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Preparation method of guanidinoacetic acid

A technology of guanidinoacetic acid and guanidinoethanol, which is applied in the preparation field of guanidinoacetic acid, can solve the problems of increased cost of guanidinoacetic acid, complicated purification process, many side reactions, etc., and achieves high utilization rate of raw materials, improved reaction efficiency, production low cost effect

Active Publication Date: 2020-07-10
内蒙古天翊生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) Many side reactions lead to many by-products in guanidinoacetic acid, which increases the difficulty of purifying the crude product of guanidinoacetic acid on the one hand, and causes low utilization of raw materials glycine and cyanamide on the other hand, which increases the yield of guanidinoacetic acid. Increased costs
[0006] (2) In the process of purifying the crude product of guanidinoacetic acid, the purification process is not only complicated, but also the solvent used in the purification process is very harmful to the environment and human body.

Method used

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  • Preparation method of guanidinoacetic acid

Examples

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Effect test

Embodiment 1

[0034] A preparation method of guanidinoacetic acid, specifically comprising the following steps:

[0035] Step 1: Add 50 g of ethanolamine and 20 g of water into the reactor, and stir to raise the temperature to 40°C.

[0036] Step 2: After the temperature rise in step 1 is completed, add 80 g of an aqueous cyanamide solution whose mass to water volume ratio of cyanamide is 0.4 to the reactor, continue to stir after the aqueous cyanamide solution is added dropwise, and React for 2h to obtain guanidinoethanol.

[0037] Step 3: Add 1 g of catalyst TEMPO to the reaction kettle of guanidinoethanol obtained in step 2, continue to stir and continue to react at this temperature for 1 h, and obtain the crude product of guanidinoacetic acid after filtering while hot.

[0038] Step 4: Dissolve the crude guanidinoacetic acid obtained in step 3 in an aqueous ethanol solution with a volume ratio of 95% before cooling, recrystallize the crude guanidinoacetic acid in aqueous ethanol, and o...

Embodiment 2

[0041] A preparation method of guanidinoacetic acid, specifically comprising the following steps:

[0042] Step 1: Add 50 g of ethanolamine and 50 g of water into the reactor, and stir to raise the temperature to 70°C.

[0043] Step 2: After the temperature rise in step 1 is completed, add 55 g of cyanamide aqueous solution whose mass to water volume ratio of cyanamide is 0.6 to the reactor, and continue to stir after the cyanamide aqueous solution is added dropwise and at this temperature After 4 hours of reaction, guanidinoethanol was obtained.

[0044] Step 3: Add 15 g of catalyst TEMPO to the reaction kettle of guanidinoethanol obtained in step 2, continue to stir and continue to react at this temperature for 2 hours, and obtain the crude product of guanidinoacetic acid after filtering while hot.

[0045] Step 4: Dissolve the crude guanidinoacetic acid obtained in step 3 in an aqueous ethanol solution with a volume ratio of 95% before cooling, recrystallize the crude guan...

Embodiment 3

[0048] A preparation method of guanidinoacetic acid, specifically comprising the following steps:

[0049] Step 1: Add 50 g of ethanolamine and 35 g of water into the reactor, and stir to raise the temperature to 50°C.

[0050] Step 2: After the temperature rise in step 1 is completed, add 65 g of cyanamide aqueous solution whose mass to water volume ratio of cyanamide is 0.5 to the reactor, continue to stir after the cyanamide aqueous solution is added dropwise and at this temperature React for 2h to obtain guanidinoethanol.

[0051] Step 3: Add 10 g of catalyst TEMPO to the reaction kettle of guanidinoethanol obtained in step 2, continue to stir and continue to react at this temperature for 2 hours, and obtain the crude product of guanidinoacetic acid after filtering while hot.

[0052] Step 4: Dissolve the crude guanidinoacetic acid obtained in step 3 in an aqueous ethanol solution with a volume ratio of 95% before cooling, recrystallize the crude guanidinoacetic acid in a...

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Abstract

The invention discloses a preparation method of guanidinoacetic acid. The method includes: selecting ethanolamine and cyanamide as the raw materials for preparing guanidinoacetic acid, firstly reacting ethanolamine with cyanamide to obtain guanidinoethanol, then catalyzing the obtained guanidinoethanol with TEMPO to obtain a guanidinoacetic acid crude product, and then purifying the guanidinoacetic acid crude product by ethanol to obtain a guanidinoacetic acid refined product. According to the preparation method of guanidinoacetic acid, almost no side reaction occurs in the preparation processof guanidinoacetic acid, so that the generation of byproducts in the preparation process of the guanidinoacetic acid is reduced, and the difficulty of a purification process for the guanidinoacetic acid crude product is reduced. Meanwhile, the whole reaction process basically has no side reaction, so that the utilization rate of raw materials is increased, the preparation cost of the guanidinoacetic acid is reduced, and the purity of the guanidinoacetic acid prepared by adopting the method is relatively high.

Description

technical field [0001] The invention specifically relates to a preparation method of guanidinoacetic acid. Background technique [0002] Guanidinoacetic acid is white or slightly yellow crystalline powder, soluble in water, very slightly soluble in ethanol and ether. Guanidinoacetic acid is mainly used as an intermediate in pharmaceutical organic synthesis, and can also be used as a food and feed additive. It plays an important role in improving production performance, improving meat quality and promoting energy metabolism. In addition, it can prevent bacterial infection, enhance animal immune function, reduce The effect of heat stress on animals, thereby reducing the mortality of animals in high temperature environments. [0003] According to relevant literature reports, the main production process of guanidinoacetic acid is: mix thiourea, ethyl bromide and absolute ethanol, and warm in a water bath for 3 hours to completely dissolve the thiourea. Then distill off ethanol...

Claims

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Application Information

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IPC IPC(8): C07C277/08C07C279/08C07C279/14
CPCC07C277/08C07C279/08C07C279/14Y02P20/584
Inventor 王磊
Owner 内蒙古天翊生物科技有限公司
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