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Method for recycling 1,1-di(tert-butylperoxy)-3,3,5-trimethylcyclohexane alkali washing water

A technology of trimethylcyclohexane base and tert-butyl peroxy group, which is applied in the field of recovery and utilization of 1,1-bis-3,3,5-trimethylcyclohexane alkali washing water, can solve problems that cannot Recycling and Utilization of Alkaline Washing Water

Inactive Publication Date: 2019-01-18
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

But how to handle the bottom solution containing the sodium salt of tert-butyl hydroperoxide is not disclosed, that is to say, in the prior art, to 1,1-bis(tert-butyl peroxy)-3,3,5- The recycling method of trimethylcyclohexane alkaline washing water cannot fully recover and utilize the substances in the alkaline washing water

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 1000kg of 1,1-bis(tert-butyl peroxy)-3,3,5-trimethylcyclohexane alkali washing water (tert-butyl hydroperoxide: 1.18% , Sodium Hydroxide: 4.5%, 3,3,5-Trimethylcyclohexanone: 0.081%, COD: 35200mg / L) the pH value is adjusted to 5.5. Distilled under reduced pressure for 6 hours to obtain fraction 18kg (tert-butyl hydroperoxide: 64.12%, 3,3,5-trimethylcyclohexanone: 4.3%), bottom liquid 1050kg (tert-butyl hydroperoxide: 0.025%, 3,3,5-trimethylcyclohexanone: 0.003%, COD: 1230mg / L).

[0057] With 600.3kg tert-butyl hydroperoxide (mass fraction is 85%) and 400kg 3,3,5-trimethylcyclohexanone (mass fraction is 99%) and 18kg described cut at 5 ℃, rotating speed is 120r / Stir and mix for 10 minutes under the condition of 10 minutes, stand still to separate the lower aqueous phase, and obtain 974.09 kg of a mixed solution of tert-butyl hydroperoxide and 3,3,5-trimethylcyclohexanone;

[0058] 114.78kg of sulfuric acid (mass fraction is 98%) and 885.22kg of aqueous phase mother liq...

Embodiment 2

[0062] 1000kg of 1,1-bis(tert-butyl peroxy)-3,3,5-trimethylcyclohexane alkali washing water (tert-butyl hydroperoxide: 2.58% , Sodium Hydroxide: 3.5%, 3,3,5-Trimethylcyclohexanone: 0.121%, COD: 70200mg / L) the pH value is adjusted to 5.7, and the vacuum degree is -0.095MPa, the temperature is 70 ℃ Distilled under reduced pressure for 12 hours to obtain a fraction of 39kg (tert-butyl hydroperoxide: 66.03%, 3,3,5-trimethylcyclohexanone: 2.9%), bottom liquid 1020kg (tert-butyl hydroperoxide: 0.0047%, 3,3,5-trimethylcyclohexanone: 0.0077%, COD: 730mg / L).

[0063] With 667.81kg tert-butyl hydroperoxide (mass fraction is 80%) and 399kg 3,3,5-trimethylcyclohexanone (mass fraction is 99%) and 39kg described cut at 10 ℃, rotating speed is 100r / Stir and mix for 20 minutes under the condition of 20 minutes, let stand to separate the lower aqueous phase, and obtain 1057.3 kg of a mixed solution of tert-butyl hydroperoxide and 3,3,5-trimethylcyclohexanone;

[0064] 205.08 kg of sulfuric ...

Embodiment 3

[0068]1000kg of 1,1-bis(tert-butyl peroxy)-3,3,5-trimethylcyclohexane alkali washing water (tert-butyl hydroperoxide: 3.78% , Sodium Hydroxide: 2.5%, 3,3,5-Trimethylcyclohexanone: 0.24%, COD: 11300mg / L) the pH value was adjusted to 5.2. Distilled under reduced pressure for 20 hours to obtain fraction 58kg (tert-butyl hydroperoxide: 65%, 3,3,5-trimethylcyclohexanone: 3.95%), bottom liquid 1030kg (tert-butyl hydroperoxide: 0.0097%, 3,3,5-trimethylcyclohexanone: 0.011%, COD: 870mg / L).

[0069] With 764.33kg tert-butyl hydroperoxide (mass fraction is 75%) and 400kg 3,3,5-trimethylcyclohexanone (mass fraction is 99%) and 58kg described cut at 15 ℃, rotating speed is 120r / Stir and mix for 20 minutes under the condition of 20 minutes, stand still to separate the lower aqueous phase, and obtain 1169.01 kg of a mixed solution of tert-butyl hydroperoxide and 3,3,5-trimethylcyclohexanone;

[0070] 255.96kg of sulfuric acid (mass fraction is 98%) and 474.04kg of aqueous phase mother li...

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PUM

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Abstract

The invention provides a method for recycling 1,1-di(tert-butylperoxy)-3,3,5-trimethylcyclohexane alkali washing water. According to the method, a sulfuric acid solution is mixed with the 1,1-di(tert-b; utylperoxy)-3,3,5-trimethylcyclohexane alkali washing water for regulating the pH value of the 1,1-di(tert-butylperoxy)-3,3,5-trimethylcyclohexane alkali washing water, so that the introduction ofother anions can be reduced, and subsequent treatment can be performed conveniently; meanwhile, sodium salt in tert-butyl hydroperoxide can be neutralized into the tert-butyl hydroperoxide in the process, so that cyclohexanone and the tert-butyl hydroperoxide in the alkali washing water can be prepared into cut fractions through subsequent distillation under reduced pressure for recycling raw materials. As proved by the experiment result, the recycling method provided by the invention is simple, and full recycling of the sodium salt of the tert-butyl hydroperoxide and the 3,3,5-trimethylcyclohexanone in the alkali washing water can be realized.

Description

technical field [0001] The invention relates to the technical field of recycling organic matter, in particular to a method for recycling 1,1-bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane alkali washing water. Background technique [0002] 1,1-bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane is a low-volatility yellowish transparent liquid, belonging to ketal organic peroxides, mainly used as benzene Polymerization initiator of ethylene and its comonomer, etc., unsaturated polyester crosslinking agent, and vulcanizing agent of silicone rubber. At present, the most common method in industrial production is to prepare 1,1-bis(tert-butyl base peroxy)-3,3,5-trimethylcyclohexane, in the existing synthesis system, tert-butyl hydroperoxide is excessive, resulting in part of tert-butyl hydroperoxide remaining in the synthetic crude product after the reaction , need to add alkali for washing to remove tert-butyl hydroperoxide. During alkaline cleaning, tert-butyl hydroperoxide r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/18
CPCC07C407/003C07C409/18C07C2601/14
Inventor 顾屹立陈丹唐明亮
Owner 常熟市滨江化工有限公司