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A kind of preparation method of 3 chloro-1,2-propanediol

A technology of propylene glycol and chloropropene, which is applied in the field of preparation of 3-chloro-1,2-propanediol, can solve the problems of many by-products, reduced yield, and difficulty in meeting the requirements, and achieves the reduction of waste acid discharge, solid waste discharge, and reduction of The effect of hydrolysis by-products

Active Publication Date: 2021-11-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of the glycerin method is that there are many by-products, and it is difficult to achieve a purity of more than 99.5% of the product content. Hydrogen chloride gas requires high equipment and requires a large investment.
Although the epichlorohydrin hydrolysis method is a relatively mature method at home and abroad, the disadvantage is that the traditional chlorohydrin production of raw material epichlorohydrin has been difficult to meet the national requirements for energy saving, emission reduction and environmental protection. In addition, the use of organic acids as catalysts will The occurrence of side reactions to the reduction of yield, and the need to add alkali to adjust the pH value will easily cause adverse effects such as difficult control of process parameters and increase of solid waste in subsequent processes
Its shortcoming is that the hydrolysis process of epichlorohydrin uses organic acid as a catalyst, and side reactions will occur to reduce the yield. After the hydrolysis reaction is completed, adding alkali to adjust the pH value will easily cause adverse effects such as difficult control of process parameters and increased solid waste in the subsequent process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In the 1000ml reactor, add chloropropene 300g, mass concentration is 50% hydrogen peroxide aqueous solution 90g, add 20g reaction control phase-transfer catalyst [π-C 5 h 5 NC 16 h 33 ] 3 (PO 4 ) (WO 3 ) 4 ], the reaction temperature was 45°C, and the reaction pressure was 0.5MPa. After 2.5 hours of reaction, the reaction materials were centrifuged to recover the reaction-controlled phase transfer catalyst.

[0024] Continue to add 90g of aqueous hydrogen peroxide solution with a mass concentration of 50%, 400g of deionized water, and solid acid catalyst B to the material containing epichlorohydrin prepared above. 2 o 3 -Al 2 o 3 5g was reacted at 75°C for 2h, and the reaction pressure was 1.5MPa.

[0025] After the hydrolysis reaction was completed, the solid acid catalyst reaction material was filtered and separated, and the filtrate was washed with 300g of chloropropene and then subjected to vacuum distillation. The vacuum of the vacuum distillation was 40...

Embodiment 2

[0027] In the 1000ml reactor, add chloropropene 300g, mass concentration is 50% hydrogen peroxide aqueous solution 90g, add 20g reaction control phase-transfer catalyst [π-C 5 h 5 NC 16 h 33 ] 3 (PO 4 ) (WO 3 ) 4 ], the reaction temperature was 45°C, and the reaction pressure was 0.5MPa. After 2.5 hours of reaction, the reaction materials were centrifuged to recover the reaction-controlled phase transfer catalyst.

[0028] The above-mentioned prepared material containing epichlorohydrin is continued to add 120 g of 50% hydrogen peroxide aqueous solution, 300 g of deionized water, and solid acid catalyst SiO 2 -Al 2 o 3 5g was reacted at 75°C for 1.5h, and the reaction pressure was 1.0MPa.

[0029] After the hydrolysis reaction was completed, the solid acid catalyst reaction material was filtered and separated, and the filtrate was washed with 350g of chloropropene and then subjected to vacuum distillation. The vacuum of the vacuum distillation was 200KPa, and the vac...

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Abstract

A preparation method of 3-chloro-1,2-propanediol provided by the present invention uses hydrogen peroxide as an oxygen source, and a reaction-controlled phase-transfer catalyst catalyzes chloropropene to generate epichlorohydrin, and then prepares 3-chloro-1,2 through hydrolysis. ‑propylene glycol, the preparation process mainly includes three steps of epoxidation reaction, hydrolysis reaction and product purification, and the product 3-chloro-1,2-propylene glycol with a content of more than 99.9% is obtained. This method has simple process, high product purity and is easy to produce .

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and in particular relates to a preparation method of 3-chloro-1,2-propanediol. Background technique [0002] 3-chloro-1,2-propanediol (3-chloro-1,2-propanediol), commonly known as 3-chloro-1,2-dihydroxypropane, molecular formula is C 3 h 7 CIO 2 , with a molecular weight of 110.55. It can be used as an intermediate in organic synthesis, widely used in the synthesis of pesticides, medicines, coatings, plasticizers, surfactants, etc. Currently, the synthesis of 3-chloro-1,2-propanediol mainly includes epichlorohydrin hydrolysis and glycerin chlorination Law. [0003] The glycerin chlorination method is to add glycerin and acetic acid to the reaction pot, stir and heat to 90-95 ° C, and pass dry hydrogen chloride gas until the weight of the reaction solution reaches 150% (theoretical value) and that is the end point. Distilled under reduced pressure to obtain crude product. Further fracti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/10C07C31/42
CPCY02P20/584
Inventor 高爽张毅吕迎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI