CN111675627A - Preparation method of calcium aspartate - Google Patents

Preparation method of calcium aspartate Download PDF

Info

Publication number
CN111675627A
CN111675627A CN202010587808.XA CN202010587808A CN111675627A CN 111675627 A CN111675627 A CN 111675627A CN 202010587808 A CN202010587808 A CN 202010587808A CN 111675627 A CN111675627 A CN 111675627A
Authority
CN
China
Prior art keywords
calcium
aspartate
calcium aspartate
preparation
homogenization
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
Application number
CN202010587808.XA
Other languages
Chinese (zh)
Inventor
郑艳丽
汪豫兰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Jiaxiang Industry Co ltd
Original Assignee
Shanghai Jiaxiang Industry Co ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shanghai Jiaxiang Industry Co ltd filed Critical Shanghai Jiaxiang Industry Co ltd
Priority to CN202010587808.XA priority Critical patent/CN111675627A/en
Publication of CN111675627A publication Critical patent/CN111675627A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/14Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
    • C07C227/18Preparation 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
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/38Separation; Purification; Stabilisation; Use of additives
    • C07C227/40Separation; Purification

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention belongs to the technical field of bioengineering, and particularly relates to a preparation method of calcium aspartate, which specifically comprises the following steps: s1, reacting raw materials; s2, primary homogenizing; s3, homogenizing for the second time; s4, drying, sieving and packaging. The preparation method of the calcium aspartate provided by the invention has the advantages that the cost and the reaction efficiency are considered, the high-purity calcium aspartate is obtained by compounding the calcium carbonate and the calcium hydroxide, the economic value is better, the resources are fully utilized, and the social benefit is greater; the preparation method is simple and convenient, and is suitable for large-scale industrial production.

Description

Preparation method of calcium aspartate
Technical Field
The invention belongs to the technical field of bioengineering, and particularly relates to a preparation method of calcium aspartate.
Background
Calcium is a major element essential to the human body. It not only constitutes the bones and teeth of the human body, but also participates in various physiological activities. According to the research data of related nutrition, the residents in China generally have insufficient calcium and nutrition, the related diseases caused by the calcium deficiency are known by the public, and the attention of people is gradually drawn to the calcium supplement. At present, calcium agents sold in the market include calcium carbonate, calcium lactate, calcium hydrogen phosphate, calcium citrate, amino acid chelated calcium and the like.
The calcium aspartate is one of amino acid chelated calcium, and is prepared by refining every two amino acid molecules and one calcium ion under the special conditions of high pressure and high frequency. The chelated calcium molecule has stable structure, the calcium atom is connected with the nitrogen atoms in the two amino acid molecules by a coordination bond and is connected with the oxygen atom of the carboxyl group by a covalent bond to form two five-membered rings with stable structure, the special chelated structure not only ensures that the calcium atom is not easily influenced by acid and alkali in the stomach and intestine, but also ensures that the chelated calcium can be covalently combined with glutathione on the cell membrane of the small intestine mucosa and directly enters the intestinal mucosa to be completely absorbed by the human body.
The aspartic acid chelated calcium has the following characteristics: 1. the absorption rate is up to more than 95 percent and is 3 to 4 times of that of other calcium products; 2. is easy to dissolve in water, and the solubility of the calcium carbonate is 400 times of that of edible calcium carbonate, so that the calcium carbonate is easier to absorb by a human body; 3. vitamin D is not needed to be added, no precipitate is generated, no calculus is formed, and the method is safer; 4. the pH value (pH value) is neutral, basically accords with the pH value of a human body, and has no stimulation to the stomach and intestine; 5. after entering blood, a slow flowing calcium reservoir is formed, hypercalcemia cannot be caused by high plasma calcium concentration, and waste cannot be caused by kidney discharge; 6. has good protection and repair effects on damaged heart and liver cells, accelerates the excretion of in vivo metabolites, and improves the immunity of human bodies.
The inorganic calcium source for the preparation of calcium aspartate is generally calcium oxide or calcium hydroxide or calcium carbonate. The calcium carbonate has poor solubility, the yield of the calcium aspartate prepared by singly using the calcium carbonate as a raw material is relatively low, and the reaction efficiency is slow; the price of calcium hydroxide is relatively high, and the preparation of calcium aspartate by only using calcium hydroxide as a raw material has the disadvantage of production cost.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for preparing calcium aspartate by compounding calcium carbonate and calcium hydroxide as an inorganic calcium source.
The preparation method of the calcium aspartate specifically comprises the following steps:
s1, mixing 0.9-1.1 parts of L-aspartic acid, 0.1-0.3 part of calcium carbonate, 0.1-0.3 part of calcium hydroxide and 3.2 parts of pure water according to parts by weight, and reacting at 65-85 ℃ and pH of 5.3-6.0 for 0.5-1 h; when the pH value of the reaction liquid is 6.1-6.5, preserving the heat for 5-10 min;
s2, primary homogenization: filtering the reaction solution obtained in the step S1 under 60-80MPa, and homogenizing for 30-60 min;
s3, secondary homogenization: filtering the reaction solution after primary homogenization at 90-130MPa, and then homogenizing for 150-300 min;
and S4, standing and precipitating the reaction solution after secondary homogenization, separating to obtain a supernatant, and drying to obtain the calcium aspartate.
Preferably, the filtration in S2 is performed by a 100-mesh screen, and the feeding speed during homogenization is 500-1000L/h; the filtration in step S3 is performed by a 500-mesh screen, and the feeding speed during homogenization is 120-200L/h.
Preferably, the drying in S4 is spray drying at 250 ℃ and 180 ℃, and the water content of the dried calcium aspartate is less than or equal to 5%.
Preferably, the particle size of the calcium aspartate in S4 is 60-120 meshes.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the calcium aspartate comprehensively considers the cost of the calcium carbonate and the reaction rate of the raw materials, the calcium carbonate is low in price but is insoluble in water, and when the calcium carbonate is used as the raw material to react with the aspartic acid, the solubility is not high, so that the reaction efficiency is influenced, and the energy consumption is improved; insoluble calcium carbonate is easy to agglomerate in the reaction kettle, and the heat transfer of the reaction kettle is influenced; calcium hydroxide as a strong base reacts with aspartic acid more easily and fully, has certain solubility in water, has reaction efficiency far higher than that of calcium carbonate, but as an inorganic calcium source, has a price far higher than that of calcium carbonate, and causes the product cost to rise; the invention gives consideration to the cost and the reaction efficiency, and the high-purity calcium aspartate is obtained by compounding the calcium carbonate and the calcium hydroxide, thereby having better economic value, fully utilizing resources and having greater social benefit; the preparation method is simple and convenient, and is suitable for large-scale industrial production.
Detailed Description
In order to make the technical solutions of the present invention better understood and enable those skilled in the art to practice the present invention, the following embodiments are further described, but the present invention is not limited to the following embodiments.
Example 1
Figure BDA0002555301920000031
The preparation method comprises the following steps:
s1, burdening reaction: adding the raw materials into a reaction kettle according to a proportion, and reacting for 0.5h at 65 ℃ and pH of 5.3; when the pH value of the reaction liquid is 6.1, preserving the temperature for 5 min;
s2, primary homogenization: filtering the reaction solution through a 100-mesh pipeline filter under the condition of 60MPa, then feeding the reaction solution into a homogenizer, controlling the feeding speed to be 500L/h, homogenizing for 30min, and then collecting the filtrate;
s3, secondary homogenization: filtering the filtrate obtained in the step S2 by using a 500-mesh screen under the condition of 90MPa, then feeding the filtrate into a homogenizer, controlling the feeding speed to be 120L/h, homogenizing for 150min, and standing the obtained homogenized material liquid overnight;
s4, spray drying: drying the supernatant of the calcium aspartate after standing by using an instantaneous high-temperature technology of spray drying at the temperature of 200 ℃, and controlling the water content of the product to be not higher than 5%;
s5, sieving: and sieving the spray-dried calcium aspartate powder by a sieve of 80 meshes, and subpackaging into 90 g/barrel to obtain the finished calcium aspartate.
The detection method is carried out according to the indexes of GB 29226: the product contains calcium 12.8%, L-aspartic acid 82.2%, pH 7.05, water 4.51%, lead 0.09mg/kg, and total arsenic 0.13 mg/kg.
Example 2
Figure BDA0002555301920000041
The preparation method comprises the following steps:
s1, burdening reaction: adding the raw materials into a reaction kettle according to a proportion, and reacting for 1.0h at 85 ℃ and pH of 6.0; when the pH value of the reaction liquid is 6.5, preserving the temperature for 10 min;
s2, primary homogenization: filtering the reaction solution through a 100-mesh pipeline filter under the condition of 80MPa, feeding the reaction solution into a homogenizer at a feeding speed of 1000L/h, and collecting filtrate after homogenizing for 60 min;
s3, secondary homogenization: filtering the primary homogenized reaction solution by using a 500-mesh screen under the condition of 130MPa, then feeding the filtered reaction solution into a homogenizer at a feeding speed of 200L/h, homogenizing for 300min, and standing the homogenized material solution overnight;
s4, spray drying: drying the supernatant of the calcium aspartate after standing by using an instant drying technology of spray drying at 180 ℃, and controlling the water content of the product to be not higher than 5%;
s5, sieving: the calcium aspartate powder after spray drying is sieved by a sieve of 80 meshes and is subpackaged into 90 g/barrel to obtain the finished product.
The detection method is carried out according to the indexes of GB 29226: the product contains calcium 12.7%, L-aspartic acid 82.3%, pH 7.00, water 4.38%, lead 0.05mg/kg, and total arsenic 0.15 mg/kg.
Example 3
Figure BDA0002555301920000051
The preparation method comprises the following steps:
s1, burdening reaction: adding the raw materials into a reaction kettle according to a proportion, and reacting for 1h at 70 ℃ and pH of 5.5; when the pH value of the reaction liquid is 6.5, preserving the temperature for 8 min;
s2, primary homogenization: filtering the reaction solution through a 100-mesh pipeline filter under the condition of 70MPa, feeding the reaction solution into a homogenizer at the feeding speed of 800L/h, and collecting filtrate after homogenizing for 60 min;
s3, secondary homogenization: filtering the primary homogenized reaction solution by using a 500-mesh screen under the condition of 120MPa, then feeding the filtered reaction solution into a homogenizer at the feeding speed of 150L/h, homogenizing for 200min, and standing the homogenized material solution overnight;
s4, spray drying: drying the supernatant of the calcium aspartate after standing by using an instant drying technology of spray drying at 250 ℃, and controlling the water content of the product to be not higher than 5%;
s5, sieving: and (3) sieving the spray-dried calcium aspartate powder by a sieve of 80 meshes, and subpackaging into 90 g/barrel to obtain the finished product.
The detection method is carried out according to the indexes of GB 29226: the product contains calcium 12.5%, L-aspartic acid 82.0%, pH 7.02, water 4.43%, lead 0.03mg/kg, and total arsenic 0.11 mg/kg.
It should be noted that when the following claims refer to numerical ranges, it should be understood that both ends of each numerical range and any value between the two ends can be selected, and since the steps and methods used are the same as those of the embodiments, the preferred embodiments of the present invention have been described for the purpose of preventing redundancy, but once the basic inventive concept is known, those skilled in the art may make other variations and modifications to the embodiments. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (4)

1. The preparation method of calcium aspartate is characterized by comprising the following steps:
s1, mixing 0.9-1.1 parts of L-aspartic acid, 0.1-0.3 part of calcium carbonate, 0.1-0.3 part of calcium hydroxide and 3.2 parts of pure water according to parts by weight, and reacting at 65-85 ℃ and pH of 5.3-6.0 for 0.5-1 h; when the pH value of the reaction liquid is 6.1-6.5, preserving the heat for 5-10 min;
s2, primary homogenization: filtering the reaction solution obtained in the step S1 under 60-80MPa, and homogenizing for 30-60 min;
s3, secondary homogenization: filtering the reaction solution after primary homogenization at 90-130MPa, and then homogenizing for 150-300 min;
and S4, standing and precipitating the reaction solution after secondary homogenization, separating to obtain a supernatant, and drying to obtain the calcium aspartate.
2. The method for preparing calcium aspartate according to claim 1, wherein the filtration in S2 is performed by passing through a 100-mesh screen, and the feeding speed during homogenization is 500-1000L/h; the filtration in step S3 is performed by a 500-mesh screen, and the feeding speed during homogenization is 120-200L/h.
3. The method for preparing calcium aspartate according to claim 1, wherein the drying in S4 is spray drying at 180 ℃ and 250 ℃, and the water content of the dried calcium aspartate is 5% or less.
4. The method for producing calcium aspartate according to claim 1, wherein the particle size of the calcium aspartate in S4 is 60 to 120 mesh.
CN202010587808.XA 2020-06-24 2020-06-24 Preparation method of calcium aspartate Pending CN111675627A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010587808.XA CN111675627A (en) 2020-06-24 2020-06-24 Preparation method of calcium aspartate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010587808.XA CN111675627A (en) 2020-06-24 2020-06-24 Preparation method of calcium aspartate

Publications (1)

Publication Number Publication Date
CN111675627A true CN111675627A (en) 2020-09-18

Family

ID=72456569

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010587808.XA Pending CN111675627A (en) 2020-06-24 2020-06-24 Preparation method of calcium aspartate

Country Status (1)

Country Link
CN (1) CN111675627A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115073315A (en) * 2022-07-06 2022-09-20 淄博润聚生物科技有限公司 Synthetic method of sodium aspartate and calcium aspartate

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002032235A2 (en) * 2000-10-19 2002-04-25 Nutrapure, Inc. Process for making mineral, food or pharmaceutical grade salt products
US20040214883A1 (en) * 2003-04-28 2004-10-28 Hagen Brent P. Calcium monoaspartate
CN102731331A (en) * 2012-06-21 2012-10-17 上海腾瑞医药技术有限公司 L-calcium aspartate and its preparation method
CN107417556A (en) * 2017-05-23 2017-12-01 王广生 L aspartase calciums and preparation method thereof
CN108976142A (en) * 2018-08-22 2018-12-11 上海青平药业有限公司 A kind of preparation method of ASPARTIC ACID calcium
CN110511155A (en) * 2019-08-15 2019-11-29 河北力维素科技有限公司 A kind of preparation method of asparatate mineral sequestration object and its salt

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002032235A2 (en) * 2000-10-19 2002-04-25 Nutrapure, Inc. Process for making mineral, food or pharmaceutical grade salt products
US20040214883A1 (en) * 2003-04-28 2004-10-28 Hagen Brent P. Calcium monoaspartate
CN102731331A (en) * 2012-06-21 2012-10-17 上海腾瑞医药技术有限公司 L-calcium aspartate and its preparation method
CN107417556A (en) * 2017-05-23 2017-12-01 王广生 L aspartase calciums and preparation method thereof
CN108976142A (en) * 2018-08-22 2018-12-11 上海青平药业有限公司 A kind of preparation method of ASPARTIC ACID calcium
CN110511155A (en) * 2019-08-15 2019-11-29 河北力维素科技有限公司 A kind of preparation method of asparatate mineral sequestration object and its salt

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
戎舜城: "天门冬氨酸钙合成的研究" *
戎舜城: "天门冬氨酸钙合成的研究", 《中国食品添加剂》 *
李金: "天冬氨酸钙的合成与分离提纯" *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115073315A (en) * 2022-07-06 2022-09-20 淄博润聚生物科技有限公司 Synthetic method of sodium aspartate and calcium aspartate

Similar Documents

Publication Publication Date Title
CN105012940B (en) A kind of preparation method of nanometre collagen peptide chelated zinc
CN101979655B (en) Enzyme method for producing mung bean peptide
CN111675627A (en) Preparation method of calcium aspartate
CN110357978A (en) A kind of preparation method of selenide of carragheen
CN106349095A (en) Threonine crystal extraction process
CN111073933A (en) Preparation method of protein peptide selenium chelate suitable for ruminants
CN102793720A (en) Method for solving crystal substance precipitation of mixed sugar electrolyte injection after disinfection
CN108373421B (en) Preparation method of L-aspartic acid chelated calcium
CN102038084B (en) Premix containing iron sucrose for raising pigs
CN102335199B (en) Microwave-hydrolyzation method of pearl powder
CN103070845A (en) Starch hollow capsule and preparation method thereof
CN102557920B (en) Process for producing calcium citrate
CN111493210A (en) Preparation method of metal ion peptide nutritional supplement
CN108640744A (en) A kind of mill water culture nutrient solution and preparation method thereof
CN103980140A (en) Abalone shell sourced calcium glutamate and preparation method thereof
CN110292147A (en) Nutrition intelligence development organic rice powder and rice paste
CN111943234A (en) Method for preparing medicinal sterile sodium bicarbonate granules with large particle size
CN112168864A (en) Cannabidiol and NMN preparation formula and preparation method thereof
CN112479866B (en) Method for co-producing citric acid complex calcium, malic acid complex calcium and fruit acid chelate calcium products
CN110973596A (en) Infant rice flour rich in easily-absorbed zinc trace element nutrition enhancer
CN109393456A (en) A kind of oyster extract and preparation method thereof rich in natural taurine
CN116406754B (en) Natural red date fulvic acid beverage and preparation method thereof
CN108840904B (en) Method for extracting selenoprotein from tobacco leaves
CN110157754B (en) Production process of water-soluble marine organism calcium
CN106434781A (en) Clean production process of L-glutamine by adopting fermentation method

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
RJ01 Rejection of invention patent application after publication

Application publication date: 20200918

RJ01 Rejection of invention patent application after publication