CN102166020A - Preparation method of surface modified nanometer calcium carbonate for foods - Google Patents
Preparation method of surface modified nanometer calcium carbonate for foods Download PDFInfo
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- CN102166020A CN102166020A CN201110050846.2A CN201110050846A CN102166020A CN 102166020 A CN102166020 A CN 102166020A CN 201110050846 A CN201110050846 A CN 201110050846A CN 102166020 A CN102166020 A CN 102166020A
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Abstract
The invention belongs to the field of food additives, and in particular relates to a preparation method of surface modified nanometer calcium carbonate for foods, comprising the following steps: (1) carbonizing a decontaminated calcium hydroxide slurry and carbon dioxide gas mixture to synthesize nanometer calcium carbonate slurry; (2) adding a sodium polyphosphate salt into the nanometer calcium carbonate slurry to disperse; (3) heating and adding stearic acid or sodium stearate to carry out surface activation on the nanometer calcium carbonate surface; (4) continuously adding sodium carboxy methyl cellulose to improve the suspension stability of the slurry; and (5) drying and smashing the modified slurry. The preparation method has the advantages that the prepared surface modified nanometer calcium carbonate for foods has the advantages of small particles, even dispersibility and good suspension property in water, does not have bad influences on the color, the stability, the flavour and the like of the foods and is especially suitable to use in milk, soymilk and other beverages.
Description
Technical field
The invention belongs to the food additives field, be specifically related to a kind of preparation method who is used for the surface modified nano calcium carbonate of food.
Background technology
Calcium is the maximum mineral matter of in-vivo content, plays an important role in human body.The calcium of adult in the bone all has 20% to be absorbed and changes the teenager of growth stage and the more calcium of the elderly's needs every year.Population of China generally ca intake deficiency is so the Chinese more than 80% need carry out replenishing the calcium in various degree.
At present, people use two class Creta Preparatas usually when carrying out the calcium reinforcement, and a kind of is water-insoluble, as calcium carbonate, calcium phosphate, calcium citrate etc.; A kind of is water miscible, as calcium lactate etc.Preceding a kind of because proportion is bigger greater than water and relative particle, inevitably can produce precipitation when in food liquid, using, in order to address this problem, generally be to add a certain amount of food stabilizer, rely on the increase viscosity to improve the supporting effect, such as carragheen, xanthans, Arabic gum etc., as patent CN00819183.2, CN98803592.8, adopt this method, the cost costliness, and cause the unstability of product easily; Common in addition calcium carbonate has the lime taste, and particle is big, disperses irregularly, and mouthfeel is poor; The expensive price of soluble calcium salt and bitter taste all are that food calcium is strengthened very real problem.
Therefore, provide that a kind of particle is little, good dispersion, resistance to settling can superior calcium-nutrition intensifying agent be very needs of people institute.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art the preparation method of the surface modified nano calcium carbonate that is used for food of provide that a kind of particle is little, good dispersion, resistance to settling can be superior.
The preparation method who is used for the surface modified nano calcium carbonate of food of the present invention may further comprise the steps:
(1) in the calcium hydroxide suspension of handling through removal of impurities, adds the nucleus controlling agent, the addition of nucleus controlling agent is the 0.3-1.0% of calcium hydroxide weight in the calcium hydroxide suspension, feed carbon dioxide and Air mixing gas, carbonization synthesis of nano calcium carbonate slurry, wherein, the weight fraction of calcium hydroxide suspension is 5-20%, and the volume fraction of carbon dioxide is 5-50% in carbon dioxide and the Air mixing gas, carburizing temperature is 5-40 ℃, and the pH value of carbonization terminal point slurry is between 6-7.5;
(2) add the polyphosphoric acid sodium salt in the nano-calcium carbonate slurry, its consumption is the 0.5-10% of nano-calcium carbonate weight in the nano-calcium carbonate slurry, is preferably 2%-6%, disperses 20-60min under high speed shear;
(3) be warmed up to 60-80 ℃, continuation adding stearic acid or odium stearate are carried out surface activation process to nano-calcium carbonate under stirring, and its consumption is the 0.1-6% of nano-calcium carbonate weight in the nano-calcium carbonate slurry, is preferably 0.5%-3%, insulated and stirred 10-30min;
(4) continue to add sodium carboxymethylcellulose and improve slurry suspension stability, its consumption is the 0.1-6% of nano-calcium carbonate weight in the nano-calcium carbonate slurry, is preferably 0.5%-2%, stirs 10-30min;
(5) modification is good slurry is dry under 60-110 ℃ of condition, and pulverizer is pulverized, and makes the surface modified nano calcium carbonate that is used for food.
It is that impurity iron element, lead element, arsenic element, barium element, magnesium elements and mercury element are formed precipitation under the pH8-14 condition that the removal of impurities of wherein said calcium hydroxide is handled, and the precipitation of generation is removed through multiple times of filtration and charcoal absorption.
Described carbonization is synthetic adopts a kind of in Bubbling method, overweight force method or the film dispersion method, is preferably overweight force method or film dispersion method, more preferably the film dispersion method.The nucleus controlling agent is the mixture of a kind of or any two kinds and above arbitrary proportion in sulfuric acid, phosphoric acid, citric acid or the carbohydrate, is preferably a kind of in sucrose, beet sugar or the maltose.
Described polyphosphoric acid sodium salt is the mixture of a kind of or any two kinds and above arbitrary proportion in sodium pyrophosphate, sodium phosphate trimer, calgon or the sodium polyphosphate, more than is to meet the food-grade modifier that GB requires.
The invention has the advantages that the surface modified nano calcium carbonate particle that is used for food that makes is little, be uniformly dispersed, good suspension is arranged in water, the color and luster of food, stability, local flavor etc. there is not harmful effect, especially suitable being applied in the beverages such as milk, soymilk.
The specific embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1:
The weight fraction that to handle through removal of impurities is 10% calcium hydroxide suspension, being transferred to film disperses in the carbonization reactor, 0.5% the sucrose that adds calcium hydroxide weight in the relative calcium hydroxide suspension, feeding carbon dioxide volume fraction is 30% carbon dioxide and Air mixing gas, it is synthetic to adopt Bubbling method to carry out carbonization at 17 ℃, when PH reduces to 6.8, continue ventilation 10 minutes, adding water, to get weight fraction be 10% nano-calcium carbonate slurry, the nano-calcium carbonate slurry is transferred in the retort, 3% the calgon that adds nano-calcium carbonate weight in the relative nano-calcium carbonate slurry then, after under high speed shear, disperseing 30min, slurry is heated to 70 ℃ of stirrings, and add 2% odium stearate of nano-calcium carbonate weight in the relative nano-calcium carbonate slurry, behind the insulated and stirred 15min, 1% the sodium carboxymethylcellulose that adds nano-calcium carbonate weight in the relative nano-calcium carbonate slurry, continue to stir 20min, stop to stir, it is dry under 80 ℃, and pulverizer is pulverized and is made surface modified nano calcium carbonate.
Get the above-mentioned surface modified nano calcium carbonate fine powder 3g that makes, join in the 300ml water, after high speed shear is disperseed, pour graduated cylinder into and leave standstill, after 72 hours, do not clarify water layer and occur by the upper strata in sedimentation for its aqueous dispersions.
Embodiment 2:
The weight fraction that to handle through removal of impurities is 15% calcium hydroxide suspension, being transferred to film disperses in the carbonization reactor, 0.5% the sucrose that adds calcium hydroxide weight in the relative calcium hydroxide suspension, feeding carbon dioxide volume fraction is 30% carbon dioxide and Air mixing gas, it is synthetic to adopt overweight force method to carry out carbonization at 17 ℃, when PH reduces to 6.8, continue ventilation 10 minutes, adding water, to get weight fraction be 10% nano-calcium carbonate slurry, the nano-calcium carbonate slurry is transferred in the retort, 4% the sodium pyrophosphate that adds nano-calcium carbonate weight in the relative nano-calcium carbonate slurry then, after under high speed shear, disperseing 30min, slurry is heated to 70 ℃ of stirrings, and add 2% stearic acid of nano-calcium carbonate weight in the relative nano-calcium carbonate slurry, behind the insulated and stirred 20min, 2% the sodium carboxymethylcellulose that adds nano-calcium carbonate weight in the relative nano-calcium carbonate slurry, continue to stir 30min, stop to stir, it is dry under 80 ℃, and pulverizer is pulverized and is made surface modified nano calcium carbonate.
Get the above-mentioned surface modified nano calcium carbonate powder 3g that makes, join in the 300ml water, after high speed shear is disperseed, pour graduated cylinder into and leave standstill, after 72 hours, do not clarify water layer and occur by the upper strata in sedimentation for its dispersion liquid.
Embodiment 3:
The weight fraction that to handle through removal of impurities is 10% calcium hydroxide suspension, be transferred in the bubble tower carbonization reactor, 0.7% the sucrose that adds calcium hydroxide weight in the relative calcium hydroxide suspension, feeding carbon dioxide volume fraction is 35% carbon dioxide and Air mixing gas, it is synthetic to adopt the film dispersion method to carry out carbonization at 19 ℃, when PH reduces to 6.8, continue ventilation 10 minutes, adding water, to get weight fraction be 10% nano-calcium carbonate slurry, the nano-calcium carbonate slurry is transferred in the retort, 4% the calgon that adds nano-calcium carbonate weight in the relative nano-calcium carbonate slurry then, after under high speed shear, disperseing 30min, slurry is heated to 80 ℃ of stirrings, and add 3% odium stearate of nano-calcium carbonate weight in the relative nano-calcium carbonate slurry, behind the insulated and stirred 20min, 0.5% the sodium carboxymethylcellulose that adds nano-calcium carbonate weight in the relative nano-calcium carbonate slurry, continue to stir 20min, stop to stir, it is dry under 80 ℃, and pulverizer is pulverized and is made surface modified nano calcium carbonate.
Get the above-mentioned surface modified nano calcium carbonate powder 3g that makes, join in the 300ml water, after high speed shear is disperseed, pour graduated cylinder into and leave standstill, after 72 hours, do not clarify water layer and occur by the upper strata in sedimentation for its aqueous dispersions.
Embodiment 4:
The 1.32g surface modified nano calcium carbonate powder that embodiment 1 is made adds in the commercially available pure fresh milk of 1000ml, and homogeneous is handled after high speed shear, and the high calcium milk that obtains is preserved in sealed glass jars by well-established law sterilization, cooling.This high calcium milk does not have obvious calcium precipitate and mouthfeel and pure fresh milk basically identical occur after preserving 7 days under 0 ℃ of-4 ℃ of low temperature.
Embodiment 5:
1.32g surface modified nano calcium carbonate powder and 3g natrium citricum, 80g white granulated sugar, 0.8g monoglyceride, 1.2g sucrose fat that embodiment 1 is made add in the commercially available pure fresh soya-bean milk of 1000ml (solid content is 9%), homogeneous is handled after high speed shear, the high calcium bean milk that obtains is preserved in sealed glass jars by well-established law sterilization, cooling.This high calcium bean milk does not have obvious calcium precipitate and mouthfeel and soymilk basically identical occur after preserving 5 days under 0 ℃ of-4 ℃ of low temperature.
Embodiment 6:
The 1.35g surface modified nano calcium carbonate powder that embodiment 2 is made adds in the commercially available pure fresh milk of 1000ml, and homogeneous is handled after high speed shear, and the high calcium milk that obtains is preserved in sealed glass jars by well-established law sterilization, cooling.This high calcium milk does not have obvious calcium precipitate and mouthfeel and pure fresh milk basically identical occur after preserving 7 days under 0 ℃ of-4 ℃ of low temperature.
Embodiment 7:
The 2.16g surface modified nano calcium carbonate powder that embodiment 3 is made adds in the commercially available pure fresh milk of 1000ml, homogeneous is handled after high speed shear, the high calcium milk that obtains is warming up to 43-45 ℃, keeps constant temperature, presses in the 3% adding milk of fresh milk amount producing with bacterial classification, ferment at constant temperature 3-5 hour, after the PH that ferments reaches 3.9, stop fermentation, cool rapidly to below 30 ℃, after stirring adding sucrose and sucrose fat then, preserve in the sealed glass jars.This high-calcium yoghurt does not have obvious calcium precipitate and mouthfeel and commercially available pure sour milk basically identical occur after preserving 7 days under 0 ℃ of-4 ℃ of low temperature.
Comparative Examples 1:
1.25g ordinary calcium carbonate powder is added in the commercially available pure fresh milk of 1000ml, and homogeneous is handled after high speed shear, and the high calcium milk that obtains is preserved in sealed glass jars by well-established law sterilization, cooling.This high calcium milk has obvious calcium precipitate to occur after preserving 7 days under 0 ℃ of-4 ℃ of low temperature, and tasting has obvious astringent taste.
Comparative Examples 2:
The unmodified nano-calcium carbonate calcium powder of 1.25g is added in the commercially available pure fresh milk of 1000ml, and homogeneous is handled after high speed shear, and the high calcium milk that obtains is preserved in sealed glass jars by well-established law sterilization, cooling.This high calcium milk has the small amount of calcium precipitation to occur after preserving 7 days under 0 ℃ of-4 ℃ of low temperature, tastes slightly astringent taste.
Claims (8)
1. preparation method who is used for the surface modified nano calcium carbonate of food is characterized in that may further comprise the steps:
(1) be to add the nucleus controlling agent in the 5-20% calcium hydroxide suspension at the weight fraction of handling through removal of impurities, the addition of nucleus controlling agent is the 0.3-1.0% of calcium hydroxide weight in the calcium hydroxide suspension, feeding the carbon dioxide volume fraction is carbon dioxide and the Air mixing gas of 5-50%, at 5-40 ℃ of following carbonization synthesis of nano calcium carbonate slurry, the pH value of carbonization terminal point slurry is between 6-7.5;
(2) add the polyphosphoric acid sodium salt in the nano-calcium carbonate slurry, its consumption is the 0.5-10% of nano-calcium carbonate weight in the nano-calcium carbonate slurry, disperses 20-60min under high speed shear;
(3) be warmed up to 60-80 ℃, continuation adding stearic acid or odium stearate are carried out surface activation process to nano-calcium carbonate under stirring, and its consumption is the 0.1-6% of nano-calcium carbonate weight in the nano-calcium carbonate slurry, insulated and stirred 10-30min;
(4) continue to add sodium carboxymethylcellulose and improve slurry suspension stability, its consumption is the 0.1-6% of nano-calcium carbonate weight in the nano-calcium carbonate slurry, stirs 10-30min;
(5) modification is good slurry is dry under 60-110 ℃ of condition, and pulverizer is pulverized, and makes the surface modified nano calcium carbonate that is used for food.
2. the preparation method who is used for the surface modified nano calcium carbonate of food according to claim 1, the removal of impurities processing that it is characterized in that calcium hydroxide is that impurity iron element, lead element, arsenic element, barium element, magnesium elements and mercury element are formed precipitation under the pH8-14 condition, and the precipitation of generation is removed through multiple times of filtration and charcoal absorption.
3. the preparation method who is used for the surface modified nano calcium carbonate of food according to claim 1, it is characterized in that carbonization is synthetic adopts a kind of in Bubbling method, overweight force method or the film dispersion method, be preferably overweight force method or film dispersion method, more preferably the film dispersion method.
4. the preparation method who is used for the surface modified nano calcium carbonate of food according to claim 1, it is characterized in that the nucleus controlling agent is the mixture of a kind of or any two kinds and above arbitrary proportion in sulfuric acid, phosphoric acid, citric acid or the carbohydrate, be preferably a kind of in sucrose, beet sugar or the maltose.
5. the preparation method who is used for the surface modified nano calcium carbonate of food according to claim 1 is characterized in that the polyphosphoric acid sodium salt is the mixture of a kind of or any two kinds and above arbitrary proportion in sodium pyrophosphate, sodium phosphate trimer, calgon or the sodium polyphosphate.
6. the preparation method who is used for the surface modified nano calcium carbonate of food according to claim 1 is characterized in that the consumption of polyphosphoric acid sodium salt is preferably the 2%-6% of nano-calcium carbonate weight in the nano-calcium carbonate slurry.
7. the preparation method who is used for the surface modified nano calcium carbonate of food according to claim 1 is characterized in that the consumption of stearic acid or odium stearate is preferably the 0.5%-3% of nano-calcium carbonate weight in the nano-calcium carbonate slurry.
8. the preparation method who is used for the surface modified nano calcium carbonate of food according to claim 1 is characterized in that the consumption of sodium carboxymethylcellulose is preferably the 0.5%-2% of nano-calcium carbonate weight in the nano-calcium carbonate slurry.
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Cited By (7)
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| CN102674424A (en) * | 2012-04-28 | 2012-09-19 | 浙江大学 | Method for preparing nanometer calcium carbonate slurry by using waste gypsum as calcium sources, products and application |
| CN104562840A (en) * | 2015-01-07 | 2015-04-29 | 浙江理工大学 | Preparation method for high-stability nano-calcium carbonate aqueous-phase dispersion liquid for papermaking coating |
| CN105858696A (en) * | 2016-03-28 | 2016-08-17 | 武汉工程大学 | Preparation method and application for micron vaterite type food-grade calcium carbonate |
| CN106509128A (en) * | 2016-11-03 | 2017-03-22 | 南京福特卡特材料科技有限公司 | Emulsified nano-calcium carbonate as well as preparation method and application thereof |
| CN107601542A (en) * | 2017-09-30 | 2018-01-19 | 广西华洋矿源材料有限公司 | A kind of preparation method of nano-calcium carbonate |
| CN110577674A (en) * | 2019-09-16 | 2019-12-17 | 江西七彩塑胶染料有限公司 | plastic modified material and preparation method thereof |
| CN117049581A (en) * | 2023-08-15 | 2023-11-14 | 江西明缘高新材料有限公司 | Preparation method of light calcium carbonate for food |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674424A (en) * | 2012-04-28 | 2012-09-19 | 浙江大学 | Method for preparing nanometer calcium carbonate slurry by using waste gypsum as calcium sources, products and application |
| CN102674424B (en) * | 2012-04-28 | 2014-11-05 | 浙江大学 | Method for preparing nanometer calcium carbonate slurry by using waste gypsum as calcium sources, products and application |
| CN104562840A (en) * | 2015-01-07 | 2015-04-29 | 浙江理工大学 | Preparation method for high-stability nano-calcium carbonate aqueous-phase dispersion liquid for papermaking coating |
| CN104562840B (en) * | 2015-01-07 | 2016-09-21 | 浙江理工大学 | A kind of papermaking paint high-stability nano calcium carbonate water phase dispersant liquid preparation method |
| CN105858696A (en) * | 2016-03-28 | 2016-08-17 | 武汉工程大学 | Preparation method and application for micron vaterite type food-grade calcium carbonate |
| CN106509128A (en) * | 2016-11-03 | 2017-03-22 | 南京福特卡特材料科技有限公司 | Emulsified nano-calcium carbonate as well as preparation method and application thereof |
| CN107601542A (en) * | 2017-09-30 | 2018-01-19 | 广西华洋矿源材料有限公司 | A kind of preparation method of nano-calcium carbonate |
| CN110577674A (en) * | 2019-09-16 | 2019-12-17 | 江西七彩塑胶染料有限公司 | plastic modified material and preparation method thereof |
| CN117049581A (en) * | 2023-08-15 | 2023-11-14 | 江西明缘高新材料有限公司 | Preparation method of light calcium carbonate for food |
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Application publication date: 20110831 |