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Method for preparing 11-bromo-undecanoic acid by direct freezing crystallization and device therefor

A technology of freezing crystallization and undecanoic acid, which is applied in the field of preparation of 11-bromoundecanoic acid, can solve the problems of large post-processing workload, large water consumption, and increased costs, and achieves low production costs, good economic benefits, response constant effect

Inactive Publication Date: 2012-07-04
山西宏远科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing technology has the disadvantages of long process and large post-processing workload. Hydrogen bromide generally needs to be washed 5 to 8 times, which requires a large amount of water consumption. Raised the cost of production

Method used

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  • Method for preparing 11-bromo-undecanoic acid by direct freezing crystallization and device therefor
  • Method for preparing 11-bromo-undecanoic acid by direct freezing crystallization and device therefor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Such as figure 1 The preparation device of the direct freeze crystallization of shown 11-bromoundecanoic acid comprises batching kettle 1, addition tower 2, crystallization kettle 3, filter press 4, and wherein the outlet at the bottom of batching kettle 1 and addition tower 2 The feed port at the top is connected, the feed port at the bottom of the addition tower 2 is connected with the feed port at the top of the crystallization kettle 3, the feed port at the bottom of the crystallization kettle 3 is connected with the feed port of the filter press 4, and the filter press The discharge port at the bottom of 4 is connected with the feed port at the top of batching kettle 1.

[0019] When working, the following steps are involved:

[0020] (1) Under the condition of keeping the temperature at -5°C in the batching kettle 1, mix undecylenic acid and toluene to obtain undecylenic acid toluene solution, wherein the mass ratio of undecylenic acid and toluene is 1:3.5;

[0...

Embodiment 2

[0026] Such as figure 1 The preparation device of the direct freeze crystallization of shown 11-bromoundecanoic acid comprises batching kettle 1, addition tower 2, crystallization kettle 3, filter press 4, and wherein the outlet at the bottom of batching kettle 1 and addition tower 2 The feed port at the top is connected, the feed port at the bottom of the addition tower 2 is connected with the feed port at the top of the crystallization kettle 3, the feed port at the bottom of the crystallization kettle 3 is connected with the feed port of the filter press 4, and the filter press The discharge port at the bottom of 4 is connected with the feed port at the top of batching kettle 1.

[0027] When working, the following steps are involved:

[0028] (1) Mix undecylenic acid and toluene under the condition of keeping the temperature at -3°C in the batching kettle 1 to obtain undecylenic acid toluene solution, wherein the mass ratio of undecylenic acid and toluene is 1:4;

[0029...

Embodiment 3

[0034] Such as figure 1 The preparation device of the direct freeze crystallization of shown 11-bromoundecanoic acid comprises batching kettle 1, addition tower 2, crystallization kettle 3, filter press 4, and wherein the outlet at the bottom of batching kettle 1 and addition tower 2 The feed port at the top is connected, the feed port at the bottom of the addition tower 2 is connected with the feed port at the top of the crystallization kettle 3, the feed port at the bottom of the crystallization kettle 3 is connected with the feed port of the filter press 4, and the filter press The discharge port at the bottom of 4 is connected with the feed port at the top of batching kettle 1.

[0035] When working, the following steps are involved:

[0036] (1) Under the condition of keeping the temperature at 0°C in the batching kettle 1, mix undecylenic acid and toluene to obtain undecylenic acid toluene solution, wherein the mass ratio of undecylenic acid and toluene is 1:3;

[0037...

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Abstract

The invention discloses a method for preparing 11-bromo-undecanoic acid by direct freezing crystallization and a device for preparing 11-bromo-undecanoic acid, and relates to a method for preparing the 11-bromo-undecanoic acid. The preparation device comprises a burdening kettle, an addition tower, a crystallization kettle and a filter press, wherein the burdening kettle is connected with the addition tower; the addition tower is connected with the crystallization kettle; the crystallization kettle is connected with the filter press; and the filter press is connected with the top part of the burdening kettle. During work, the preparation method comprises the steps of: mixing undecylenic acid and toluene in a mass ratio of 1:(3-4) at a temperature of -5-0 DEG C in the burdening kettle; allowing the mixed liquid with hydrogen bromide in a mole ratio of 1:1.05 at a temperature of 0-30 DEGC in the addition tower to react so as to generate an addition liquid; putting the addition liquid in the crystallization kettle, carrying out freezing crystallization at a temperature of -4 DEG C to -16 DEG C, a revolving speed of 8 round / min and a vacuum degree of -0.02MPa to -0.03MPa; and filtering crystal in the filter press. The device disclosed by the invention has the advantages of a simple structure, strong continuity and operability and is suitable for industrial production. The preparation method has the advantages of a short process flow, constant reaction, high product purity and good economic benefits.

Description

Technical field [0001] The present invention relates to a preparation method of 11-bromoundecanoic acid, and in particular to a preparation method and device for direct freeze crystallization of 11-bromoundecanoic acid. Background technique [0002] The current method for preparing 11-bromoundecanoic acid is generally to enter the toluene solution of undecenoic acid from the top of the addition tower, and the hydrogen bromide gas enters from the bottom of the addition tower, and then conduct anti-Martens addition in the addition tower. The reaction liquid flows out from the bottom of the tower. It is heated to remove hydrogen bromide and washed with water. Then the toluene is distilled, left to stand for thermal separation, and the crude bromide is separated. The bromide is recrystallized to obtain 11-bromoundecanoic acid. , the tail gas at the top of the tower is absorbed by alkali liquid and sent to the bromine recovery section, and the steamed toluene is neutralized, drie...

Claims

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Application Information

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IPC IPC(8): C07C53/19C07C51/363C07C51/43
Inventor 王慧远刘跃锋李元明
Owner 山西宏远科技股份有限公司
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