CN102127107B - Preparation method of calcium glycerophosphate with high calcium content - Google Patents
Preparation method of calcium glycerophosphate with high calcium content Download PDFInfo
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- CN102127107B CN102127107B CN 201010586713 CN201010586713A CN102127107B CN 102127107 B CN102127107 B CN 102127107B CN 201010586713 CN201010586713 CN 201010586713 CN 201010586713 A CN201010586713 A CN 201010586713A CN 102127107 B CN102127107 B CN 102127107B
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Abstract
The invention discloses a preparation method of calcium glycerophosphate with high calcium content. The preparation method comprises the following steps of: (i) synthetic reaction: putting glycerol, monocalcium phosphate and phosphoric acid into an agitated reactor in proportion, and simultaneously adding a small amount of citric acid to undergo a synthetic reaction; (ii) diluting; (iii) filtering; (iv) concentrating; (v) precipitating; (vi) drying, and the like. The calcium glycerophosphate product prepared by adopting the preparation method disclosed by the invention has stable quality and high calcium content up to more than 95 percent and can simultaneously meet requirements of a calcium supplement and a toothpaste additive.
Description
Technical field
The invention belongs to a kind of preparation method of neurosin, be specifically related to a kind of preparation method of neurosin of high calcium content.
Background technology
Neurosin can be used as toothpaste additive, chewing gum additive, food enrichment and medicine etc., uses comparatively extensive.At present, the neurosin of domestic industry production can be divided into two kinds of specifications substantially: the first specification has good solubleness, but calcium contents is on the low side; The second specification calcium content is higher, but solubleness is not up to standard.There is larger difference in the product processes of different size, and the product of producing can not satisfy the needs of a plurality of industries simultaneously.
Summary of the invention
The present invention proposes in order to overcome the shortcoming that exists in the prior art, and purpose provides a kind of preparation method of neurosin of high calcium content.
Technical scheme of the present invention is: a kind of preparation method of neurosin of high calcium content may further comprise the steps:
(ⅰ) building-up reactions
With glycerine: monocalcium phosphate: the raw material that phosphoric acid molar ratios equals 1.5:0.1～0.2:1 drops in the reactor, 1%～3% the citric acid that adds simultaneously above-mentioned reactant gross weight, carry out building-up reactions, this reaction is carried out in two stages, fs: under the normal pressure, 80 ℃ of temperature kept 0.5 hour; Fs: vacuum tightness 0.08MPa, 140 ℃ of temperature kept 7.5 hours;
(ⅱ) dilution
Above-mentioned esterification products is let cool to about 80 ℃, and the pure water that adds 4 times of its weight dilutes normal pressure, 100～120 ℃, stirring and refluxing 2 hours;
(ⅲ) filter
Above-mentioned product is chilled to room temperature, under the agitation condition, adds above-mentioned product take the technical grade calcium hydroxide dirty solution of mass percent concentration as 4%, regulate its PH to 8.0～9.0, kept 3 hours, filter, remove solid;
(ⅳ) concentrated
Measure above-mentioned filtrate, volume is designated as V, begins to concentrate, and when the volume that steams water is 2V/3, stops to concentrate;
(ⅴ) precipitation
Slowly add the reagent grade ethanol of V/6 volume in the above-mentioned concentrated solution, fully stir, neurosin is precipitated out;
(ⅵ) drying
Under agitation condition, with the mixture input spray-drier of neurosin solid, second alcohol and water, the steam of alcohol and water directly passes into the ethanol recovery tower, separates to obtain ethanol and pure water; Collect dried white solid powder, be the Phosphoric acid glycerol esters calcium product.
Described glycerine, monocalcium phosphate, phosphoric acid and citric acid all adopt food grade.
Described calcium hydroxide is technical grade.
The neurosin constant product quality of the present invention's preparation, calcium contents can satisfy the requirement of calsium supplement and toothpaste additive simultaneously up to more than 95%.
Embodiment
Below, with reference to embodiment the preparation method of the neurosin of a kind of high calcium content of the present invention is elaborated.
A kind of preparation method of neurosin of high calcium content may further comprise the steps:
(ⅰ) building-up reactions
With glycerine: monocalcium phosphate: the raw material that phosphoric acid molar ratios equals 1.5:0.1～0.2:1 drops in the reactor, 1%～3% the citric acid that adds simultaneously above-mentioned reactant gross weight, carry out building-up reactions, this reaction is esterification, and above-mentioned each component all adopts food grade.
The fs is carried out in this reaction in two stages: under the normal pressure, 80 ℃ of temperature kept 0.5 hour; Fs: vacuum tightness 0.08MPa, 140 ℃ of temperature kept 7.5 hours.
Before reaction, add a small amount of citric acid, utilize the huge legendary turtle cooperation of citric acid with the solubleness that can increase monocalcium phosphate, make its attend fully esterification, be beneficial to the calcium contents that improves final Phosphoric acid glycerol esters calcium product.
(ⅱ) dilution
Above-mentioned esterification products is let cool to about 80 ℃, and the pure water that adds 4 times of its weight dilutes normal pressure, 100～120 ℃, stirring and refluxing 2 hours.
(ⅲ) filter
Above-mentioned product is chilled to room temperature, under the agitation condition, with the 4%(mass percent concentration) technical grade calcium hydroxide dirty solution add above-mentioned product, regulate its PH to 8.0～9.0, kept 3 hours, filter, remove solid.
(ⅳ) concentrated
Measure above-mentioned filtrate, volume is designated as V, begins to concentrate, and when the volume that steams water is 2V/3, stops to concentrate.
(ⅴ) precipitation
Slowly add the reagent grade ethanol of V/6 volume in the above-mentioned concentrated solution, fully stir, neurosin is precipitated out.
(ⅵ) drying
Under agitation condition, with the mixture input spray-drier of neurosin solid, second alcohol and water, the steam of alcohol and water directly passes into the ethanol recovery tower, separates to obtain ethanol and pure water; Collect dried white solid powder, be the Phosphoric acid glycerol esters calcium product.
Embodiment 1
40 gram glycerine, 8 gram monocalcium phosphates, 32.7 gram phosphoric acid, 0.08 gram citric acid are put into equipment condensation division box, in the reactor with agitator.Open and stir, fully stirred 20 minutes, begin heating, when temperature rises to 80 ℃, kept 0.5 hour, guarantee that solid matter fully dissolves in the reaction raw materials.Begin to vacuumize, and continue to heat up, during to 140 ℃ of vacuum tightness 0.08MPa, temperature, kept 7.5 hours.
Esterification finishes, and water weight 30.8 grams in the metering collector converse in the reactor approximately 50 grams of esterification products weight.Product lets cool to about 80 ℃, adds 200 milliliters of pure water, normal pressure, 105 ℃, and stirring and refluxing 2 hours obtains safran transparent acid liquid.
Under the agitation condition, add the 4%(mass percent concentration) the calcium hydroxide dirty solution, behind regulation system PH to 8.0～9.0, successive reaction 3 hours, solids removed by filtration impurity.
3200 milliliters of filtrates adopt rotary evaporation concentrated, when 80 ℃ of oil bath heating, 1650 milliliters of accumulative total water outlets, stop to concentrate.1200 milliliters of remaining liqs slowly add 600 milliliter of 95% ethanol and fully stir, and have a large amount of white precipitates to generate.
Continue to stir, adopt peristaltic pump to suck spraying drying with the speed of 100ml/min, temperature in is set 120 ℃, and temperature out is set 90 ℃.White powder is neurosin after dry, and after testing, its calcium contents is 96.46%, and other indexs all meet the requirements.
Embodiment 2
141 gram glycerine, 41 gram monocalcium phosphates, 115.3 gram phosphoric acid, 5.6 gram citric acids are put into equipment condensation division box, in the reactor with agitator.Stir 20 minutes post-heating and be warming up to 80 ℃, kept 0.5 hour, solid matter fully dissolves in the reaction raw materials.Begin to vacuumize, and continue to heat up, during to 140 ℃ of vacuum tightness 0.08MPa, temperature, kept 7.5 hours.
Esterification finishes, and water weight 97.6 grams in the metering collector converse in the reactor approximately 205 grams of esterification products weight.Product lets cool to about 80 ℃, adds 820 milliliters of pure water, normal pressure, 110 ℃, and stirring and refluxing 2 hours obtains safran transparent acid liquid.
Under the agitation condition, add the 4%(mass percent concentration) the calcium hydroxide dirty solution, behind regulation system PH to 8.0～9.0, successive reaction 3 hours, solids removed by filtration impurity.
10500 milliliters of filtrates adopt rotary evaporation concentrated, when 80 ℃ of oil bath heating, 7050 milliliters of accumulative total water outlets, stop to concentrate.3100 milliliters of remaining liqs slowly add 1600 milliliter of 95% ethanol and fully stir, and have a large amount of white precipitates to generate.
Continue to stir, adopt peristaltic pump to suck spraying drying with the speed of 100ml/min, temperature in is set 120 ℃, and temperature out is set 90 ℃.White powder is neurosin after dry, and after testing, its calcium contents is 98.06%, and other indexs all meet the requirements.
Embodiment 3
70 gram glycerine, 27.18 gram monocalcium phosphates, 57.2 gram phosphoric acid, 0.5 gram citric acid are put into equipment condensation division box, in the reactor with agitator.Open and stir, fully stirred 20 minutes, begin heating, when temperature rises to 80 ℃, kept 0.5 hour, guarantee that solid matter fully dissolves in the reaction raw materials.Begin to vacuumize, and continue to heat up, during to 140 ℃ of vacuum tightness 0.08MPa, temperature, kept 7.5 hours.
Esterification finishes, and water weight 44.5 grams in the metering collector converse in the reactor approximately 110 grams of esterification products weight.Product lets cool to about 80 ℃, adds 440 milliliters of pure water, normal pressure, 115 ℃, and stirring and refluxing 2 hours obtains safran transparent acid liquid.
Under the agitation condition, add the 4%(mass percent concentration) the calcium hydroxide dirty solution, behind regulation system PH to 8.0～9.0, successive reaction 3 hours, solids removed by filtration impurity.
4730 milliliters of filtrates adopt rotary evaporation concentrated, when 80 ℃ of oil bath heating, 2760 milliliters of accumulative total water outlets, stop to concentrate.1600 milliliters of remaining liqs slowly add 800 milliliter of 95% ethanol and fully stir, and have a large amount of white precipitates to generate.
Continue to stir, adopt peristaltic pump to suck spraying drying with the speed of 100ml/min, temperature in is set 120 ℃, and temperature out is set 90 ℃.White powder is neurosin after dry, and after testing, its calcium contents is 95.23%, and other indexs all meet the requirements.
Its technical target of the product is as follows:
Leading indicator standard-required (European Pharmacopoeia 63 editions) this product index
Solubleness 〉=2 grams/100 ml waters meet the requirements
Potential of hydrogen≤1.7ml/g 0.68ml/g
Solvend in free glycerol and the alcohol≤1.0% 0.29%
Loss on ignition 51.0%～57.0% 53.85%
Weight loss on drying≤12.0% 6.50%
More than Phosphoric acid glycerol esters calcium contents (butt) 〉=85% 85%.
Beneficial effect of the present invention:
The neurosin constant product quality of the present invention's preparation meets 63 editions standard-requireds of European Pharmacopoeia, and calcium contents can satisfy the requirement of calsium supplement and toothpaste additive simultaneously up to more than 85%.
Claims (3)
1. the preparation method of the neurosin of a high calcium content is characterized in that: may further comprise the steps:
(ⅰ) building-up reactions
With glycerine: monocalcium phosphate: the raw material that phosphoric acid molar ratios equals 1.5:0.1～0.2:1 drops in the reactor, 1%～3% the citric acid that adds simultaneously above-mentioned reactant gross weight, carry out building-up reactions, this reaction is carried out in two stages, fs: under the normal pressure, 80 ℃ of temperature kept 0.5 hour; Subordinate phase: vacuum tightness 0.08MPa, 140 ℃ of temperature kept 7.5 hours;
(ⅱ) dilution
Above-mentioned esterification products is let cool to about 80 ℃, and the pure water that adds 4 times of its weight dilutes normal pressure, 100～120 ℃, stirring and refluxing 2 hours;
(ⅲ) filter
Above-mentioned product is chilled to room temperature, under the agitation condition, adds above-mentioned product take the technical grade calcium hydroxide dirty solution of mass percent concentration as 4%, regulate its pH to 8.0～9.0, kept 3 hours, filter, remove solid;
(ⅳ) concentrated
Measure above-mentioned filtrate, volume is designated as V, begins to concentrate, and when the volume that steams water is 2V/3, stops to concentrate;
(ⅴ) precipitation
Slowly add the reagent grade ethanol of V/6 volume in the above-mentioned concentrated solution, fully stir, neurosin is precipitated out;
(ⅵ) drying
Under agitation condition, with the mixture input spray-drier of neurosin solid, second alcohol and water, the steam of alcohol and water directly passes into the ethanol recovery tower, separates to obtain ethanol and pure water; Collect dried white solid powder, be the Phosphoric acid glycerol esters calcium product.
2. the preparation method of the neurosin of a kind of high calcium content according to claim 1, it is characterized in that: described glycerine, monocalcium phosphate, phosphoric acid and citric acid all adopt food grade.
3. the preparation method of the neurosin of a kind of high calcium content according to claim 1, it is characterized in that: described calcium hydroxide is technical grade.
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| CN108383553A (en) * | 2018-04-20 | 2018-08-10 | 浙江新安化工集团股份有限公司 | A kind of fertilizer and the preparation method and application thereof containing middle trace element |
| CN108516988B (en) * | 2018-05-17 | 2020-04-07 | 扬州工业职业技术学院 | Novel synthesis process of toothpaste additive calcium glycerophosphate |
| CN112521417B (en) * | 2020-12-07 | 2022-11-08 | 长沙兴嘉生物工程股份有限公司 | Preparation method and application of calcium glycerophosphate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101220053A (en) * | 2008-01-17 | 2008-07-16 | 核工业理化工程研究院华核新技术开发公司 | Method for synthesizing calcium glycerinophosphate |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220053A (en) * | 2008-01-17 | 2008-07-16 | 核工业理化工程研究院华核新技术开发公司 | Method for synthesizing calcium glycerinophosphate |
Non-Patent Citations (1)
| Title |
|---|
| 刘家福.甘油磷酸钙.《食品词典》.1991,第102页. * |
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