CN101525147A - Preparation method of nano calcium carbonate - Google Patents
Preparation method of nano calcium carbonate Download PDFInfo
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- CN101525147A CN101525147A CN200810183666A CN200810183666A CN101525147A CN 101525147 A CN101525147 A CN 101525147A CN 200810183666 A CN200810183666 A CN 200810183666A CN 200810183666 A CN200810183666 A CN 200810183666A CN 101525147 A CN101525147 A CN 101525147A
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Abstract
The invention discloses a preparation method of nano calcium carbonate. Firstly, industrial calcium oxide is added in hot water with the temperature of 60-70 DEG C to stir at an instant temperature to generate Ca(OH)2 suspending liquid, the mass ratio of the industrial calcium oxide to the water is 6/100-8/100, the concentration of the suspending liquid is controlled to be 4-9 percent, in a stirring state, chemical additives easy to be dissolved into the water are added so as to control the shape and the structure of a calcium carbonate product, and the adding amount of the chemical additives is 0.1-2 percent of the Ca(OH)2 suspending liquid; mixed gases with carbon dioxide and air are led to the suspending liquid for carbonation reaction at the temperature of 12-18 DEG C; the stirring speed is 300r/min-500r/min; dispersant which is sodium dodecylbenzene sulfonate, or dodecyl sodium sulfate or sodium pyrophosphate is added, when the pH value of the suspending liquid is lowered to 6.8-7.2, the reaction stops, and the product can be obtained by filtering and drying.
Description
Technical field
The present invention relates to technical field of nano material, be specifically related to the preparation method of the controlled nano-calcium carbonate of a kind of pattern.
Background technology
Nano-calcium carbonate is a kind of novel ultrafine solids material.It not only has the increase small product size of ordinary calcium carbonate, reduces the effect of product cost, also has outstanding reinforcement and half reinforcement, becomes a kind of functional materials of excellence.Present known method of producing nano-calcium carbonate is to unslaked lime specification of quality higher (common more than 95%), and cost is higher, is difficult to big area and promotes, thereby limited the nano-calcium carbonate industrial expansion.Secondly the pattern of nano-calcium carbonate is an important factor of its application performance of decision, how to accomplish pattern controlled be the gordian technique of synthesis of nano lime carbonate, and different operational paths and equipment are often adopted in the preparation of various pattern nano-calcium carbonates, the facility investment scale is big, and technology cost height, condition harshness, unstable properties.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nano-calcium carbonate.
The present invention is a kind of preparation method of nano-calcium carbonate, the steps include:
1. earlier industrial calcium oxide being added in 60 ℃～70 ℃ the hot water constant temperature stirs and generates Ca (OH)
2Suspension, the mass ratio of industrial calcium oxide and water are 6/100～8/100, and through the slagging-off of 200～300 order mesh screen sieving separating, ageing, the control suspension concentration is 4%～9%.
2. under whipped state, add crystal control agent soluble in water, with the pattern and the structure of control calcium carbonate product, the add-on of crystal control agent is Ca (OH)
20.1%～2% of suspension.
3. feed carbonic acid gas and Air mixing gas in above-mentioned suspension, the ratio of carbonic acid gas wherein is 25～40%, carries out carburizing reagent, and the temperature of carburizing reagent is 12～18 ℃; Stirring velocity is 300r/min～500r/min.
4. add dispersion agent in above-mentioned reaction process, dispersion agent is a Sodium dodecylbenzene sulfonate, perhaps sodium laurylsulfonate, and perhaps trisodium phosphate, the add-on of dispersion agent is Ca (OH)
20.1～0.3% of suspension, stopped reaction when the PH of suspension reduces to 6.8～7.2 filters, and oven dry can obtain product.
The present invention is to be raw material with industrial common lime (calcium oxide content 90%-95%), under essentially identical process conditions, the operation that adds different inorganic crystalline form directed agents and dispersion agent by the different periods in reaction process prepares the high-quality ultrafine calcium carbonate of different-shape.For the crystalline form directed agents prepares spherical nanometer calcium carbonate, prepare acicular nanometer lime carbonate for the crystalline form directed agents with sulfuric acid with the Sodium hexametaphosphate 99; Prepare flake nano carbonic acid calcium with the trisodium phosphate for the crystalline form directed agents.The used crystal control agent price of reaction process is low, and consumption is few.Its pattern of nano-calcium carbonate of the inventive method preparation is whole unified, better dispersed.The particle diameter of spherical product is 30～40nm.Needle-like product length-to-diameter ratio is 15～20, radially is about 20～30nm.Flaked product plane mean size 0.2 μ m * 0.12 μ m (long * wide).
Description of drawings
Fig. 1 is the transmission electron microscope picture of the spherical product of embodiment 1 gained, and Fig. 2 is the transmission electron microscope picture of embodiment 2 gained needle-like products, and Fig. 3 is the transmission electron microscope picture of embodiment 3 gained flaked product.
Embodiment
Embodiment 1
The industrial calcium oxide that elder generation generates a certain amount of calcining back joins constant temperature stirring generation Ca (OH) in 60 ℃ of hot water
2Suspension, the mass ratio of industry calcium oxide and water is 6/100, remove the gred through 200 order sieving separating, ageing, get the above-mentioned suspension of 5L, controlling concn is 5%, the sulfuric acid 60mL that under whipped state, adds crystal control agent 0.1mol/L, feeding carbonic acid gas volume content is 30% carbonic acid gas and Air mixing gas in above-mentioned suspension, carries out carburizing reagent, and the temperature of carburizing reagent is controlled to be 16 ℃, stirring velocity is 300r/min, add dispersion agent trisodium phosphate 5.3g in reaction process, stopped reaction when the PH of suspension reduces to 6.8 filters, can obtain spheric nano-calcium carbonate, median size 40nm 60 ℃ of oven dry.Figure 1 shows that the transmission electron microscope photo of product.
Embodiment 2
The industrial calcium oxide that elder generation generates a certain amount of calcining back joins constant temperature stirring generation Ca (OH) in 70 ℃ of hot water
2Suspension, the mass ratio of industry calcium oxide and water is 7/100, through the slagging-off of 250 order mesh screen sieving separating, ageing, get the above-mentioned suspension of 5L, controlling concn is 8%, under whipped state, under whipped state, add crystal control agent Sodium hexametaphosphate 99 7g, above-mentioned solution mutually in feeding carbonic acid gas volume content be 30% carbonic acid gas and Air mixing gas, carry out carburizing reagent.The temperature of carburizing reagent is controlled to be 15 ℃; Stirring velocity is 400r/min, adds dispersion agent Sodium dodecylbenzene sulfonate 8g in reaction process, stopped reaction when the PH of suspension reduces to 7.0, filter, can obtain acicular Nano particles of calcium carbonate 70 ℃ of oven dry, needle-like product length-to-diameter ratio is 15-20, radially is about 20-30nm.The product transmission electron microscope photo is seen Figure of description.
Embodiment 3
The industrial calcium oxide that elder generation generates a certain amount of calcining back joins constant temperature stirring generation Ca (OH) in 70 ℃ of hot water
2Suspension, the mass ratio of industry calcium oxide and water is 8/100, remove the gred through 300 order mesh screen sieving separating, ageing, get the above-mentioned suspension of 5L, controlling concn is 6%, under whipped state, under whipped state, add crystal control agent trisodium phosphate 2.6g, feeding carbonic acid gas volume content is 30% carbonic acid gas and Air mixing gas in above-mentioned suspension, carry out carburizing reagent, the temperature of carburizing reagent is controlled to be 16 ℃, stirring velocity is 500r/min, adds dispersion agent sodium laurylsulfonate 11g in reaction process, stopped reaction when the PH of suspension reduces to 7.0, filter, can obtain flaky Nano particles of calcium carbonate 60 ℃ of oven dry, as shown in Figure 2, flaked product plane mean size 0.2 μ m * 0.12 μ m (long * wide).
Embodiment 4
The industrial calcium oxide that elder generation generates a certain amount of calcining back joins constant temperature stirring generation Ca (OH) in 60 ℃ of hot water
2Suspension, the mass ratio of industry calcium oxide and water is 6/100, remove the gred through 300 order sieving separating, ageing, get the above-mentioned suspension of 5L, controlling concn is 9%, under whipped state, under whipped state, add crystal control agent 0.1mol/L sulfuric acid 80mL, feeding carbonic acid gas volume content is 40% carbonic acid gas and Air mixing gas in above-mentioned suspension, carry out carburizing reagent, the temperature of carburizing reagent is controlled to be 15 ℃, and stirring velocity is 400r/min, in reaction process, add dispersion agent trisodium phosphate 14g, stopped reaction when the PH of suspension reduces to 6.9 filters, and can obtain the spheric nano-calcium carbonate 60 ℃ of oven dry.
Embodiment 5
The industrial calcium oxide that elder generation generates a certain amount of calcining back joins constant temperature stirring generation Ca (OH) in 60 ℃ of hot water
2Suspension, the mass ratio of industry calcium oxide and water is 8/100, remove the gred through 300 order sieving separating, ageing, get the above-mentioned suspension of 5L, controlling concn is 9%, under whipped state, under whipped state, add crystal control agent 0.1mol/L sulfuric acid 80mL, feeding carbonic acid gas volume content is 35% carbonic acid gas and Air mixing gas in above-mentioned suspension, carry out carburizing reagent, the temperature of carburizing reagent is controlled to be 12 ℃, and stirring velocity is 500r/min, in reaction process, add dispersion agent trisodium phosphate 14g, stopped reaction when the PH of suspension reduces to 7.2 filters, and can obtain spherical nanometer calcium carbonate 60 ℃ of oven dry.
Embodiment 6
The industrial calcium oxide that elder generation generates a certain amount of calcining back joins constant temperature stirring generation Ca (OH) in 60 ℃ of hot water
2Suspension, the mass ratio of industry calcium oxide and water is 7/100, remove the gred through 200 order sieving separating, ageing, get the above-mentioned suspension of 5L, controlling concn is 4%, under whipped state, under whipped state, add crystal control agent 0.1mol/L sulfuric acid 50mL, feeding carbonic acid gas volume content is 25% carbonic acid gas and Air mixing gas in above-mentioned suspension, carry out carburizing reagent, the temperature of carburizing reagent is controlled to be 18 ℃, and stirring velocity is 300r/min, in reaction process, add dispersion agent trisodium phosphate 5g, stopped reaction when the PH of suspension reduces to 6.9 filters, and can obtain spherical nanometer calcium carbonate 60 ℃ of oven dry.
Embodiment 7
The industrial calcium oxide that elder generation generates a certain amount of calcining back joins constant temperature stirring generation Ca (OH) in 70 ℃ of hot water
2Suspension, the mass ratio of industry calcium oxide and water is 6/100, remove the gred through 200 order mesh screen sieving separating, ageing, get the above-mentioned suspension of 5L, controlling concn is 4%, under whipped state, under whipped state, add crystal control agent Sodium hexametaphosphate 99 6g, feeding carbonic acid gas volume content is 35% carbonic acid gas and Air mixing gas in above-mentioned suspension, carry out carburizing reagent, the temperature of carburizing reagent is controlled to be 12 ℃, and stirring velocity is 400r/min, in reaction process, add dispersion agent Sodium dodecylbenzene sulfonate 7g, stopped reaction when the PH of suspension reduces to 7.0 filters, and can obtain acicular nanometer lime carbonate 60 ℃ of oven dry.
Embodiment 8
The industrial calcium oxide that elder generation generates a certain amount of calcining back joins constant temperature stirring generation Ca (OH) in 70 ℃ of hot water
2Suspension, the mass ratio of industry calcium oxide and water is 8/100, remove the gred through 300 order mesh screen sieving separating, ageing, get the above-mentioned suspension of 5L, controlling concn is 9%, under whipped state, under whipped state, add crystal control agent Sodium hexametaphosphate 99 12g, feeding carbon dioxide content in mutually at above-mentioned solution is 35% carbonic acid gas and Air mixing gas, carry out carburizing reagent, the temperature of carburizing reagent is controlled to be 17 ℃, and stirring velocity is 500r/min, in reaction process, add dispersion agent sodium laurylsulfonate 14g, stopped reaction when the PH of suspension reduces to 7.0 filters, and can obtain acicular nanometer lime carbonate 70 ℃ of oven dry.
Embodiment 9
The industrial calcium oxide that elder generation generates a certain amount of calcining back joins constant temperature stirring generation Ca (OH) in 70 ℃ of hot water
2Suspension, the mass ratio of industry calcium oxide and water is 7/100, remove the gred through 300 order mesh screen sieving separating, ageing, get the above-mentioned suspension of 5L, controlling concn is 8%, under whipped state, under whipped state, add crystal control agent trisodium phosphate 4g, feeding the carbonic acid gas volume content in mutually at above-mentioned solution is 35% carbonic acid gas and Air mixing gas, carry out carburizing reagent, the temperature of carburizing reagent is controlled to be 12 ℃, and stirring velocity is 400r/min, in reaction process, add dispersion agent Sodium dodecylbenzene sulfonate 15g, stopped reaction when the PH of suspension reduces to 6.8 filters, and can obtain flake nano carbonic acid calcium 60 ℃ of oven dry.
Claims (3)
1, a kind of preparation method of nano-calcium carbonate the steps include:
1. earlier industrial calcium oxide being added in 60 ℃～70 ℃ the hot water constant temperature stirs and generates Ca (OH)
2Suspension, the mass ratio of industrial calcium oxide and water are 6/100～8/100, and through the slagging-off of 200～300 order mesh screen sieving separating, ageing, the control suspension concentration is 4%～9%;
2. under whipped state, add crystal control agent soluble in water, with the pattern and the structure of control calcium carbonate product, the add-on of crystal control agent is Ca (OH)
20.1%～2% of suspension;
3. feed carbonic acid gas and Air mixing gas in above-mentioned suspension, the ratio of carbonic acid gas wherein is 25～40%, carries out carburizing reagent, and the temperature of carburizing reagent is 12～18 ℃; Stirring velocity is 300r/min～500r/min;
4. add dispersion agent in above-mentioned reaction process, dispersion agent is a Sodium dodecylbenzene sulfonate, perhaps sodium laurylsulfonate, and perhaps trisodium phosphate, the add-on of dispersion agent is Ca (OH)
20.1～0.3% of suspension, stopped reaction when the PH of suspension reduces to 6.8～7.2 filters, and oven dry can obtain product.
2, the preparation method of nano-calcium carbonate according to claim 1 is characterized in that crystal control agent is a sulfuric acid, or Sodium hexametaphosphate 99, or trisodium phosphate; For the crystalline form directed agents prepares spherical nanometer calcium carbonate, prepare acicular nanometer lime carbonate for the crystalline form directed agents with sulfuric acid with the Sodium hexametaphosphate 99; Prepare flake nano carbonic acid calcium with the trisodium phosphate for the crystalline form directed agents.
3, the preparation method of nano-calcium carbonate according to claim 1, the drying temperature that it is characterized in that step 3 is 60 ℃～70 ℃.
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| CN102372300A (en) * | 2010-08-10 | 2012-03-14 | 上海华明高技术（集团）有限公司 | Preparation method of needle-like nano calcium carbonate |
| CN102424392A (en) * | 2011-09-11 | 2012-04-25 | 中国科学院过程工程研究所 | Method for preparing white carbon black cogeneration nanometer calcium carbonate by integrally utilizing micro silicon powder |
| CN102491395A (en) * | 2011-11-22 | 2012-06-13 | 曾庆铭 | Preparation method of nano-grade calcium carbonate |
| CN102531017A (en) * | 2012-03-02 | 2012-07-04 | 连州市凯恩斯纳米材料有限公司 | Carbonizer and method for producing nano calcium carbonate |
| CN103523813A (en) * | 2013-10-22 | 2014-01-22 | 山西兰花华明纳米材料有限公司 | Industrial preparation method of producing nano calcium carbonate by recycling filter-pressing water |
| CN103864126A (en) * | 2014-03-21 | 2014-06-18 | 扬州大学 | Method for preparing suspended dispersing type calcium carbonate |
| CN104803405A (en) * | 2014-01-28 | 2015-07-29 | 李广 | White mud calcium carbonate treatment technology |
| CN105417569A (en) * | 2015-12-28 | 2016-03-23 | 常熟市宏宇钙化物有限公司 | Preparation method of rodlike nano-calcium carbonate |
| CN107445188A (en) * | 2017-09-18 | 2017-12-08 | 广西华纳新材料科技有限公司 | A kind of preparation method of rod-like precipitates calcium carbonate |
| CN107445189A (en) * | 2017-09-30 | 2017-12-08 | 广西华洋矿源材料有限公司 | A kind of preparation method of needle-like nano calcium carbonate |
| CN107555461A (en) * | 2017-09-30 | 2018-01-09 | 广西华洋矿源材料有限公司 | A kind of Nano calcium carbonate dedicated preparation method of plastics |
| CN107628634A (en) * | 2017-09-30 | 2018-01-26 | 广西华洋矿源材料有限公司 | A kind of preparation method of decentralized nano-calcium carbonate |
| CN109704380A (en) * | 2018-12-12 | 2019-05-03 | 东升新材料（山东）有限公司 | A method of continuously preparing precipitated calcium carbonate filler using power-plant flue gas |
| CN109809457A (en) * | 2019-03-21 | 2019-05-28 | 广西碳酸钙产业化工程院有限公司 | Regular spherical calcium carbonate and its preparation process |
| CN110240188A (en) * | 2019-07-19 | 2019-09-17 | 良德纳米粉体创新科技(安徽)有限公司 | A kind of processing method of nanometer calcium carbonate |
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| CN111317132A (en) * | 2018-12-14 | 2020-06-23 | 解冰 | Papaya enzyme composition for assisting in enhancing digestion and absorption functions of critically ill patients, preparation method and composite nano-preparation |
| CN111484060A (en) * | 2020-04-30 | 2020-08-04 | 广西夏阳环保科技有限公司 | Preparation method of high-purity calcium carbonate |
| CN111533149A (en) * | 2020-03-31 | 2020-08-14 | 常熟市宏宇钙化物有限公司 | Preparation method of light high-dispersion calcium oxide |
| CN114736534A (en) * | 2022-04-08 | 2022-07-12 | 深圳市锦昊辉实业发展有限公司 | Preparation method of active nano calcium powder |
| CN115028183A (en) * | 2022-06-29 | 2022-09-09 | 上海第二工业大学 | Preparation method of modified rodlike calcium carbonate |
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2008
- 2008-12-04 CN CN200810183666A patent/CN101525147A/en active Pending
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| CN102372300A (en) * | 2010-08-10 | 2012-03-14 | 上海华明高技术（集团）有限公司 | Preparation method of needle-like nano calcium carbonate |
| CN102424392A (en) * | 2011-09-11 | 2012-04-25 | 中国科学院过程工程研究所 | Method for preparing white carbon black cogeneration nanometer calcium carbonate by integrally utilizing micro silicon powder |
| CN102491395A (en) * | 2011-11-22 | 2012-06-13 | 曾庆铭 | Preparation method of nano-grade calcium carbonate |
| CN102531017A (en) * | 2012-03-02 | 2012-07-04 | 连州市凯恩斯纳米材料有限公司 | Carbonizer and method for producing nano calcium carbonate |
| CN103523813A (en) * | 2013-10-22 | 2014-01-22 | 山西兰花华明纳米材料有限公司 | Industrial preparation method of producing nano calcium carbonate by recycling filter-pressing water |
| CN104803405A (en) * | 2014-01-28 | 2015-07-29 | 李广 | White mud calcium carbonate treatment technology |
| CN103864126A (en) * | 2014-03-21 | 2014-06-18 | 扬州大学 | Method for preparing suspended dispersing type calcium carbonate |
| CN105417569A (en) * | 2015-12-28 | 2016-03-23 | 常熟市宏宇钙化物有限公司 | Preparation method of rodlike nano-calcium carbonate |
| CN107445188A (en) * | 2017-09-18 | 2017-12-08 | 广西华纳新材料科技有限公司 | A kind of preparation method of rod-like precipitates calcium carbonate |
| CN107445188B (en) * | 2017-09-18 | 2019-03-15 | 广西华纳新材料科技有限公司 | A kind of preparation method of rod-like precipitates calcium carbonate |
| CN107555461A (en) * | 2017-09-30 | 2018-01-09 | 广西华洋矿源材料有限公司 | A kind of Nano calcium carbonate dedicated preparation method of plastics |
| CN107628634A (en) * | 2017-09-30 | 2018-01-26 | 广西华洋矿源材料有限公司 | A kind of preparation method of decentralized nano-calcium carbonate |
| CN107445189A (en) * | 2017-09-30 | 2017-12-08 | 广西华洋矿源材料有限公司 | A kind of preparation method of needle-like nano calcium carbonate |
| CN109704380A (en) * | 2018-12-12 | 2019-05-03 | 东升新材料（山东）有限公司 | A method of continuously preparing precipitated calcium carbonate filler using power-plant flue gas |
| CN111317123A (en) * | 2018-12-14 | 2020-06-23 | 解冰 | Papaya enzyme composition for improving and promoting functions of digestive absorption system, preparation method and composite nano preparation |
| CN111317132A (en) * | 2018-12-14 | 2020-06-23 | 解冰 | Papaya enzyme composition for assisting in enhancing digestion and absorption functions of critically ill patients, preparation method and composite nano-preparation |
| CN109809457A (en) * | 2019-03-21 | 2019-05-28 | 广西碳酸钙产业化工程院有限公司 | Regular spherical calcium carbonate and its preparation process |
| CN110240188A (en) * | 2019-07-19 | 2019-09-17 | 良德纳米粉体创新科技(安徽)有限公司 | A kind of processing method of nanometer calcium carbonate |
| CN111533149A (en) * | 2020-03-31 | 2020-08-14 | 常熟市宏宇钙化物有限公司 | Preparation method of light high-dispersion calcium oxide |
| CN111484060A (en) * | 2020-04-30 | 2020-08-04 | 广西夏阳环保科技有限公司 | Preparation method of high-purity calcium carbonate |
| CN114736534A (en) * | 2022-04-08 | 2022-07-12 | 深圳市锦昊辉实业发展有限公司 | Preparation method of active nano calcium powder |
| CN115028183A (en) * | 2022-06-29 | 2022-09-09 | 上海第二工业大学 | Preparation method of modified rodlike calcium carbonate |
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