CN1257062A - Process for preparing calcium citrate malate by using citric acid, malic acid and calcium carbonate - Google Patents
Process for preparing calcium citrate malate by using citric acid, malic acid and calcium carbonate Download PDFInfo
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- CN1257062A CN1257062A CN 99124065 CN99124065A CN1257062A CN 1257062 A CN1257062 A CN 1257062A CN 99124065 CN99124065 CN 99124065 CN 99124065 A CN99124065 A CN 99124065A CN 1257062 A CN1257062 A CN 1257062A
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Abstract
A preparation method of calcium citromalate is technically characterized by that according to a specific mixing ratio of citric acid, malic acid and calcium carbonate, adding a certain quantity of water to obtain a solution, fully reacting and controlling reaction temp. and reaction time in the course of reaction, continuously stirring until the product is crystallized and separated out, dewatering, washing, dewatering, drying, cooling and pulverizing so as to obtain the invented product calcium citromalate which can be used as good calcium-supplementing agent and food additive.
Description
The present invention relates to a kind of method of utilizing special proportioning between citric acid, oxysuccinic acid, the lime carbonate to produce calcium cirate malate.
Calcium cirate malate (CCM) is a kind of metastable state compound that adopts lime carbonate (or calcium oxide or calcium hydroxide) and citric acid, oxysuccinic acid to make under the certain reaction condition.This product solubleness in water is big, and it is the compound form of the highest a kind of calcium of bio-absorbable.
The KAWAI SHIRO of Japan has described the citrate of lime of its development and the coordination compound of calcium malate in the patent of application in 1981, by lime carbonate, citric acid, oxysuccinic acid reaction make.Calcium, citric acid, oxysuccinic acid proportioning are 5: 2: 2 in the product, this compound of solubilized 0.5g in 100 ml waters in the time of 20 ℃.
U.S.'s Prolongert---Gamble Co., Ltd calcium, citric acid, oxysuccinic acid proportioning in the CCM of development in 1993 are 6: 2: 2, solubilized 1.1 these products of gram in 100 ml waters during 20.73%, 25 ℃ of calcium content in the product.
Calcium, citric acid, oxysuccinic acid proportioning (, be divided into single even numbers and arrange two series): (1) 3 (2i+1): (2i+1): (3i+1) make i=1,2 among the CCM of our development by citrate, 3,4,5 ... n (2) 3 (2i+2): (2i+2): (3i+2) make i=1,2,3,4,5, calcium content 22.21%-23.66% in the n product, in the time of 20 ℃ in 100 ml waters solubilized 0.5-1.1 restrain this product (seeing the embodiment of the invention for details)
Technical characterictic of the present invention is:
A. starting material are carried out purifying treatment, remove various impurity in the starting material, press calcium among the CCM, the proportioning of citric acid, oxysuccinic acid is (by citrate, be divided into single even numbers and arrange two series): (1) 3 (2i+1): (2i+1): (3i+1) make i=1,2,3,4,5, n (2) 3 (2i+2): (2i+2): (3i+2) make i=1,2,3,4,5 ... fully react behind n and water (water yield is 2.5-3 a times of the above-mentioned three kinds of starting material gross weights) wiring solution-forming, its temperature of reaction is controlled at 20 ℃-80 ℃.
B. feed above-mentioned solution with pressurized air, ceaselessly stir, last 1.5-2 hour with pressurized air.
C. after passing through above-mentioned two steps, product is after crystallization is separated out from reaction solution, promptly gets calcium cirate malate through dehydration, washing, dehydration, dry, cooling, after pulverizing.
The present invention compared with prior art has the following advantages: product grade and quality height, and the product purity height, product calcium content height, the simple cost of production technique is low.
Embodiments of the invention:
1. by proportioning of calcium, citric acid, oxysuccinic acid among the CCM (odd number arranges 1) 9: 3: 4 and water (water yield is 2.7 times of above-mentioned three kinds of raw material gross weights) wiring solution-forming, fully react, 37 ℃ of temperature of reaction, after 1 hour 50 minutes reaction times, after the product crystallization is separated out, after dehydration, washing, dehydration, drying, cooling, pulverizing, its quality index of products obtained therefrom is: calcium contents (butt) 22.91%; Arsenic content＜0.5PPM; Lead content＜1PPM; This product 0.847 gram of dissolving in 100 ml waters in the time of 20 ℃.
2. by proportioning of calcium, citric acid, oxysuccinic acid among the CCM (even numbers arranges 1) 12: 4: 5 and water (water yield is 2.7 times of above-mentioned three kinds of raw material gross weights) wiring solution-forming, fully react, 50 ℃ of temperature of reaction, after 2 hours reaction times, after the product crystallization is separated out, through dehydration, washing, dehydration, dry, cooling, pulverize after its quality index of products obtained therefrom be: calcium contents (butt) 22,49%; Arsenic content＜0.5PPM; This product 0.989 gram of dissolving in 100 ml waters in the time of lead content＜1PPM20 ℃.
Claims (1)
1. one kind is utilized the special proportioning between citric acid, oxysuccinic acid, the lime carbonate, produces the method for calcium cirate malate.
Its feature:
A. starting material are carried out purifying treatment, remove various impurity in the starting material, by the proportioning of calcium, citric acid, oxysuccinic acid among the CCM (by citrate, be divided into single even numbers and arrange two series): (1) 3 (2i+1): (2i+1): (3i+1) make i=1,2,3,4,5 ... n (2) 3 (2i+2): (2i+2): (3i+2) make i=1,2,3,4,5, fully react behind n and water (water yield is 2.5-3 a times of the above-mentioned three kinds of starting material gross weights) wiring solution-forming, its temperature of reaction is controlled at 20 ℃-80 ℃.
B. feed above-mentioned solution with pressurized air, ceaselessly stir, last 1.5-2 hour with pressurized air.
C. after passing through above-mentioned two steps, product crystallization from reaction solution is separated out, and promptly gets calcium cirate malate through dehydration, washing, dehydration, dry, cooling, after pulverizing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99124065A CN1086378C (en) | 1999-11-23 | 1999-11-23 | Process for preparing calcium citrate malate by using citric acid, malic acid and calcium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99124065A CN1086378C (en) | 1999-11-23 | 1999-11-23 | Process for preparing calcium citrate malate by using citric acid, malic acid and calcium carbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1257062A true CN1257062A (en) | 2000-06-21 |
| CN1086378C CN1086378C (en) | 2002-06-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99124065A Expired - Fee Related CN1086378C (en) | 1999-11-23 | 1999-11-23 | Process for preparing calcium citrate malate by using citric acid, malic acid and calcium carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1086378C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7504536B2 (en) | 2006-08-17 | 2009-03-17 | The Procter & Gamble Company | Compositions comprising calcium citrate malate and methods for making the same |
| US8889195B2 (en) | 2006-08-17 | 2014-11-18 | The Procter & Gamble Company | Compositions comprising calcium citrate malate and methods for making the same |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5186965A (en) * | 1990-06-14 | 1993-02-16 | The Procter & Gamble Company | Calcium citrate malate composition |
| DE69227320T2 (en) * | 1991-12-26 | 1999-06-02 | Procter & Gamble | STORAGE BEVERAGE CONCENTRATES WITH CALCIUM ADDITIVE |
| CN1160503A (en) * | 1995-12-28 | 1997-10-01 | 田中四郎 | Soluble concentrated frozen/refrigerated calcium preparation comprising calcium citrate-malate and process for producing the same |
-
1999
- 1999-11-23 CN CN99124065A patent/CN1086378C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7504536B2 (en) | 2006-08-17 | 2009-03-17 | The Procter & Gamble Company | Compositions comprising calcium citrate malate and methods for making the same |
| US8889195B2 (en) | 2006-08-17 | 2014-11-18 | The Procter & Gamble Company | Compositions comprising calcium citrate malate and methods for making the same |
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| Publication number | Publication date |
|---|---|
| CN1086378C (en) | 2002-06-19 |
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