CN1136035A - Preparation of amino-acetic acid - Google Patents
Preparation of amino-acetic acid Download PDFInfo
- Publication number
- CN1136035A CN1136035A CN 95105301 CN95105301A CN1136035A CN 1136035 A CN1136035 A CN 1136035A CN 95105301 CN95105301 CN 95105301 CN 95105301 A CN95105301 A CN 95105301A CN 1136035 A CN1136035 A CN 1136035A
- Authority
- CN
- China
- Prior art keywords
- reaction
- water
- liquid
- methanol
- hexamethylenetetramine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A process for preparing amino acetic acid from liquid chloracetic acid as raw material and methenamine as catalyst includes ammonolysis reaction in presence of water, methanol extraction, sentrifugal separationa nd baking, and features simple technology, low production cost, and less environmental pollution.
Description
The invention relates to a method for preparing aminoacetic acid by utilizing a chloroacetic acid ammoniation method.
Aminoacetic acid is a white crystal, soluble in water and slightly soluble in alcohol, is a common amino acid and is widely used in chemical, pharmaceutical and food industries.
Some of the existing methods for preparing glycine use urotropine, chloroacetic acid and liquid ammonia (or ammonia water) as raw materials and synthesize the urotropine in an alcohol phase, and some of the existing methods use ammonium carbonate (or ammonium carbonate) or ammonium carbamate, chloroacetic acid and chlorine water as raw materials and synthesize the urotropine in a water phase, and the synthesis methods have complex process and low yield.
The invention aims to overcome the defects of the preparation of the aminoacetic acid and adopts liquid chloroacetic acid as a raw material and lotropine as a catalyst to carry out a series of processes in the presence of water.
The invention is realized by the following steps:
a preparation process of aminoacetic acid comprises the following raw materials in proportion: (based on a 500l reaction vessel)
Chloroacetic acid 180 kg and 210kg
60-70kg of liquid ammonia
20-40kg of hexamethylenetetramine
95% methanol 1.5-2.5m3
100kg of water
The preparation process comprises the following steps:
a. adding hexamethylenetetramine and water into a reaction kettle to dissolve the hexamethylenetetramine and the water, pumping chloroacetic acid into a metering tank,
b. introducing ammonia into the reaction kettle, dropwise adding chloroacetic acid for reaction at 70-85 ℃ for 3-4h,
c. and (3) extraction: putting the reaction liquid into an extraction tank, stirring and adding the reaction liquid for 2m3Cooling to 30-45 deg.C with methanol, stopping stirring, and crystallizing to obtain glycine,
d. the mixture is centrifuged and then is processed by centrifugal separation,
c. drying at 60-90 deg.C.
The present invention is described in detail below:
according to the invention, liquid chloroacetic acid is used as a raw material, hexamethylenetetramine is used as a catalyst, and ammonia is introduced to carry out ammonolysis reaction in the presence of water; extracting with methanol, centrifuging, and oven drying to obtain mother liquor, rectifying to recover methanol for cyclic utilization, and collecting ammonium chloroacetate as residue.
The reaction equation of the invention is as follows:
the acid liquid has the density of 1.30-1.40
The density of the reaction solution is 1.15-1.25
The reaction temperature is 70-85 DEG C
The pH value is 6.5-8
The extraction temperature is 40-45 DEG C
The present invention will be described with reference to examples.
According to the ingredients, 20 kg of hexamethylenetetramine and 110 kg of water are added into a 500l reaction kettle to be dissolved, and liquid chloroacetic acid is pumped into a metering tank.
1. Ammonolysis reaction:
opening an ammonia introducing valve to introduce ammonia into the kettle, opening an acid valve to dropwise add chloroacetic acid, controlling the reaction temperature to be 80 +/-2 ℃, controlling the pH value to be 7-8, controlling the specific gravity to reach 1.2-1.23, and reacting for about three hours to finish the reaction.
2. And (3) extraction: and putting the reaction liquid into an extraction tank while the reaction liquid is hot, starting stirring, adding 2m3 methanol, stopping stirring when the temperature is reduced to 30-45 ℃, and separating out white crystal glycine from the reaction liquid in the methanol.
3. Centrifuging: stirring, and centrifuging the methanol glycine solution in a centrifuge to obtain a wet product.
4. And (3) drying: drying the wet aminoacetic acid at 60-90 deg.C, oven drying, testing, packaging, and storing.
5. And (3) rectification: pumping the methanol water solution of the centrifugate into a rectifying towerby a pump to distill and recover methanol, putting the residual liquid in a kettle into a storage pool, naturally cooling, and taking out the ammonium chloride as a byproduct.
The process for preparing the aminoacetic acid has the following characteristics:
1. the process is mature and reliable, and is simple and industrialized.
2. The product has stable quality and the content is more than 97.5 percent.
3. The product yield is more than 80 percent, and the economic benefit is obvious.
4. The methanol mother liquor can be recycled by continuous distillation recovery, thereby greatly reducing the product cost.
5. The chloroacetic acid adopts liquid raw materials, and the pipeline transportation reduces the acid dissolving process and reduces the environmental pollution.
Claims (2)
1. A preparation process of aminoacetic acid comprises the following raw materials in proportion: (based on a 500l reaction vessel)
Chloroacetic acid 180 kg and 210kg
60-70kg of liquid ammonia
20-40kg of hexamethylenetetramine
95% methanol 1.5-2.5m3
100kg of water
The preparation process comprises the following steps:
a. adding hexamethylenetetramine and water into a reaction kettle to dissolve the hexamethylenetetramine and the water, pumping chloroacetic acid into a metering tank,
b. introducing ammonia into the reaction kettle, dropwise adding chloroacetic acid for reaction at 70-85 ℃ for 3-4h,
c. and (3) extraction: putting the reaction liquid into an extraction tank, stirring and adding the reaction liquid for 2m3Cooling to 30-45 deg.C with methanol, stopping stirring, and crystallizing to obtain glycine,
d. the mixture is centrifuged and then is processed by centrifugal separation,
c. drying at 60-90 deg.C.
2. The process for preparing glycine as claimed in claim 1, wherein the raw material ratio is (based on 500l reaction vessel):
chloroacetic acid 180 kg and 210kg
60-70kg of liquid ammonia
20-40kg of hexamethylenetetramine
95% methanol 1.5-2.5m3
100kg of water
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95105301 CN1136035A (en) | 1995-05-19 | 1995-05-19 | Preparation of amino-acetic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95105301 CN1136035A (en) | 1995-05-19 | 1995-05-19 | Preparation of amino-acetic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1136035A true CN1136035A (en) | 1996-11-20 |
Family
ID=5075453
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 95105301 Pending CN1136035A (en) | 1995-05-19 | 1995-05-19 | Preparation of amino-acetic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1136035A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100369822C (en) * | 2006-04-28 | 2008-02-20 | 石家庄东华金龙化工有限公司 | Method for treating mother liquor discharged from amino acetic acid production |
| CN105037186A (en) * | 2015-06-17 | 2015-11-11 | 苏州敬业医药化工有限公司 | Preparation method of aminomethylbenzoic acid |
| CN105294466A (en) * | 2015-11-12 | 2016-02-03 | 冀州市格润德生物科技有限公司 | Technology for producing high-purity aminoacetic acid based on urotropine cyclic utilization technology |
| CN109970213A (en) * | 2019-04-03 | 2019-07-05 | 石家庄宝川生物科技有限公司 | Biological bacteria conditioner |
| CN113563214A (en) * | 2021-07-06 | 2021-10-29 | 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 | Synthetic method of aminoacetic acid |
-
1995
- 1995-05-19 CN CN 95105301 patent/CN1136035A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100369822C (en) * | 2006-04-28 | 2008-02-20 | 石家庄东华金龙化工有限公司 | Method for treating mother liquor discharged from amino acetic acid production |
| CN105037186A (en) * | 2015-06-17 | 2015-11-11 | 苏州敬业医药化工有限公司 | Preparation method of aminomethylbenzoic acid |
| CN105294466A (en) * | 2015-11-12 | 2016-02-03 | 冀州市格润德生物科技有限公司 | Technology for producing high-purity aminoacetic acid based on urotropine cyclic utilization technology |
| CN105294466B (en) * | 2015-11-12 | 2019-03-19 | 冀州市格润德生物科技有限公司 | The production technology of high-purity amion acetic acid is produced based on methenamine recycle utilization |
| CN109970213A (en) * | 2019-04-03 | 2019-07-05 | 石家庄宝川生物科技有限公司 | Biological bacteria conditioner |
| CN113563214A (en) * | 2021-07-06 | 2021-10-29 | 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 | Synthetic method of aminoacetic acid |
| CN113563214B (en) * | 2021-07-06 | 2024-02-02 | 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 | Synthesis method of glycine |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4050338B2 (en) | Method for recovering fluorinated carboxylic acid | |
| TW200453B (en) | ||
| US20020102672A1 (en) | Process for producing a purified lactic acid solution | |
| CN1152853C (en) | Process for preparing glycine | |
| CN103664665A (en) | Solid sodium sarcosine preparation method | |
| EP1003707A1 (en) | Malonic acid and esters thereof | |
| CN1136035A (en) | Preparation of amino-acetic acid | |
| CN102030669A (en) | Clean production method for glycine | |
| CN1594302A (en) | Process for continuous preparation of trimellitic anhydride by step catalytic oxidation process | |
| CN1990460A (en) | Comprehensive treatment of glycine crystallization mother liquid | |
| CN1594281A (en) | Process for preparing iminodiacetic acid | |
| CN113636948B (en) | DL-p-hydroxyphenylglycine asymmetric conversion resolution waste liquid treatment method | |
| CN1745914A (en) | Recovering method of acetone and ammonia in hydrated hydrazine waste salt water by ketone azine method | |
| CN110878028A (en) | Preparation method of amino acid ester hydrochloride solution | |
| CN101709037A (en) | Method for preparing high-purity D-amino acid | |
| CN110041233B (en) | Preparation method of N-fatty acyl-N-methyl sodium taurate | |
| WO2005087702A1 (en) | Process for producing lactic ester | |
| WO2002074402A1 (en) | Azeotropic distillation process for producing organic acids or organic acid amides | |
| CN1176062C (en) | Preparation method of glycine | |
| CN1616434A (en) | Method for producing 1,3-dimethyl -2-imidazolinone | |
| CN1166616C (en) | Process and apparatus for purifying raw lactic acid | |
| CN1196392A (en) | Method for preparing levomethionine by decomposing mixed methionine with amino-acylation-hoydrolase | |
| CN111454172A (en) | Production method for preparing glutaronitrile by aminolysis of ester substance | |
| CN1006756B (en) | Method for preparing liquid state 2-hydroxy-4-methylthiobutyric acid used for animal food additive | |
| CN1491948A (en) | Spliting method for DL-pantoyl internal ester |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |