A kind of continuous refining method of glycidyl tertiary carbonic acid ester

A glycidyl ester and refining method technology, applied in the direction of organic chemistry, can solve the problems of high equipment cost, long separation process time, non-continuous production, etc., and achieve the goal of overcoming low product purity, long production cycle, and reducing equipment cost Effect

Active Publication Date: 2017-04-26
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The Chinese patent application whose publication number is CN102924407A provides a kind of refining method of glycidyl monocarboxylate, the purpose is to solve the refining problem of heavy components contained in the crude product of glycidyl monocarboxylate. Separation operation and process steps such as distillation and water removal, the separation process takes a long time, many steps, and cannot be continuously produced. At the same time, it needs to be connected with the distillation process of the previous section and the distillation and water removal process of the last section A large number of storage tanks and power equipment, increasing investment costs and operating costs
[0006] U.S. Patent No. 5,880,297 also mentions a method for processing the heavy product of glycidyl tertiary carbonate. Its high-temperature distillation method to separate heavy components and glycidyl tertiary carbonate is a physical process. At the same time, high-temperature operation increases the amount of heavy components. Through the treatment of this process, the separation yield of glycidyl tertiary carbonic acid ester is lower than its gas phase yield. At the same time, the equipment scraper type thin film evaporator is complicated to manufacture, expensive, and the equipment cost is high. It is difficult for enterprises to withstand, its application is limited

Method used

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  • A kind of continuous refining method of glycidyl tertiary carbonic acid ester
  • A kind of continuous refining method of glycidyl tertiary carbonic acid ester
  • A kind of continuous refining method of glycidyl tertiary carbonic acid ester

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Embodiment 1

[0049] A method for refining glycidyl tertiary carbonic acid ester, the method adopts the above-mentioned continuous alkali cleaning device for glycidyl tertiary carbonic acid ester, the specific steps are: in a jacketed 1L continuous alkaline washing kettle, continuously add impurities Content is 5.4% crude glycidyl ester of tertiary carbonic acid (Pt / Co chromaticity 60), rate is 3.5L / h, continuously adds sodium hydroxide aqueous solution (sodium hydroxide weight percent is 50%), rate is 0.35L / h ,Such as figure 1 As shown, enter the continuous phase separator from the first discharge port at the lower end of the continuous alkali cleaning kettle, and the glycidyl tertiary carbonic acid ester enters the upper end of the first stage continuous water washing kettle of the three-stage continuous countercurrent washing device from the upper end outlet of the continuous phase separator. Feed port, the water phase flowing out from the outlet at the lower end of the second-stage cont...

Embodiment 2

[0051] Repeat the process of embodiment 1, difference is in step (1), the sodium hydroxide that adds changes potassium hydroxide into.

Embodiment 3

[0053] The process of Example 1 was repeated, except that the crude product and sodium ethylate in step (1) were added in a ratio of 5:1 (molar ratio).

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Abstract

The invention belongs to the field of synthesis of an organic compound, and in particular provides a continuous refining method of versatate glycidyl. The method comprises the following steps: (1) continuous alkali wash and continuous phase splitting separation; and (2) continuous water wash and continuous phase splitting separation. By utilizing the refining method, the problems of high wastewater quantity and long time of alkali wash and water wash of versatate glycidyl crude product are solved; a large amount of wastewater and alkali liquor can be generated by refining by an intermittent alkali wash and water alkali technology, furthermore, the mixing time and standing time are long, and the efficiency is low. The continuous operation of separation process of products is realized, the production period of products is shortened, the yield of unit time is improved, meanwhile, through recycling the water of various eluting stages in the continuous water wash operation, the consumption of materials during the operation process is reduced, and the production effectiveness is improved.

Description

technical field [0001] The invention belongs to the field of organic compound synthesis, in particular to a continuous refining method for glycidyl tertiary carbonic acid ester. Background technique [0002] The structural formula of tertiary carbonic acid glycidyl ester is as follows: [0003] [0004] Wherein R1 and R2 are respectively the same or different alkyl groups of straight chain or branched chain structure with 1 to 6 carbon atoms, and R1+R2=C7. Glycidyl tert-carbonate has epoxy-functional end groups and is widely used in solvent-borne formulations of automotive OEM and refinish paints. In the preparation process of glycidyl tertiary carbonate, some heavy components will remain in the product, so it is necessary to refine glycidyl tertiary carbonate to improve its purity. [0005] The Chinese patent application whose publication number is CN102924407A provides a kind of refining method of glycidyl monocarboxylate, the purpose is to solve the refining problem ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/16C07D301/32
CPCC07D301/32C07D303/16
Inventor 肖英李毅黄超明陈春玉
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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