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Preparation method of alpha, alpha'-bis(tert-butyl peroxy) diisopropylbenzene

A kind of technology of tert-butylperoxy and diisopropylbenzene, applied in the field of synthesis technology of organic peroxide, can solve the problems such as no related reports, and achieve the effect of reducing production cost, simplifying operation process and reducing pollution

Inactive Publication Date: 2009-09-30
HUNAN YIXIANG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, there have also been reports on the synthesis of organic peroxides catalyzed by heteropolyacids, including the reaction of TBHP and tert-butanol (see M.K.Faraj, US 5288919, 1994, Preparation of dialkyl peroxides), TBHP and α, α-dimethylbenzyl Alcohol reaction, etc. (A. Tarlani, Catalytic condensation process for the preparation of organic peroxides from tert-butylhydroperoxide and benzylic alcohols, Applied Catalysis A: General, 315 (2006) 150-152), but no application of heteropolyacids has been seen Related reports on catalytic synthesis of environmentally friendly crosslinker BIPB

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In a 250mL three-necked flask, 150g of cyclohexane, 4.5g of catalyst, 21.2g of TBHP80% hydrate (commercially available) and 19.5g of DC were successively added, and the mixed material was stirred and reacted at 30°C for 20h, then suction filtered, and the filtrate was Distill under reduced pressure at 50°C to 60°C until no solvent is distilled out; the raffinate after distillation is cooled to below 25°C to obtain 20.8g of solid product BIPB with a yield of 60.8% (calculated as DC), and the content reaches 98.5% (determined by high performance liquid chromatography, i.e. HPLC).

Embodiment 2

[0015] Add 100g of dichloromethane, 18.5g of catalyst, 26.5g of TBHP80% hydrate and 19.5g of DC in sequence into a 250mL three-necked flask. The mixed material is stirred and reacted at 45°C for 16h, then suction filtered, and the filtrate is heated at 50°C to 55°C Distillation under reduced pressure under ℃ condition, to solvent-free distillation; The raffinate after distillation is cooled to below 25 ℃, promptly obtains the solid product BIPB of 17.5g, and yield is 50.8% (in DC), and content reaches 98.2% (HPLC analytical determination).

Embodiment 3

[0017] Add 150 g of di-tert-butyl peroxide, 9.8 g of catalyst, 21.5 g of TBHP 80% hydrate and 19.5 g of DC successively into a 250 mL three-necked flask. The mixed material is stirred and reacted at 45° C. for 20 h, then suction filtered, and the filtrate is Under reduced pressure distillation at ℃~60℃, until no solvent is distilled out; the distillation raffinate is cooled to below 25℃, and the solid product BIPB of 18.3g is obtained, the yield is 54.0% (in terms of DC), and the content reaches 99.1% ( determined by HPLC analysis).

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PUM

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Abstract

The present invention discloses a preparation method of alpha, alpha'-bis(tert-butyl peroxy) diisopropylbenzene, including the following steps: put tert-butyl peroxyhydrate and alpha, alpha'-dihydroxy-p- diisopropylbenzene (mass ratio: 0.8-1.9) into an organic solvent, add heteropoly acid as catalyst, react under agitation at room temperature, filter the material 15-25h later, remove the organic solvent from filtrate through decompression, cool down residual solution to below 30 DEG C to solidify it, and obtain product alpha, alpha'-bis(tert-butyl peroxy) diisopropylbenzene. The present invention is characterized by simple process, easy operation, low cost, high safety and effective reduction of environmental pollution and equipment corrosion.

Description

technical field [0001] The invention relates to a synthesis process of organic peroxides, in particular to a preparation process of bis(tert-butyl peroxy) dicumyl. Background technique [0002] α, α'-bis(tert-butylperoxy) diisopropylbenzene (abbreviated as BIPB or double BP) is a new type of high-efficiency non-polluting crosslinking agent replacing dicumyl peroxide (abbreviated as DCP), mainly used as Crosslinking agent for polyethylene, unsaturated resin, silicone rubber, nitrile rubber, ethylene propylene rubber and polyurethane, especially suitable for indoor products, children's toys, food utensils and other occasions with high requirements, improving the performance of general crosslinking agent DCP It is an excellent crosslinking agent with a wide range of uses. The BIPB product is mainly composed of a mixture of meta-position and para-position isomers. It is a white powder with a molecular weight of 338.49, a theoretical active oxygen of 9.45%, an activation energy ...

Claims

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Application Information

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IPC IPC(8): C07C409/16C07C407/00C08K5/14
Inventor 李玉新单文伟
Owner HUNAN YIXIANG TECH
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