A method for preparing 11-aminoundecanoic acid from 10-undecenoic acid

A technology of undecanoic acid and enoic acid, which is applied in the field of preparing 11-aminoundecanoic acid from 10-undecenoic acid, can solve the problems such as non-crystallization, and achieves high quality, improved utilization rate, and improved reaction selectivity. Effect

Active Publication Date: 2016-01-27
江苏东鼎化学科技有限公司
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0008] Aiming at the problems existing in the existing 10-undecenoic acid production process of 11-aminoundecanoic acid, the present invention provides a method for directly producing 11-aminoundecanoic acid without crystallization of the 11-bromoundecanoic acid reaction liquid

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  • A method for preparing 11-aminoundecanoic acid from 10-undecenoic acid

Examples

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Effect test

Embodiment 1

[0031] Example 1: Using 10-undecylenic acid with a melting point of 23°C and a purity greater than 98% as a raw material, the ratio of the raw material solution to 10-undecylenic acid to toluene and benzene is 1:3:2, and 10-undecylenic acid is added. 4% azobisisobutyronitrile of undecylenic acid quality, reaction device such as figure 1 , start to put about 1 / 2 volume of raw material liquid into the addition kettle first, feed hydrogen bromide gas to the bottom of the addition kettle according to the molar ratio of 10-undecylenic acid to hydrogen bromide 1:1.1, and then feed the raw material liquid with hydrogen bromide Hydrogen bromide is kept in proportion and fed continuously, cooling water or frozen brine is passed through to control the reaction temperature of the addition tank at 18-20°C, and the reaction residence time is controlled for about 45 minutes by adjusting the liquid storage in the reactor by discharging. The jacket of the aging kettle is steamed to control th...

Embodiment 2

[0034]Example 2: Using 10-undecylenic acid with a melting point of 23°C and a purity greater than 98% as a raw material, the volume ratio of the raw material liquid ratio 10-undecylenic acid to toluene and benzene is 1:3:2, and 10-undecylenic acid is added. 4% azobisisobutyronitrile of undecylenic acid quality, reaction device such as figure 1 , start to put about 1 / 2 volume of raw material liquid into the addition kettle first, feed hydrogen bromide gas to the bottom of the addition kettle according to the molar ratio of 10-undecylenic acid to hydrogen bromide 1:1.1, and then feed the raw material liquid with hydrogen bromide Hydrogen bromide is kept in proportion and fed continuously, cooling water or frozen brine is passed through to control the reaction temperature of the addition tank at 18-20°C, and the reaction residence time is controlled for about 45 minutes by adjusting the liquid storage in the reactor by discharging. The jacket of the aging kettle is steamed to con...

Embodiment 3

[0038] Example 3: Using 10-undecylenic acid with a melting point of 23°C and a purity greater than 98% as a raw material, the ratio of the raw material solution to 10-undecylenic acid and toluene, benzene The volume ratio is 1:3:2, and 10-undecylenic acid is added 4% azobisisobutyronitrile of undecylenic acid quality, reaction device such as figure 1 , start to put about 1 / 2 volume of raw material liquid into the addition kettle first, feed hydrogen bromide gas to the bottom of the addition kettle according to the molar ratio of 10-undecylenic acid to hydrogen bromide 1:1.1, and then feed the raw material liquid with hydrogen bromide Hydrogen bromide is kept in proportion and fed continuously, cooling water or frozen brine is passed through to control the reaction temperature of the addition tank at 18-20°C, and the reaction residence time is controlled for about 45 minutes by adjusting the liquid storage in the reactor by discharging. The jacket of the aging kettle is steamed...

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Abstract

The invention relates to a process for producing nylon 11 resin by utilizing castor oil, in particular to a method for preparing 11-aminoundecanoic acid by utilizing 10-undecenoic acid. The method comprises the following steps: proportioning 10-undecenoic acid, methylbenzene and benzene to prepare a raw material solution, and generating 11-bromoundecanoic acid by virtue of the additive reaction of the raw material solution with hydrogen bromide in a double-kettle reaction device in the presence of catalyst; ammonolyzing the 11-bromoundecanoic acid by virtue of three different processing ways without the crystallization; adding a phase-transfer catalyst in the ammonolysis reaction to accelerate the ammonolysis reaction; carrying out vacuum filtering after the ammonolysis reaction is completed, wherein a filter cake is a 11-aminoundecanoic acid crude product; adding the crude product into the deionized water, dissolving the crude product by heating the crude product, cooling and crystallizing the crude product, and filtering the crude product to obtain the refined 11-aminoundecanoic acid product.

Description

technical field [0001] The invention relates to a process for producing nylon 11 resin from castor oil, specifically a method for preparing 11-aminoundecanoic acid from 10-undecylenic acid in the process. Background technique [0002] The chemical name of nylon 11 is polyundecylactam, the English name is Polyundecancylamide (abbreviated as PA11), and the chemical structure is H[NH(CH 2 ) 10 CO] n OH, a long carbon chain soft nylon synthesized from castor oil, is an important variety of polyamide engineering plastics. The production of nylon 11 mainly includes the production of 10-undecylenic acid, 11-aminoundecylic acid, monomer polymerization and resin modification. [0003] 11-aminoundecanoic acid is used as a monomer for synthesizing nylon 11, and the synthesis route adopted at home and abroad is divided into two steps. The first step is the bromination reaction. The raw material 10-undecylenic acid is mixed with toluene first, and hydrogen bromide gas undergoes rever...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/08C07C227/08
Inventor 唐昌盛袁志红
Owner 江苏东鼎化学科技有限公司
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