CN102126736A - Method for preparing nano-calcium carbonate powder by using soluble carbonate - Google Patents
Method for preparing nano-calcium carbonate powder by using soluble carbonate Download PDFInfo
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- CN102126736A CN102126736A CN2011100214721A CN201110021472A CN102126736A CN 102126736 A CN102126736 A CN 102126736A CN 2011100214721 A CN2011100214721 A CN 2011100214721A CN 201110021472 A CN201110021472 A CN 201110021472A CN 102126736 A CN102126736 A CN 102126736A
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- calcium carbonate
- soluble carbon
- aqueous solution
- carbon hydrochlorate
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Abstract
The invention relates to a method for preparing nano-calcium carbonate powder. The method comprises the following steps: spraying a clear soluble carbonate aqueous solution containing dispersing agents into calcium hydroxide slurry at high speed under high-speed stirring under normal temperature and pressure and carrying out rapid filtration to obtain nano-calcium carbonate precipitate; and drying the precipitate to obtain the nano-calcium carbonate powder with grain size being lower than 100nm. The method has the advantages of simple and easily controlled process, low investment and cost, high purity and stable product quality, is pollution-free and is easy for industrial scale production.
Description
Technical field
The present invention relates to a kind of preparation particle scale is nano level Paris white body method, is to use the soluble carbon hydrochlorate specifically, directly obtains the preparation method of nanometer grade calcium carbonate powder by chemical reaction.
Technical background
The nano-calcium carbonate powder is present unique excellent function nano material that reaches the ton scale and be most widely used, and its particle diameter yardstick is between 1-100nm.Nano-calcium carbonate not only has the effect that increase-volume is filled, reduced cost, and its toughened and reinforced effect can greatly improve the performance and the quality of relevant industries product, has been widely used as the filler and the additive of industries such as rubber, plastics, papermaking, coating, electric wire, cable, printing ink, welding electrode, organic synthesis, metallurgy, glass, asbestos industry, medicine, food, daily use chemicals, feed.
At present, the preparation method of nano-calcium carbonate mainly adopts traditional carborization.Carborization be domestic develop comparatively sophisticated a kind of method, its cardinal principle be utilize the Wingdale high-temperature calcination to make calcium oxide, the digestion reaction by calcium oxide and water obtains calcium hydroxide slurry, these slurries and carbonic acid gas generation carburizing reagent and prepares lime carbonate, its gordian technique is how to control carbonation reaction, and its main drawback is that cost height, productive rate are low, production and equipment complexity etc.According to the carbonization technique difference, carborization mainly is divided into: intermittently bubbling carbonizing method, three kinds of multistage spray carbonation method and hypergravity carborizations continuously.The ammonium carborization of developing based on carborization, its cardinal principle are to prepare nano-calcium carbonate by the carburizing reagent between carbonic acid gas and calcium chloride, the ammoniacal liquor, and its gordian technique also is carburizing reagent.
Summary of the invention
The present invention relates to a kind of method that adopts the soluble carbon hydrochlorate to prepare the nano-calcium carbonate powder.Its objective is for fear of traditional method to prepare the above-mentioned shortcoming that the nanometer grade calcium carbonate powder exists, provide that a kind of investment is little, cost is low, constant product quality, technology is simple and easy to control and can realize mass-producing continuous production high-purity Nano-class preparing calcium carbonate powder.
Soluble carbon hydrochlorate of the present invention is a kind of of following chemicals: yellow soda ash, salt of wormwood and volatile salt.
The preparation method of nano-calcium carbonate powder of the present invention comprises following processing step:
(1). the preparation calcium hydroxide slurry.Utilize continuous digestion machine, calcium oxide and water thorough mixing that the Wingdale high temperature sintering is made obtain calcium hydroxide slurry 1-5M/L;
(2). preparation soluble carbon hydrochlorate clear aqueous solution.Contain in the soluble carbon hydrochlorate clear aqueous solution: carbonate 1-5M/L, dispersion agent 0.01-0.05M/L;
(3). under normal temperature, atmospheric pressure state, spray into the soluble carbon hydrochlorate clear aqueous solution of above-mentioned preparation in the calcium hydroxide slurry at a high speed and stir with 300-500 rev/min rotating speed simultaneously, behind soluble carbon hydrochlorate clear aqueous solution and the calcium hydroxide slurry thorough mixing fast filtration obtain nano-calcium carbonate throw out and oxyhydroxide settled solution;
(4). above-mentioned nano-calcium carbonate throw out is carried out drying, and obtaining the granularity yardstick is the following nano-calcium carbonate powder of 100nm;
(5). according to the mol ratio of pure substance 1: 1.2, be transported in the above-mentioned oxyhydroxide clear aqueous solution after the carbon dioxide that the Wingdale high temperature sintering is obtained purifies and stir with 50-100 rev/min rotating speed simultaneously, obtain soluble carbon hydrochlorate settled solution and also recycle.
The chemical principle that soluble carbon hydrochlorate of the present invention is a yellow soda ash is:
Ca(OH)
2+Na
2CO
3＝CaCO
3↓+2NaOH
2NaOH+CO
2＝Na
2CO
3+H
2O
The chemical principle that soluble carbon hydrochlorate of the present invention is a salt of wormwood is:
Ca(OH)
2+K
2CO
3＝CaCO
3↓+2KOH
2KOH+CO
2＝K
2CO
3+H
2O
The chemical principle that soluble carbon hydrochlorate of the present invention is a volatile salt is:
Ca(OH)
2+(NH
4)
2CO
3＝CaCO
3↓+2NH
4OH
2NH
4OH+CO
2＝(NH
4)
2CO
3+H
2O
Contained dispersion agent is at least a kind of of following chemicals in the soluble carbon hydrochlorate clear aqueous solution of the present invention: polyoxyethylene glycol, C8-10 alkylene phenol Soxylat A 25-7, polyoxyethylene nonylphenol ether, polyoxyethylene oleic acid ester, bromination dodecyl dimethyl hexadecyldimethyl benzyl ammonium, the chlorination dimethyl dioctadecyl ammonium, the polyoxyethylene nonylphenol ether sulfuric acid amine salt, the alkylphenol polyoxyethylene phosphoric acid ester, dodecyl sulphate and salt thereof, dodecyl sodium sulfonate and salt thereof, Witco 1298 Soft Acid and salt thereof.
The present invention is under normal temperature, normal pressure, utilizes chemical reaction directly to obtain the nano-calcium carbonate powder, its technological process is simple and easy to control, investment is little, cost is low, purity is high, constant product quality, pollution-free, be easy to industrially scalable production.
Embodiment
Below in conjunction with embodiment the inventive method is described in further detail.
Embodiment 1
Prepare the nano-calcium carbonate powder by following processing step.
(1). the preparation calcium hydroxide slurry, contain in these slurries: calcium hydroxide 1M/L;
(2). preparation yellow soda ash clear aqueous solution, contain in this solution: yellow soda ash 2M/L, sodium lauryl sulphate (dispersion agent) 0.02M/L; The compound method of yellow soda ash clear aqueous solution is that the yellow soda ash of calculated amount, sodium lauryl sulphate are used deionized water dissolving respectively, then lauryl sodium sulfate aqueous solution is joined to mix and be diluted in the aqueous sodium carbonate to require concentration.
(3). under normal temperature, atmospheric pressure state, spray into the yellow soda ash clear aqueous solution of above-mentioned preparation in the calcium hydroxide slurry at a high speed and stir with 500 rev/mins rotating speed simultaneously, obtain nano-calcium carbonate throw out and sodium hydroxide clear aqueous solution after the filtration fast behind yellow soda ash clear aqueous solution and the calcium hydroxide slurry thorough mixing;
(4). carry out drying with obtaining the nano-calcium carbonate throw out after the above-mentioned filtration, obtaining the granularity yardstick is the nano-calcium carbonate powder of 15-30nm;
(5). according to the mol ratio of pure substance 1: 1.2, be transported to the carbon dioxide after purifying in the sodium hydroxide clear aqueous solution and stir with 50-100 rev/min rotating speed simultaneously, obtain the yellow soda ash clear aqueous solution and also recycle.
The dispersion agent that uses in the inventive method helps reducing the reunion of nano grain surface energy, control nano-powder and growing up, and the following chemicals of also optional usefulness is made dispersion agent: polyoxyethylene glycol, C8-10 alkylene phenol Soxylat A 25-7, polyoxyethylene nonylphenol ether, polyoxyethylene oleic acid ester, bromination dodecyl dimethyl hexadecyldimethyl benzyl ammonium, chlorination dimethyl dioctadecyl ammonium, polyoxyethylene nonylphenol ether sulfuric acid amine salt, alkylphenol polyoxyethylene phosphoric acid ester, dodecyl sulphate and salt, dodecyl sodium sulfonate and salt thereof, Witco 1298 Soft Acid and salt thereof.
Embodiment 2
Prepare the nano-calcium carbonate powder by following processing step.
(1). the preparation calcium hydroxide slurry, contain in these slurries: calcium hydroxide 5M/L;
(2). preparation yellow soda ash clear aqueous solution, contain in this solution: yellow soda ash 5M/L, dodecyl sodium sulfonate (dispersion agent) 0.04M/L; The compound method of yellow soda ash clear aqueous solution is that the yellow soda ash of calculated amount, dodecyl sodium sulfonate are used deionized water dissolving respectively, then the dodecyl sodium sulfonate aqueous solution is joined to mix and be diluted in the aqueous sodium carbonate to require concentration.
(3). under normal temperature, atmospheric pressure state, spray into the yellow soda ash clear aqueous solution of above-mentioned preparation in the calcium hydroxide slurry at a high speed and stir with 300 rev/mins rotating speed simultaneously, obtain nano-calcium carbonate throw out and sodium hydroxide clear aqueous solution after the filtration fast behind yellow soda ash clear aqueous solution and the calcium hydroxide slurry thorough mixing;
(4). carry out drying with obtaining the nano-calcium carbonate throw out after the above-mentioned filtration, obtaining the granularity yardstick is the nano-calcium carbonate powder of 35-55nm;
(5). according to the mol ratio of pure substance 1: 1.2, be transported to the carbon dioxide after purifying in the sodium hydroxide clear aqueous solution and stir with 50-100 rev/min rotating speed simultaneously, obtain the yellow soda ash clear aqueous solution and also recycle.
Embodiment 3
(1). the preparation calcium hydroxide slurry, contain in these slurries: calcium hydroxide 3M/L;
(2). preparation yellow soda ash clear aqueous solution, contain in this solution: yellow soda ash 3M/L, dodecyl dimethyl hexadecyldimethyl benzyl ammonium (dispersion agent) 0.03M/L; The compound method of yellow soda ash clear aqueous solution is that the yellow soda ash of calculated amount, dodecyl dimethyl hexadecyldimethyl benzyl ammonium are used deionized water dissolving respectively, then the dodecyl dimethyl hexadecyldimethyl benzyl ammonium aqueous solution is joined to mix and be diluted in the aqueous sodium carbonate to require concentration.
(3). under normal temperature, atmospheric pressure state, spray into the yellow soda ash clear aqueous solution of above-mentioned preparation in the calcium hydroxide slurry at a high speed and stir with 400 rev/mins rotating speed simultaneously, obtain nano-calcium carbonate throw out and sodium hydroxide clear aqueous solution after the filtration fast behind yellow soda ash clear aqueous solution and the calcium hydroxide slurry thorough mixing;
(4). carry out drying with obtaining the nano-calcium carbonate throw out after the above-mentioned filtration, obtaining the granularity yardstick is the nano-calcium carbonate powder of 25-40nm;
(5). according to the mol ratio of pure substance 1: 1.2, be transported to the carbon dioxide after purifying in the sodium hydroxide settled solution and stir with 50-100 rev/min rotating speed simultaneously, obtain the yellow soda ash clear aqueous solution and also recycle.
Embodiment 4
(1). the preparation calcium hydroxide slurry, contain in these slurries: calcium hydroxide 3M/L;
(2). preparation salt of wormwood clear aqueous solution, contain in this solution: salt of wormwood 3M/L, sodium lauryl sulphate (dispersion agent) 0.03M/L; The compound method of salt of wormwood clear aqueous solution is that the lime carbonate of calculated amount, sodium lauryl sulphate are used deionized water dissolving respectively, then lauryl sodium sulfate aqueous solution is joined to mix and be diluted in the wet chemical to require concentration.
(3). under normal temperature, atmospheric pressure state, spray into the salt of wormwood clear aqueous solution of above-mentioned preparation in the calcium hydroxide slurry at a high speed and stir with 400 rev/mins rotating speed simultaneously, obtain nano-calcium carbonate throw out and potassium hydroxide clear aqueous solution after the filtration fast behind salt of wormwood clear aqueous solution and the calcium hydroxide slurry thorough mixing;
(4). carry out drying with obtaining the nano-calcium carbonate throw out after the above-mentioned filtration, obtaining the granularity yardstick is the nano-calcium carbonate powder of 20-35nm;
(5). according to the mol ratio of pure substance 1: 1.2, be transported to the carbon dioxide after purifying in the potassium hydroxide settled solution and stir with 50-100 rev/min rotating speed simultaneously, obtain the salt of wormwood clear aqueous solution and also recycle.
Embodiment 5
(1). the preparation calcium hydroxide slurry, contain in these slurries: calcium hydroxide 2M/L;
(2). preparation volatile salt clear aqueous solution, contain in this solution: volatile salt 2M/L, dodecyl dimethyl hexadecyldimethyl benzyl ammonium (dispersion agent) 0.02M/L; The compound method of volatile salt clear aqueous solution is that the volatile salt of calculated amount, dodecyl dimethyl hexadecyldimethyl benzyl ammonium are used deionized water dissolving respectively, then the dodecyl dimethyl hexadecyldimethyl benzyl ammonium aqueous solution is joined to mix and be diluted in the ammonium carbonate solution to require concentration.
(3). under normal temperature, atmospheric pressure state, spray into the volatile salt clear aqueous solution of above-mentioned preparation in the calcium hydroxide slurry at a high speed and stir with 400 rev/mins rotating speed simultaneously, obtain nano-calcium carbonate throw out and ammonium hydroxide clear aqueous solution after the filtration fast behind volatile salt clear aqueous solution and the calcium hydroxide slurry thorough mixing;
(4). carry out drying with obtaining the nano-calcium carbonate throw out after the above-mentioned filtration, obtaining the granularity yardstick is the nano-calcium carbonate powder of 25-35nm;
(5). according to the mol ratio of pure substance 1: 1.2, be transported to the carbon dioxide after purifying in the ammonium hydroxide settled solution and stir with 50-100 rev/min rotating speed simultaneously, obtain the volatile salt clear aqueous solution and also recycle.
Claims (4)
1. method of using the soluble carbon hydrochlorate to prepare the nano-calcium carbonate powder, it is characterized in that calcium hydroxide and soluble carbon hydrochlorate carry out in the presence of the dispersion agent chemical reaction directly obtain nanometer grade calcium carbonate throw out and oxyhydroxide settled solution, oxyhydroxide settled solution and purify after carbonic acid gas carry out chemical reaction and obtain the soluble carbon hydrochlorate and recycle.
Described soluble carbon hydrochlorate is a kind of of following chemicals: refer to yellow soda ash, salt of wormwood and volatile salt.
Described dispersion agent is at least a kind of of following chemicals: polyoxyethylene glycol, C8-10 alkylene phenol Soxylat A 25-7, polyoxyethylene nonylphenol ether, polyoxyethylene oleic acid ester, bromination dodecyl dimethyl hexadecyldimethyl benzyl ammonium, chlorination dimethyl dioctadecyl ammonium, polyoxyethylene nonylphenol ether sulfuric acid amine salt, alkylphenol polyoxyethylene phosphoric acid ester, dodecyl sulphate and salt, dodecyl sodium sulfonate and salt thereof, Witco 1298 Soft Acid and salt thereof.
2. the described a kind of method of using the soluble carbon hydrochlorate to prepare nano-calcium carbonate powder and soluble carbon hydrochlorate of claim 1 is characterized in that calcium hydroxide and contains the soluble carbon hydrochlorate and carry out chemical reaction directly obtain the nanometer grade calcium carbonate throw out in the presence of dispersion agent.Its concrete technical process is: under normal temperature, atmospheric pressure state, the soluble carbon hydrochlorate clear aqueous solution 1-5M/L that will contain dispersion agent 0.01-0.05M/L sprays at a high speed among the calcium hydroxide slurry 1-5M/L also simultaneously with 300-500 rev/min of stirring, the quick filtration obtains the nano-calcium carbonate throw out and carries out drying behind soluble carbon hydrochlorate clear aqueous solution and the calcium hydroxide slurry thorough mixing, and obtaining the granularity yardstick is the following nano-calcium carbonate powder of 100nm.
3. claim 1 and 2 described a kind of methods of using the soluble carbon hydrochlorate to prepare nano-calcium carbonate powder and soluble carbon hydrochlorate is characterized in that calcium hydroxide and soluble carbon hydrochlorate carry out chemical reaction acquisition soluble carbon hydrochlorate at the carbonic acid gas that carries out in the presence of the dispersion agent after chemical reaction directly obtains nanometer grade calcium carbonate throw out and oxyhydroxide clear aqueous solution, oxyhydroxide clear aqueous solution and purification.Its concrete technical process was: according to the mol ratio of pure substance 1: 1.2, be transported in the above-mentioned oxyhydroxide clear aqueous solution after the carbon dioxide that the Wingdale high temperature sintering is obtained purifies and stir with 50-100 rev/min rotating speed simultaneously, obtain soluble carbon hydrochlorate clear aqueous solution and also recycle.
4. according to claim 1 and 2 described a kind of methods of using the soluble carbon hydrochlorate to prepare the nano-calcium carbonate powder, it is characterized in that contained dispersion agent is sodium lauryl sulfate or dodecyl sodium sulfonate or bromination dodecyl dimethyl hexadecyldimethyl benzyl ammonium in the described soluble carbon hydrochlorate clear aqueous solution.
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Cited By (8)
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|---|---|---|---|---|
| CN103007721A (en) * | 2012-11-26 | 2013-04-03 | 东南大学 | Ammonia circulation-based method and device for carbonating fixation of CO2 in coal-fired flue gas |
| CN105084404A (en) * | 2015-08-13 | 2015-11-25 | 安徽世华化工有限公司 | Preparation method for micro-calcium-carbonate particles |
| CN107758718A (en) * | 2017-11-17 | 2018-03-06 | 宁波普莱斯帝金属制品有限公司 | A kind of method that calcium carbonate superfine powder nano-powder is prepared with calcite |
| CN107935013A (en) * | 2017-11-17 | 2018-04-20 | 宁波普莱斯帝金属制品有限公司 | A kind of method for preparing calcium carbonate superfine powder nano-powder |
| CN107986310A (en) * | 2017-11-17 | 2018-05-04 | 宁波普莱斯帝金属制品有限公司 | A kind of method for preparing hollow calcium oxide powder |
| CN110813059A (en) * | 2018-08-13 | 2020-02-21 | 中国石油化工股份有限公司 | Method for reducing regeneration energy consumption of carbon dioxide capture solvent |
| CN111439770A (en) * | 2019-11-21 | 2020-07-24 | 东北石油大学 | Hydrophobic calcium carbonate and preparation method thereof |
| CN113233490A (en) * | 2021-06-02 | 2021-08-10 | 桐乡市思远环保科技有限公司 | Method for preparing nano calcium carbonate by using natural calcium carbonate |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007721A (en) * | 2012-11-26 | 2013-04-03 | 东南大学 | Ammonia circulation-based method and device for carbonating fixation of CO2 in coal-fired flue gas |
| CN103007721B (en) * | 2012-11-26 | 2015-01-28 | 东南大学 | Ammonia circulation-based method and device for carbonating fixation of CO2 in coal-fired flue gas |
| CN105084404A (en) * | 2015-08-13 | 2015-11-25 | 安徽世华化工有限公司 | Preparation method for micro-calcium-carbonate particles |
| CN107758718A (en) * | 2017-11-17 | 2018-03-06 | 宁波普莱斯帝金属制品有限公司 | A kind of method that calcium carbonate superfine powder nano-powder is prepared with calcite |
| CN107935013A (en) * | 2017-11-17 | 2018-04-20 | 宁波普莱斯帝金属制品有限公司 | A kind of method for preparing calcium carbonate superfine powder nano-powder |
| CN107986310A (en) * | 2017-11-17 | 2018-05-04 | 宁波普莱斯帝金属制品有限公司 | A kind of method for preparing hollow calcium oxide powder |
| CN107758718B (en) * | 2017-11-17 | 2020-08-28 | 池州市富华粉体科技有限公司 | Method for preparing superfine calcium carbonate nano powder from calcite |
| CN107935013B (en) * | 2017-11-17 | 2020-08-28 | 南阳中瑞微粉科技有限公司 | Method for preparing superfine calcium carbonate nano powder |
| CN110813059A (en) * | 2018-08-13 | 2020-02-21 | 中国石油化工股份有限公司 | Method for reducing regeneration energy consumption of carbon dioxide capture solvent |
| CN111439770A (en) * | 2019-11-21 | 2020-07-24 | 东北石油大学 | Hydrophobic calcium carbonate and preparation method thereof |
| CN111439770B (en) * | 2019-11-21 | 2022-09-16 | 东北石油大学 | Hydrophobic calcium carbonate and preparation method thereof |
| CN113233490A (en) * | 2021-06-02 | 2021-08-10 | 桐乡市思远环保科技有限公司 | Method for preparing nano calcium carbonate by using natural calcium carbonate |
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