CN101531609A - Method for preparing calcium glycine - Google Patents
Method for preparing calcium glycine Download PDFInfo
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- CN101531609A CN101531609A CN200910030767A CN200910030767A CN101531609A CN 101531609 A CN101531609 A CN 101531609A CN 200910030767 A CN200910030767 A CN 200910030767A CN 200910030767 A CN200910030767 A CN 200910030767A CN 101531609 A CN101531609 A CN 101531609A
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Abstract
The invention discloses a method for preparing calcium glycine, which comprises the following steps: respectively taking 15 to 30 weight percent of glycin, 0.8 to 15 weight percent of mineral calcium and 60 to 80 weight percent of water, mixing and stirring the raw materials in a reaction kettle to make the raw materials fully dissolved, performing reaction for 3 to 24 hours by heating at a temperature between 30 and 80 DEG C, and then standing for 6 to 24 hours; taking reaction solution, and performing spray drying or freeze drying to obtain a dry substance; and crushing the dry substance, passing through a 80 to 120-mesh sieve, performing sterilizing and split charging. The method for preparing the calcium glycine has easily obtained raw material used, scientific and reasonable mixture ratio of the raw materials, simple preparation process, high yield of the synthesized calcium glycine, low cost and suitability for industrial production.
Description
Technical field
The invention discloses a kind of preparation method of compound, specifically disclose a kind of preparing calcium glycine.
Background technology
China's different ages, the crowd of different occupation, calcium intake is generally on the low side, on average take in calcium for each person every day and have only 400mg, only recommend to take in about 50% of calcium amount for Chinese Soclety of Nutrition, the phenomenon of children and teenager's calcium deficiency is even more serious, has 70% to 80% children and teen-age calcium intake not to reach and recommends 50% of feed rate.The calcium replenishing product of present domestic use, major part is the Calcium of intensifiens of the first-generation and the common organic salt calcium of the s-generation, first-generation calsium supplement (Calcium of intensifiens) wherein, actual is exactly calcium oxide or lime carbonate, this product is strong basicity (pH value〉12), in human stomach, to consume a large amount of hydrochloric acid in gastric juice, very big to gastric irritation, and the calcium nutrition that replenishes is difficult to absorb, as life-time service or excessively be easy to cause calculi in vivo or maldigestion, s-generation calsium supplement (common organic salt calsium supplement), this type of calcium is generally: calcium lactate, calcium acetate, calisanin, Tricalcium dicitrate or calcium maleate generally have only 30% or lower in the intravital specific absorption of people, compare with first kind product not have much improvement.Calcium glycinate proves through clinical trial, it is a kind of small molecules organic calcium of biologically active, superior Bc is arranged, it is effective carrier as calcium ion, can be by the biologically active substance that allows after the cytolemma identification to pass through, very permeable is crossed cytolemma on the intestines, is directly absorbed by enteron aisle, therefore can reach the absorptive capacity of 90% above specific absorption and 180mg/kg.But present preparing calcium glycine, the synthetic ratio of finished product is low, complex process, cost is higher.
Summary of the invention
Goal of the invention: the objective of the invention is provides a kind of technology simple preparing calcium glycine in order to solve the deficiencies in the prior art.
Technical scheme: for realizing purpose of the present invention, preparing calcium glycine provided by the invention may further comprise the steps:
(1) gets glycine, minerals calcium, water respectively and in reactor, mix, stir and make abundant dissolving,, left standstill 6 to 24 hours 30 to 80 ℃ of following reacting by heating 3 to 24 hours;
(2) get the reaction solution of step (1) gained, spraying drying or lyophilize, dry thing;
(3) get step (2) gained dry thing, pulverizing, cross 80 to 120 mesh sieves, sterilization, packing.
Wherein the weight percent of the used glycine of step (1) is that the weight percent of 15-30%, minerals calcium is that the weight percent of 0.8-15%, water is 60-80%, is that the weight percent of 17-25%, minerals calcium is that the weight percent of 1-10%, water is 70-80% as the weight percent of the used glycine of another program step (1).
As preferred version, wherein used glycine, minerals calcium, water three's weight ratio is 2.5:1.0:6.5 in the step (1), and temperature of reaction is 40 to 70 ℃, and the reaction times is 5 to 18 hours.
As another preferred version, wherein used glycine, minerals calcium, water three's weight ratio is 2.1:0.9:7 in the step (1), and temperature of reaction is 50 to 60 ℃, and the reaction times is 6 to 8 hours.
As another preferred version, wherein used glycine, minerals calcium, water three's weight ratio is 1.8:1.3:6.9 in the step (1), and temperature of reaction is 55 ℃, and the reaction times is 6 hours.
Wherein above-described minerals calcium is one of calcium oxide, lime carbonate, Calcium hydrogen carbonate or their mixture, and used water is pure water or redistilled water.
As the used calcium oxide of preferred version the present invention, lime carbonate or Calcium hydrogen carbonate is nano level calcium oxide, lime carbonate or Calcium hydrogen carbonate.
As preferred version, spray-dired temperature is 220～280 ℃ in the step of the present invention (2), and step (3) is pulverized the back and crossed 90 to 100 purposes sieve.
As preferred scheme, spray-dired temperature is 280 ℃ in the step of the present invention (2), and step (3) is pulverized the back and crossed 100 purposes sieve.
Beneficial effect: used raw material is easy to get in the method for preparing Calcium glycinate provided by the invention, proportioning is scientific and reasonable between the raw material, through lot of experiments, generate the productive rate height of Calcium glycinate during glycine provided by the invention, minerals calcium, water three's weight ratio 2.1:0.9:7.The present invention selects glycine and calcium oxide for use, the preparation technology of lime carbonate or Calcium hydrogen carbonate reaction is simple, adopt spraying drying, make finished product Calcium glycinate contained humidity few, constant product quality, pulverize the back and cross 80 to 120 orders, particle diameter is little, the human absorptivity is higher, and preparation method provided by the invention the productive rate height of synthetic Calcium glycinate, cost is lower, be fit to suitability for industrialized production, the Calcium glycinate that obtains by preparation method of the present invention is that two glycine and a calcium ion bonded inner complex are arranged, in human intestinal not can because of with food in oxalic acid, the combination of acidic substance such as humic acid and loss, and can not cause calculosis therefrom, calcium level is stable, and better tolerance has no adverse reaction.
Description of drawings
Accompanying drawing is the process flow sheet of preparation Calcium glycinate.
Embodiment:
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment only is used to the present invention is described and is not used in and limit the scope of the invention, after having read the present invention, those skilled in the art all fall within the application's claims institute restricted portion to the modification of the various equivalent form of values of the present invention.
Embodiment 1
Get raw material glycine 210kg, calcium oxide 90kg and water 700kg, put in the reactor and mix, stir and make abundant dissolving, reaction is 5 hours under 30 ℃ of temperature, extracts reaction solution, and leaves standstill 8 hours; 280 ℃ of following spraying dryings, detect moisture content, make the moisture weight percentage be lower than 9%, get dry thing 210kg, get dry thing, pulverizing, cross 100 mesh sieves, sterilization, packing.
Embodiment 2
Get raw material glycine 300kg, calcium oxide 100kg and water 60kg, put in the reactor and mix, stir and make abundant dissolving, reaction is 12 hours under 70 ℃ of temperature, leaves standstill 10 hours; Extract reaction solution,, detect moisture content, make the moisture weight percentage be lower than 7%, get dry thing 270kg, get dry thing, pulverizing, cross 80 mesh sieves, sterilization, packing 200 ℃ of following spraying dryings.
Embodiment 3
Get raw material glycine 150kg, lime carbonate 80kg and water 770kg, put in the reactor and mix, stir and make abundant dissolving, reaction is 18 hours under 55 ℃ of temperature, leaves standstill 12 hours; Extract reaction solution,, detect moisture content, make the moisture weight percentage be lower than 8%, get dry thing 142kg, get dry thing, pulverizing, cross 120 mesh sieves, sterilization, packing 250 ℃ of following spraying dryings.
Embodiment 4
Get raw material glycine 200kg, lime carbonate 150kg and water 650kg, put in the reactor and mix, stir and make abundant dissolving, reaction is 24 hours under 75 ℃ of temperature, leaves standstill 16 hours; Extract reaction solution,, detect moisture content, make the moisture weight percentage be lower than 9%, get dry thing 195kg, get dry thing, pulverizing, cross 100 mesh sieves, sterilization, packing 280 ℃ of following spraying dryings.
Embodiment 5
Get raw material glycine 250kg, Calcium hydrogen carbonate 100kg and water 650kg, put in the reactor and mix, stir and make abundant dissolving, reaction is 12 hours under 80 ℃ of temperature, leaves standstill 24 hours; Extract reaction solution, lyophilize detects moisture content, makes the moisture weight percentage be lower than 9%, gets dry thing 251kg, gets dry thing, pulverizing, crosses 100 mesh sieves, sterilization, packing.
Embodiment 6
Get raw material glycine 300kg, nano level carbonic acid hydrogen calcium 150kg and water 600kg, put in the reactor and mix, stir and make abundant dissolving, reaction is 8 hours under 60 ℃ of temperature, leaves standstill 6 hours; Extract reaction solution, lyophilize detects moisture content, makes the moisture weight percentage be lower than 9%, gets dry thing 306kg, gets dry thing, pulverizing, crosses 100 mesh sieves, sterilization, packing.
Embodiment 7
Get raw material glycine 260kg, the mixture 110kg of nano level calcium oxide and Calcium hydrogen carbonate and water 630kg put in the reactor and mix, and stir and make abundant dissolving, and reaction is 10 hours under 65 ℃ of temperature, leaves standstill 12 hours; Extract reaction solution, lyophilize detects moisture content, makes the moisture weight percentage be lower than 9%, gets dry thing 258kg, gets dry thing, pulverizing, crosses 90 mesh sieves, sterilization, packing.
Embodiment 8
Get raw material glycine 250kg, the mixture 120kg of calcium oxide, Calcium hydrogen carbonate and lime carbonate and water 630kg put in the reactor and mix, and stir and make abundant dissolving, and reaction is 8 hours under 70 ℃ of temperature, leaves standstill 17 hours; Extract reaction solution,, detect moisture content, make the moisture weight percentage be lower than 9%, get dry thing 243kg, get dry thing, pulverizing, cross 110 mesh sieves, sterilization, packing 280 ℃ of following spraying dryings.
Claims (10)
1, a kind of preparing calcium glycine is characterized in that may further comprise the steps:
(1) gets glycine, minerals calcium, water respectively and in reactor, mix, stir and make abundant dissolving,, left standstill 6 to 24 hours 30 to 80 ℃ of following reacting by heating 3 to 24 hours;
(2) get the reaction solution of step (1) gained, spraying drying or lyophilize, dry thing;
(3) get step (2) gained dry thing, pulverizing, cross 80 to 120 mesh sieves, sterilization, packing.
2, preparing calcium glycine according to claim 1 is characterized in that: the weight percent of the described glycine of step (1) is that the weight percent of 15-30%, minerals calcium is that the weight percent of 0.8-15%, water is 60-80%.
3, preparing calcium glycine according to claim 2 is characterized in that: the weight percent of the described glycine of step (1) is that the weight percent of 17-25%, minerals calcium is that the weight percent of 1-10%, water is 70-80%.
4, preparing calcium glycine according to claim 3 is characterized in that: used glycine, minerals calcium, water three's weight ratio is 2.5:1.0:6.5 in the step (1), and temperature of reaction is 40 to 70 ℃, and the reaction times is 5 to 18 hours.
5, preparing calcium glycine according to claim 3 is characterized in that: used glycine, minerals calcium, water three's weight ratio is 2.1:0.9:7 in the step (1), and temperature of reaction is 50 to 60 ℃, and the reaction times is 6 to 8 hours.
6, preparing calcium glycine according to claim 3 is characterized in that: used glycine, minerals calcium, water three's weight ratio is 1.8:1.3:6.9 in the step (1), and temperature of reaction is 55 ℃, and the reaction times is 6 hours.
7, according to each described preparing calcium glycine of claim 1 to 6, it is characterized in that: used minerals calcium is one of calcium oxide, lime carbonate, Calcium hydrogen carbonate or their mixture in the step (1), and used water is pure water or redistilled water.
8, preparing calcium glycine according to claim 7 is characterized in that: described calcium oxide, lime carbonate or Calcium hydrogen carbonate are nano level.
8, preparing calcium glycine according to claim 1 is characterized in that: spray-dired temperature is 200～280 ℃ in the step (2), and step (3) is pulverized the back and crossed 90 to 100 mesh sieves.
9, preparing calcium glycine according to claim 8 is characterized in that: spray-dired temperature is 280 ℃ in the step (2), and step (3) is pulverized the back and crossed 100 mesh sieves.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910030767A CN101531609A (en) | 2009-04-15 | 2009-04-15 | Method for preparing calcium glycine |
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| CN200910030767A CN101531609A (en) | 2009-04-15 | 2009-04-15 | Method for preparing calcium glycine |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102011011924A1 (en) | 2011-02-17 | 2012-08-23 | Isf Gmbh | Process for the preparation of amino acid chelate compounds, amino acid chelate compounds and use of amino acid chelate compounds |
| CN105595346A (en) * | 2015-09-01 | 2016-05-25 | 张伟 | Liquid preparation for calcium supplementation and preparation method thereof |
| CN106146328A (en) * | 2016-08-02 | 2016-11-23 | 河北东华冀衡化工有限公司 | A kind of preparation method of calcium glycine chelate |
| 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 |
| CN110437057A (en) * | 2019-08-20 | 2019-11-12 | 长江大学 | A kind of synthetic method of caprylic acid calcium |
-
2009
- 2009-04-15 CN CN200910030767A patent/CN101531609A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102011011924A1 (en) | 2011-02-17 | 2012-08-23 | Isf Gmbh | Process for the preparation of amino acid chelate compounds, amino acid chelate compounds and use of amino acid chelate compounds |
| CN105595346A (en) * | 2015-09-01 | 2016-05-25 | 张伟 | Liquid preparation for calcium supplementation and preparation method thereof |
| CN106146328A (en) * | 2016-08-02 | 2016-11-23 | 河北东华冀衡化工有限公司 | A kind of preparation method of calcium glycine chelate |
| 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 |
| CN110437057A (en) * | 2019-08-20 | 2019-11-12 | 长江大学 | A kind of synthetic method of caprylic acid calcium |
| CN110437057B (en) * | 2019-08-20 | 2022-04-05 | 长江大学 | Synthesis method of calcium n-octoate |
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Application publication date: 20090916 |