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Method for preparing isooctyl thioglycolate by utilizing thionocarbamate tail liquid

A technology of isooctyl thioglycolate and thiourethane, which is applied in the preparation of mercaptans, organic chemistry and other directions, can solve the problems of unstable product quality, unsafe handling of ether, and difficult operation, and achieves outstanding substantive features and reduces The effect of removing impurities and reducing operation steps

Active Publication Date: 2012-11-14
YANTAI HUMON CHEM AUX CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to overcome the above-mentioned deficiencies in the prior art, and provide a method for utilizing thiourethane tail liquid to manufacture isooctyl thioglycolate, mainly solve existing technological operation difficulty, long reaction time, high cost, poor product quality Stability and unsafe ether treatment cause environmental pollution and other issues

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  • Method for preparing isooctyl thioglycolate by utilizing thionocarbamate tail liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Example 1, the thiourethane tail liquid and the xylene extractant are uniformly mixed under normal pressure at a molar ratio of 1:7, and the tail liquid is removed for impurity removal; dilute hydrochloric acid is added for acidification while removing impurities, and the adjustment pH 4 ~5； After the acidification is completed, let it stand for stratification, separate the bottom acidification solution, and keep the xylene extractant in the upper layer for recycling in the original process; under the condition of stirring in the acidification solution, add 1%-2% zinc powder of the weight of the acidification solution to make the acidification solution It is colorless; the esterification liquid is subjected to multi-stage continuous extraction with isooctyl alcohol in the extraction tank, the content of thioglycolic acid in the extraction liquid is 55%-60%, and the content of thioglycolic acid in the tail liquid is ≤0.2%; in the extraction liquid , adding 0.2% benzenesu...

Embodiment 2

[0020] Example 2, the thiourethane tail liquid and the toluene extractant are uniformly mixed under normal pressure at a molar ratio of 1:6 to remove impurities from the tail liquid; while removing impurities, dilute hydrochloric acid is added to acidify and adjust the pH value 4 ~5； After the acidification is completed, let it stand for stratification, separate the bottom acidification solution, and keep the toluene extractant in the upper layer for recycling; under the condition of stirring in the acidification solution, add zinc powder of 1%-2% of the weight of the acidification solution to make the acidification solution reach Colorless; the esterification liquid is subjected to multi-stage continuous extraction with isooctyl alcohol in the extraction tank, the content of thioglycolic acid in the extraction liquid is 55%-60%, and the content of thioglycolic acid in the tail liquid is ≤0.2%; in the extraction liquid, Add 0.02% benzenesulfonic acid catalyst of the weight of ...

Embodiment 3

[0021] Example 3, the thiourethane tail liquid and the dinitrobenzene extractant are uniformly mixed under normal pressure at a molar ratio of 1:8, and the tail liquid is removed; while removing impurities, dilute hydrochloric acid is added for acidification , adjust the pH value to 4 ~5； After the acidification is completed, let it stand for stratification, separate the bottom acidification solution, and keep the dinitrobenzene extractant in the upper layer for recycling; under the condition of stirring in the acidification solution, add zinc powder of 1%-2% of the weight of the acidification solution to make The acidified solution is colorless; the esterified solution is subjected to multi-stage continuous extraction with isooctyl alcohol in the extraction tank, the content of thioglycolic acid in the extraction solution is 55%-60%, and the content of thioglycolic acid in the extraction tail liquid is ≤0.2%; In the liquid, add 0.5% benzenesulfonic acid catalyst of the weight...

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Abstract

The invention discloses a method for preparing isooctyl thioglycolate by utilizing thionocarbamate tail liquid, which is characterized by comprising the following process steps of: impurity removal and acidification, Zn powder decolorizing, extraction, crude distillation and rectification. The method has the beneficial effects that the impurity removal and the acidification are integrated, an efficient benzene extraction agent is adopted for replacing ethyl ether to reduce the risk and the pollution and the operation steps are also simplified, and meanwhile, the efficient benzene extraction agent can be recycled and is convenient to operate; a zinc powder decoloring process is increased, so that the he product quality stability is ensured; the esterification reaction is finished at the same time in the crude distillation process, and a qualified coarse ester semi-product is obtained at one time, so that the operation steps are reduced, and the efficiency is improved; and through direct rectification, a distillation kettle substrate is left in a crude distillation process, and no rectification kettle substrate is generated, so that the production capacity and the product yield are improved, and the cost is reduced.

Description

Technical field: [0001] The invention relates to the technical field of chemical engineering, in particular to a method for producing isooctyl thioglycolate using thiourethane tail liquid. Background technique: [0002] At present, with the continuous expansion of the plastic stabilizer market, the demand for isooctyl ester as a raw material for the manufacture of stabilizers is also increasing. The existing processes are: 1. acidification of tail liquid; 2. removal of impurities with ether; 3. extraction of isooctyl alcohol; 4. esterification reaction; 5. removal of impurities of crude ester; Large, long reaction time, high cost, unstable product quality, and problems such as environmental pollution caused by unsafe ether treatment. Invention content: [0003] The purpose of the present invention is to overcome the above-mentioned deficiencies in the prior art, and provide a method for utilizing thiourethane tail liquid to manufacture isooctyl thioglycolate, mainly solve...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/12
Inventor 王雄斌姜维远徐晓黄东梅鲁新洲林乐平李海平
Owner YANTAI HUMON CHEM AUX CO LTD
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