temperature of 20 to 50°C. The product at the top of the tower is condensed to 57.9g. Chromatographic analysis shows that the content of di-tert-butyl peroxide is greater than...

Embodiment 3

[0049] Mix 100g of 35% hydrogen peroxide, 30g of 70% sulfuric acid, 2g of sodium citrate, 1g of phosphotungstic acid, and 2g of hydroxyethylidene diphosphonic acid at 15°C to prepare a mixed solution.

[0050] Add 74 g of tert-butanol into a three-necked flask, then add the above mixed solution while stirring, raise the temperature to 50° C., and keep it warm for 60 minutes to obtain a crude product.

[0051] The crude product was separated with a separatory funnel to obtain 88 g of the oil phase. The oil phase is analyzed by chromatography, and it is detected that the content of tert-butyl hydroperoxide is 55.19%, the content of di-tert-butyl peroxide is 44.70%, and the others are 0.19%.

[0052] The above oil phase was subjected to vacuum rectification at an absolute pressure of 2.5-10Kpa and a temperature of 20-50°C. The product at the top of the tower condensed and weighed 47.5g g. According to chromatographic analysis, the content of di-tert-butyl peroxide was greater tha...

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Abstract

The invention discloses a preparation method of tert-butyl hydroperoxide and di-t-butyl peroxide which includes the following steps: after mixing vitriol, oxyful and phosphotungstic acid with certain concentration, adding tertiary butyl alcohol into a mixed liquor or adding the mixed liquor into the tertiary butyl alcohol; reacting for 0.5 to 5 hours under 20 to 60 DEG C; obtaining an oil phase after carrying out liquid separation on the crude product of the reaction; obtaining the tert-butyl hydroperoxide and di-t-butyl peroxide products by carrying out decompressing and rectifying on the oil phase; the method has the advantages of simple and convenient operation, low manufacture cost, safety, high efficiency and high yield; in addition, the method of the invention can adjust the relative content of the two reaction products by changing the reaction conditions. The reaction products of tert-butyl hydroperoxide and di-t-butyl peroxide are separated by decompressing and rectifying, thus avoiding the working procedures of acid cleaning and caustic wash in the traditional technique, solving the defect of overlarge waste water amount in the traditional technique, being beneficial to protecting the environment, reducing the manufacture cost and being capable of greatly increasing the enterprise benefits.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a preparation method of tert-butyl hydroperoxide and di-tert-butyl peroxide. Background technique [0002] Tert-butyl hydroperoxide (tert.butyl hydroperoxide, TBHP for short) is an important branch of organic peroxides. It is a volatile, yellowish transparent liquid and an alkyl hydrogen organic peroxide. Tert-butyl hydroperoxide has good thermal stability, is safe to use, and is easy to control. Its activity does not change significantly within three months below 50°C, and it does not require expensive frozen storage. The decomposition products of TBHP are mainly tert-butanol and a small amount of acetone, etc., which are non-corrosive and require little equipment. The product can be used in the fields of diesel oil additives, paint industry and polymerization reaction (such as polyvinyl chloride, polyacrylic emulsion polymerization after monomer elimination, etc.), crosslinkin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C409/16C07C409/02
Inventor 陈惜明
Owner ZHEJIANG JINKE CHEM
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