CN111517970A - Preparation method of L-aspartic acid sodium salt monohydrate - Google Patents
Preparation method of L-aspartic acid sodium salt monohydrate Download PDFInfo
- Publication number
- CN111517970A CN111517970A CN202010439821.0A CN202010439821A CN111517970A CN 111517970 A CN111517970 A CN 111517970A CN 202010439821 A CN202010439821 A CN 202010439821A CN 111517970 A CN111517970 A CN 111517970A
- Authority
- CN
- China
- Prior art keywords
- sodium
- solid phase
- phase reactor
- aspartic acid
- controlled
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
Abstract
The invention provides a preparation method of sodium L-aspartate monohydrate, which comprises the following steps: s1, mixing the raw materials: placing L-aspartic acid and a solid alkaline reactant into a mixing bin for mixing to obtain a mixture for later use S2 and carrying out chemical reaction: and grinding the mixture in a solid phase reactor to perform chemical reaction to obtain a reactant, wherein the temperature in the solid phase reactor is controlled to be 15-80 ℃, and the vacuum degree in the solid phase reactor is controlled to be 0.005-0. lMPa. The method has the advantages of simple process, short reaction time, high yield and low energy consumption, effectively avoids the hard agglomeration phenomenon of the product, does not use a solvent, has little pollution to the environment, has relatively high sodium content, is safe and reliable, has low cost, is a real green chemical reaction, and provides guarantee for the low-cost production of the L-sodium aspartate monohydrate.
Description
Technical Field
The invention relates to the technical field of preparation of sodium L-aspartate, in particular to a preparation method of sodium L-aspartate monohydrate.
Background
Sodium L-Aspartate (Sodium L-Aspartate, molecular weight 173.10) is an organic dibasic acid, and can generate acid salt when being neutralized with alkali, and Sodium L-Aspartate is colorless to white crystal or crystalline powder, is easily soluble in water, and is insoluble in alcohol. The water solution is neutral to slightly alkaline, is a food additive of flavor enhancer due to seafood flavor similar to shellfish, is widely applied to a fresh-keeping agent and a preservative in the food industry, and can replace monosodium glutamate.
The traditional process for producing the sodium L-aspartate by using the L-aspartate takes water as a medium, firstly, solid L-aspartate and sodium hydroxide or sodium carbonate react in an aqueous solution, and then the sodium L-aspartate is obtained by filtering, concentrating, alcohol precipitation and drying. Another method for producing sodium L-aspartate is to perform neutralization reaction between L-aspartate and sodium hydroxide or sodium carbonate in an aqueous solution, vacuum concentrating, cooling for crystallization, filtering and drying.
The above process mainly has the following defects: (1) waste water and waste residue are generated in the production process; (2) a large amount of energy is required in the product drying process; (3) the yield is low, and the production cost is high; (4) large investment and large occupied area of factory buildings.
Disclosure of Invention
The invention provides a preparation method of an L-aspartic acid sodium salt monohydrate, aiming at the defects of the prior art.
The invention solves the technical problems through the following technical means:
a method for preparing sodium L-aspartate monohydrate comprises the following steps:
s1, mixing the raw materials: placing L-aspartic acid and a solid alkaline reactant in a mixing bin for mixing to obtain a mixture for later use;
s2, chemical reaction: placing the mixture in a solid phase reactor for grinding, and carrying out chemical reaction to obtain a reactant, wherein the temperature in the solid phase reactor is controlled to be 15-80 ℃, and the vacuum degree in the solid phase reactor is controlled to be 0.005-0. lMPa;
s3, taking out the reactant.
Preferably, the alkaline reactant is any one of sodium hydroxide, sodium carbonate and sodium bicarbonate.
Preferably, the ratio of L-aspartic acid: the molar ratio of sodium hydroxide to sodium carbonate to sodium bicarbonate is 1:1 to 1.5.
Preferably, the ratio of L-aspartic acid: the molar ratio of sodium hydroxide/sodium carbonate/sodium bicarbonate is 1: 1-1.1.
Preferably, the solid phase reactor is a dry milling device.
Preferably, the dry grinding device is one of a vibration mill, a stirring mill (also called an attritor mill) and a horizontal ball mill.
Preferably, the temperature in the solid phase reactor is controlled to be 30-50 ℃.
Preferably, the vacuum degree in the solid phase reactor is controlled to be 0.01MPa to 0.05 MPa.
The invention has the advantages that: (1) the production process is simple; (2) the reaction process does not need heating, thereby saving energy; (3) no waste gas, waste water and waste residue are generated: (4) the equipment investment is low, the yield is high, and the occupied factory building is small.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for preparing sodium L-aspartate monohydrate comprises the following steps:
s1, mixing the raw materials: placing L-aspartic acid and a solid alkaline reactant in a mixing bin for mixing to obtain a mixture for later use;
s2, chemical reaction: placing the mixture in a solid phase reactor for grinding, and carrying out chemical reaction to obtain a reactant, wherein the temperature in the solid phase reactor is controlled to be 15-80 ℃, and the vacuum degree in the solid phase reactor is controlled to be 0.005-0. lMPa;
s3, taking out the reactant.
All reactants are in a solid state, are mixed and ground to carry out chemical reaction in a solid state to generate a solid product, and the reaction does not need heating and does not generate three wastes.
The process flow for synthesizing Beta-alanine calcium by solid phase reaction is as follows:
l-aspartic acid + sodium hydroxide/sodium carbonate/sodium bicarbonate → sodium L-aspartate;
the alkaline reactant is any one of sodium hydroxide, sodium carbonate and sodium bicarbonate.
The sodium used for synthesizing the sodium L-aspartate is mainly sodium hydroxide, sodium carbonate and sodium bicarbonate, and when the sodium hydroxide reacts with the L-aspartate, the sodium hydroxide, the sodium carbonate and the sodium bicarbonate are used independently;
the L-aspartic acid: the molar ratio of sodium hydroxide to sodium carbonate to sodium bicarbonate is 1:1 to 1.5.
The L-aspartic acid: the molar ratio of sodium hydroxide/sodium carbonate/sodium bicarbonate is 1: 1-1.1.
The solid phase reactor is dry grinding equipment.
The dry grinding equipment is one of vibration mill, stirring mill (also called vertical ball mill) and horizontal ball mill.
The temperature in the solid phase reactor is controlled to be 30-50 ℃.
L-aspartic acid is an organic acid, so that water is generated in the reaction, the initial speed of the solid-phase reaction is slow, the reaction speed is gradually increased along with the increase of the generated water in the reaction, and in order to prevent the reduction of the product quality caused by the temperature rise of the system due to the heat release caused by the over-high reaction speed, measures are taken to control the temperature rise.
Controlling the reaction temperature by two modes, namely a vacuum pumping method, namely evaporating and discharging water under the action of vacuum when the reaction temperature reaches 60 ℃, wherein the vacuum degree is 0.005-0.1 MPa, and preferably is controlled between 0.01-0.05 MPa; the second is cooling the reaction system mainly by jacket coolant method, cold air cooling method, or cooling method by continuously charging liquid nitrogen into the reaction system
The vacuum degree in the solid phase reactor is controlled to be 0.01 MPa-0.05 MPa.
The method for adding the reactant is that all L-aspartic acid is added into a solid phase reactor, the L-aspartic acid is ground for a certain time, the time is 10 minutes to L80 minutes, then sodium hydroxide or sodium carbonate (sodium bicarbonate) is added in 3-6 times by times according to different amounts of the reactor or the reactant.
Example 1
Taking l.33kg of L-aspartic acid, putting the L-aspartic acid into a small vertical ball mill, adjusting the rotating speed to 1200 r/min, adding 0.2kg of sodium hydroxide, cooling the mixture by using water to keep the temperature between 20 and 60 ℃, reacting for 30 minutes, then adding 0.15kg of sodium hydroxide, continuously grinding for 65 minutes, adding 0.05kg of sodium hydroxide again, finishing grinding for 40 minutes, filtering by using 95 percent ethanol, and drying to obtain 1.65kg of L-aspartic acid monohydrate (the yield of the L-aspartic acid sodium is 95 percent).
Example 2
Taking l.33kg of L-aspartic acid, putting the L-aspartic acid into a small vertical ball mill, regulating the rotating speed to 1200 r/min, adding 0.3kg of sodium carbonate, cooling the mixture by using water to keep the temperature between 20 and 60 ℃, reacting for 30 minutes, then adding 0.15kg of sodium carbonate, continuously grinding for 65 minutes, adding the rest 0.08kg of sodium carbonate again, finishing grinding for 40 minutes, filtering by using 95 percent ethanol, and drying to obtain 1.68kg of L-aspartic acid monohydrate (the yield of the L-aspartic acid sodium is 97%).
Example 3
Taking l.33kg of L-aspartic acid, putting the L-aspartic acid into a small vertical ball mill, regulating the rotating speed to 1200 r/min, adding 0.5kg of sodium bicarbonate, cooling the mixture by using water to keep the temperature between 20 and 60 ℃, reacting for 30 minutes, then adding 0.25kg of sodium bicarbonate, continuing to grind for 65 minutes, adding the rest 0.09kg of sodium bicarbonate again, finishing grinding for 40 minutes, filtering the mixture by using 95 percent ethanol, and drying the mixture to obtain 1.62kg of L-aspartic acid monohydrate (the yield of the L-aspartic acid sodium is 93.6 percent).
It is noted that, in this document, relational terms such as first and second, and the like, if any, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A method for preparing L-aspartic acid sodium monohydrate is characterized by comprising the following steps: the method comprises the following steps:
s1, mixing the raw materials: placing L-aspartic acid and a solid alkaline reactant in a mixing bin for mixing to obtain a mixture for later use;
s2, chemical reaction: placing the mixture in a solid phase reactor for grinding, and carrying out chemical reaction to obtain a reactant, wherein the temperature in the solid phase reactor is controlled to be 15-80 ℃, and the vacuum degree in the solid phase reactor is controlled to be 0.005-0. lMPa;
s3, taking out the reactant.
2. The method for preparing sodium L-aspartate monohydrate according to claim 1, wherein: the alkaline reactant is any one of sodium hydroxide, sodium carbonate and sodium bicarbonate.
3. The method for preparing sodium L-aspartate monohydrate according to claim 2, wherein: the L-aspartic acid: the molar ratio of sodium hydroxide to sodium carbonate to sodium bicarbonate is 1:1 to 1.5.
4. The method for preparing sodium L-aspartate monohydrate according to claim 3, wherein: the L-aspartic acid: the molar ratio of sodium hydroxide/sodium carbonate/sodium bicarbonate is 1: 1-1.1.
5. The method for preparing sodium L-aspartate monohydrate according to claim 4, wherein: the solid phase reactor is dry grinding equipment.
6. The method for preparing sodium L-aspartate monohydrate according to claim 2, wherein: the dry grinding equipment is one of vibration mill, stirring mill (also called vertical ball mill) and horizontal ball mill.
7. The method for preparing sodium L-aspartate monohydrate according to claim 1, wherein: the temperature in the solid phase reactor is controlled to be 30-50 ℃.
8. The method for preparing sodium L-aspartate monohydrate according to claim 2, wherein: the vacuum degree in the solid phase reactor is controlled to be 0.01 MPa-0.05 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010439821.0A CN111517970A (en) | 2020-05-22 | 2020-05-22 | Preparation method of L-aspartic acid sodium salt monohydrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010439821.0A CN111517970A (en) | 2020-05-22 | 2020-05-22 | Preparation method of L-aspartic acid sodium salt monohydrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111517970A true CN111517970A (en) | 2020-08-11 |
Family
ID=71905717
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010439821.0A Pending CN111517970A (en) | 2020-05-22 | 2020-05-22 | Preparation method of L-aspartic acid sodium salt monohydrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111517970A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1045969A (en) * | 1962-10-09 | 1966-10-19 | Rolland Lab A | Sodium betaine aspartate |
| DE19842053A1 (en) * | 1998-09-15 | 2000-03-23 | Bayer Ag | Use of polyaspartic acids in cleaning formulations with an abrasive effect |
| JP2000136172A (en) * | 1998-08-26 | 2000-05-16 | New Japan Chem Co Ltd | Production of n-substituted asparagic acid or its salt |
| CN101130798A (en) * | 2007-08-24 | 2008-02-27 | 安徽华恒生物工程有限公司 | Method for preparing sodium L-aspartate by bio-enzyme |
| CN106117070A (en) * | 2016-06-17 | 2016-11-16 | 宜兴市前成生物有限公司 | A kind of method preparing L asparagine acid disodium |
| CN109970586A (en) * | 2019-04-29 | 2019-07-05 | 安徽安力肽生物科技有限公司 | A kind of preparation method of Beta- Alanine calcium salt |
-
2020
- 2020-05-22 CN CN202010439821.0A patent/CN111517970A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1045969A (en) * | 1962-10-09 | 1966-10-19 | Rolland Lab A | Sodium betaine aspartate |
| JP2000136172A (en) * | 1998-08-26 | 2000-05-16 | New Japan Chem Co Ltd | Production of n-substituted asparagic acid or its salt |
| DE19842053A1 (en) * | 1998-09-15 | 2000-03-23 | Bayer Ag | Use of polyaspartic acids in cleaning formulations with an abrasive effect |
| CN101130798A (en) * | 2007-08-24 | 2008-02-27 | 安徽华恒生物工程有限公司 | Method for preparing sodium L-aspartate by bio-enzyme |
| CN106117070A (en) * | 2016-06-17 | 2016-11-16 | 宜兴市前成生物有限公司 | A kind of method preparing L asparagine acid disodium |
| CN109970586A (en) * | 2019-04-29 | 2019-07-05 | 安徽安力肽生物科技有限公司 | A kind of preparation method of Beta- Alanine calcium salt |
Non-Patent Citations (1)
| Title |
|---|
| 徐景峰 等: "衣康酸/2- 丙烯酰胺-2- 甲基丙磺酸/ 次磷酸钠共聚物的合成与阻垢性能", 《水处理技术》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP3127896B1 (en) | Method for preparing iminodisuccinate chelating agent | |
| Zhao et al. | Hydrothermal synthesis and lanthanide doping of complex fluorides, LiYF 4, KYF 4 and BaBeF 4 under mild conditions | |
| CN100445278C (en) | Method of synthesizing dehydro sodium acetate | |
| CN109053535A (en) | A kind of preparation method of n-acetyl-5-methoxytryptamine | |
| JPH0367967B2 (en) | ||
| JPH1059711A (en) | Magnesium hydroxide and production of aqueous liquid suspension thereof | |
| CN102965077B (en) | Powdered ore additive | |
| CN111517970A (en) | Preparation method of L-aspartic acid sodium salt monohydrate | |
| CN104058844B (en) | Threonine mother liquor is utilized to prepare the method for multicomponent chelate thing fertilizer | |
| CN101357885B (en) | Method for synthesizing sodium succinate through solid phase reaction | |
| CN109516487B (en) | Method for preparing calcium bicarbonate powder by solvent method | |
| KR100415419B1 (en) | Production of boric oxide | |
| CN104693483B (en) | Preparation method of high-dispersibility melamine pyrophosphate fire retardant | |
| CN108840349B (en) | Preparation method of superfine amorphous boron powder | |
| CN106830742B (en) | Preparation method of composite foam stabilizer for producing self-heat-insulation lightweight concrete building block and composite foam stabilizer | |
| US4629508A (en) | Process for forming hydrated calcium silicate products | |
| US4026932A (en) | Method for converting alkenoic acid copolymer latexes into water solutions | |
| US10239813B2 (en) | Method for producing calcium dipropionate | |
| CN104276944A (en) | Method for controlling continuous reaction crystal size of 2,4-dichlorphenoxyacetic acid | |
| CN109970586A (en) | A kind of preparation method of Beta- Alanine calcium salt | |
| CN112811614A (en) | Circulating water phosphorus-free scale inhibitor and preparation method thereof | |
| CN113321592A (en) | Preparation method of magnesium glycinate | |
| CN111004362A (en) | Preparation method of naphthalene-based superplasticizer | |
| CN112978701A (en) | Preparation method of sodium hexametaphosphate | |
| RU2189355C2 (en) | Method of synthesis of aluminium oxychlorosulfate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |