CN103509378A - Normal-temperature high-air-flow industrial nano-calcium carbonate preparation method - Google Patents
Normal-temperature high-air-flow industrial nano-calcium carbonate preparation method Download PDFInfo
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- CN103509378A CN103509378A CN201310498210.3A CN201310498210A CN103509378A CN 103509378 A CN103509378 A CN 103509378A CN 201310498210 A CN201310498210 A CN 201310498210A CN 103509378 A CN103509378 A CN 103509378A
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Abstract
The invention relates to a normal-temperature high-air-flow industrial nano-calcium carbonate preparation method, and solves the problems of poor product quality reproducibility and unstable product quality of the conventional nano calcium carbonate preparation method. The normal-temperature high-air-flow industrial nano-calcium carbonate preparation method comprises the following steps: adding a Ca(OH)2 suspending liquid of which the volume is 60 to 80 percent of the volume of a carburizing reaction kettle into the carburizing reaction kettle, wherein the mass concentration of the Ca(OH)2 suspending liquid is 6 to 10 percent; adjusting the temperature of the Ca(OH)2 suspending liquid added into the carburizing reaction kettle to be 25 to 40 DEG C; pumping the mixed gas of carbon dioxide and nitrogen gas into the carburizing reaction kettle at a velocity of 0.6 to 0.8 m<3>/s; adding a dispersant of which the mass is 0.02 to 0.05 percent of the total mass of the Ca(OH)2 into the Ca(OH)2 suspending liquid; heating the nano-calcium carbonate sizing agent to be 60 to 80 DEG C; adding a coating agent. The nano-calcium carbonate prepared according to the normal-temperature high-air-flow industrial nano-calcium carbonate preparation method has the advantages that the product quality reproducibility is high; the reaction device industrialization is easy to realize.
Description
Technical field
The present invention relates to a kind of preparation method of calcium carbonate, particularly a kind of industrial production process of nano-calcium carbonate.
Background technology
Nano-calcium carbonate refers to that particle diameter is less than the superfine powder of 100 nanometers, and nm-class active calcium carbonate refers to that calcium carbonate becomes oil loving Chemicals by wetting ability after surperficial organic process, and product can be widely used in the industries such as vehicle paint base, rubber, plastics.Super-refinement, narrow diameter distribution, crystal morphology stablize and product quality circulation ratio height is a basic demand of this product.At present, the preparation method of nano-calcium carbonate has multilevel spray carbonization, gravity Method, band to stir the carbonization at low temperature precipitator method etc.Multilevel spray carbonization is produced nano-calcium carbonate, the problem such as exist spray material port to stop up in production process, utilization rate of carbon dioxide is low, and product energy consumption is high, and production equipment is difficult to realize long-period stable operation; Gravity Method production nano-calcium carbonate, production equipment energy consumption is high, and the nano-calcium carbonate of the high surface energy that reaction generates easily knot, in reactor, need regularly carry out pickling for assurance quality product, and operation stability is poor; Band stirs the carbonization at low temperature precipitator method and produces nano-calcium carbonate, and compound particle size distribution is wide, bad dispersibility, and the temperature that needs to control the intake of carbonic acid gas in reaction process and control reaction process, device capbility is low, energy consumption is higher.The production method of above-mentioned several nano-calcium carbonates, in industrialization process, because energy consumption is higher, in the unstable and process of preparing of reaction unit, in industrialization, impact is evaluated not enoughly, has caused the poor reproducibility of nano-calcium carbonate product quality, and product quality is unstable.。
Summary of the invention
The invention provides a kind of normal temperature atm number and produce the industrial production process of nano-calcium carbonate, solved poor reproducibility and the unsettled problem of product quality of the nano-calcium carbonate product quality of existing preparation method's existence.
The present invention solves above technical problem by the following technical programs:
Normal temperature atm number is produced an industrial production process for nano-calcium carbonate, comprises the following steps:
The first step, in carburizing reagent still, add the Ca (OH) of the 60-80% of reactor volume
2suspension, Ca (OH)
2the mass concentration of suspension is 6-10%;
Second step, adjustment join the Ca (OH) in carburizing reagent still
2the temperature of suspension, makes it reach 25-40 ℃;
The 3rd step, with the speed of 0.6-0.8 cube of meter per second to the mixed gas that passes into carbonic acid gas and nitrogen in carburizing reagent still, in the volumetric concentration of this carbon dioxide in gas mixture gas, be 35%-60%, with Ca (OH)
2the mass concentration of suspension is that benchmark goes out Ca (OH)
2total mass, as Ca (OH)
2the Ca (OH) of participation and carbon dioxide reaction in suspension
2quality reach Ca (OH)
2the 8-10% of total mass time, add Ca (OH)
2the crystal structure adjusting agent of 0.5-2% of total mass, continue carbonization, until Ca(OH)
2the pH value of suspension reaches 6-7, generates nano level calcite, and temperature of reaction is controlled at 38-70 ℃;
The 4th step, at Ca (OH)
2suspension in add Ca (OH)
2the dispersion agent of 0.2-0.5 ‰ of total mass, by dispersion agent, be combined with calcium carbonate hydrophilic radical and form the surface charge that electrostatic double layer is adjusted nanoparticle;
The 5th step, one or both and water in lipid acid or water soluble peptide acid esters coupling agent are mixedly configured into coating, the mass concentration of coating is 10-20%;
The 6th step, nano-calcium carbonate slurry is heated to 60-80 ℃, then adds coating, coating is by the Ca (OH) that participates in reaction
2the 1-6% of total mass add, by the 5th step, be configured to the aqueous solution, the coated treatment time is 1-3 hour, obtains nm-class active calcium carbonate.
Said crystal structure adjusting agent is a kind of or its mixture in phosphoric acid salt, vitriol, acetate, Citrate trianion, monose or polysaccharide.
Said dispersion agent is one or more mixtures of chloride salt, polyacrylate.
Said lipid acid is C
12-C
18lipid acid, water-soluble metatitanic acid fat coupling agent is one or more in CT-54 coupling agent, propionic acid titanium CT-64 coupling agent or hydramine lipid acid titanium coupling agent.
Synthetic nm-class active calcium carbonate particle is controlled between 50-80nm as stated above, cube, and specific surface area is greater than 24m
2/ g, oil-absorption(number) is less than 27g/100gCaOC3, and good dispersity, without agglomeration, can be used as the functional stuffing of high-grade rubber, plastics and vehicle paint base.Adopt present method, 20% of the generated time that generated time is the production of the band stirring carbonization at low temperature precipitator method, product repetition rate reaches 99%.
The invention provides a kind of new method of preparing nm-class active calcium carbonate.The method is drawn the advantage that stirs the carbonization precipitator method, according to the ultimate principle of crystallography, introduce brilliant control agent and dispersion agent, significantly increase the carbonic acid gas tolerance that participates in reaction, search out the nano-calcium carbonate production method under a kind of and high speed of response, compare with traditional nano-calcium carbonate production technique, the method speed of response is high, and reaction finishing temperature is high, and the reaction times is short, product quality repetition rate is high, and reaction unit industrialization realizes easily.Complex optimum speed of response, rate of mass transfer, crystallization control three aspect factor, realized the control of the nucleation rate of crystal and the growth velocity of each crystal face.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment mono-:
The first step, at diameter, be that 3 meters of height are in the carburizing reagent still of 6 meters, to add the Ca (OH) of 40 cubic metres
2suspension, Ca (OH)
2the mass concentration of suspension is 7.92%;
Second step, adjustment Ca (OH)
2the temperature to 24 of suspension ℃;
The 3rd step, with the speed of 0.6-0.8 cube of meter per second, to the mixed gas that passes into carbonic acid gas and nitrogen in reactor, the volumetric concentration of carbon dioxide in gas mixture gas is 52%, after 10 minutes, as Ca (OH)
2when the carbonation rate of suspension reaches 8-10%, add the polysaccharide of 66 kilograms, continue carbonization, until Ca (OH)
2the pH value 6.85 of suspension, generates nano level calcite, and reaction finishing temperature is 61 ℃;
The 4th step, at Ca (OH)
2suspension in add the polyacrylate of 9 kilograms;
The 5th step, the lipid acid of 164 kilograms is configured to 10% aqueous solution coating;
The 6th step, nano-calcium carbonate slurry is heated to 85 ℃, then adds coating, the coated treatment time is 4 hours, obtains nm-class active calcium carbonate.
Embodiment bis-:
The first step, at diameter, be that 3 meters of height are in the carburizing reagent still of 6 meters, to add the Ca (OH) of high 35 cubic metres
2suspension, Ca (OH)
2the mass concentration of suspension is 8.0%;
Second step, adjustment Ca (OH)
2the temperature to 35 of suspension ℃;
The 3rd step, with the speed of 0.6-0.8 cube of meter per second to the mixed gas that passes into carbonic acid gas and nitrogen in reactor, the volumetric concentration of carbon dioxide in gas mixture gas is 52%, after 10 minutes, Ca (OH)
2when the carbonation rate of suspension reaches 8-10%, add polysaccharide and the phosphatic mixture of 50 kilograms, continue carbonization, until Ca (OH)
2the pH value 6.78 of suspension, generates nano level calcite, and reaction finishing temperature is 43 ℃; .
The 4th step, at Ca (OH)
2suspension in add 15Kg polyacrylate;
The 5th step, the lipid acid of 172 kilograms is configured to 10% aqueous solution coating;
The 6th step, nano-calcium carbonate slurry is heated to 85 ℃, then adds coating, the coated treatment time is 3 hours, obtains nm-class active calcium carbonate.
Claims (4)
1. normal temperature atm number is produced an industrial production process for nano-calcium carbonate, comprises the following steps:
The first step, in carburizing reagent still, add the Ca (OH) of the 60-80% of reactor volume
2suspension, Ca (OH)
2the mass concentration of suspension is 6-10%;
Second step, adjustment join the Ca (OH) in carburizing reagent still
2the temperature of suspension, makes it reach 25-40 ℃;
The 3rd step, with the speed of 0.6-0.8 cube of meter per second to the mixed gas that passes into carbonic acid gas and nitrogen in carburizing reagent still, in the volumetric concentration of this carbon dioxide in gas mixture gas, be 35%-60%, with Ca (OH)
2the mass concentration of suspension is that benchmark goes out Ca (OH)
2total mass, as Ca (OH)
2the Ca (OH) of participation and carbon dioxide reaction in suspension
2quality reach Ca (OH)
2the 8-10% of total mass time, add Ca (OH)
2the crystal structure adjusting agent of 0.5-2% of total mass, continue carbonization, until Ca (OH)
2the pH value of suspension reaches 6-7, generates nano level calcite, and temperature of reaction is controlled at 38-70 ℃;
The 4th step, at Ca (OH)
2suspension in add Ca (OH)
2the dispersion agent of 0.2-0.5 ‰ of total mass, by dispersion agent, be combined with calcium carbonate hydrophilic radical and form the surface charge that electrostatic double layer is adjusted nanoparticle;
The 5th step, one or both and water in lipid acid or water soluble peptide acid esters coupling agent are mixedly configured into coating, the mass concentration of coating is 10-20%;
The 6th step, nano-calcium carbonate slurry is heated to 60-80 ℃, then adds coating, coating is by the Ca (OH) that participates in reaction
2the 1-6% of total mass add, by the 5th step, be configured to the aqueous solution, the coated treatment time is 1-3 hour, obtains nm-class active calcium carbonate.
2. a kind of normal temperature atm number according to claim 1 is produced the industrial production process of nano-calcium carbonate, it is characterized in that, said crystal structure adjusting agent is a kind of or its mixture in phosphoric acid salt, vitriol, acetate, Citrate trianion, monose or polysaccharide.
3. a kind of normal temperature atm number according to claim 1 is produced the industrial production process of nano-calcium carbonate, it is characterized in that, said dispersion agent is one or more mixtures of chloride salt, polyacrylate.
4. a kind of normal temperature atm number according to claim 1 is produced the industrial production process of nano-calcium carbonate, it is characterized in that, said lipid acid is C
12-C
18lipid acid, water-soluble metatitanic acid fat coupling agent is one or more in CT-54 coupling agent, propionic acid titanium CT-64 coupling agent or hydramine lipid acid titanium coupling agent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556184A (en) * | 2014-12-12 | 2015-04-29 | 安徽雪城超细碳酸钙有限公司 | Method for producing industrial precipitation-type nano calcium carbonate |
| CN105175686A (en) * | 2015-10-01 | 2015-12-23 | 常州市奥普泰科光电有限公司 | Preparation method of epoxy resin modified by ultra-dispersed nano calcium carbonate |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1330039A (en) * | 2001-08-03 | 2002-01-09 | 上海卓越纳米新材料股份有限公司 | Industrial process for preparing nm-class active calcium carbonate |
| CN1631789A (en) * | 2003-12-24 | 2005-06-29 | 上海华明高技术（集团）有限公司 | Method for preparing nano calcium carbonate particle |
| CN101475759A (en) * | 2009-01-21 | 2009-07-08 | 山东海泽纳米材料有限公司 | Practical method for preparing high thixotropy surface treating nano calcium carbonate |
| CN101565198A (en) * | 2009-05-26 | 2009-10-28 | 建德市双超钙业有限公司 | Production method of nano calcium carbonate special for organosilicon |
| CN101570343A (en) * | 2009-06-11 | 2009-11-04 | 福建省万旗非金属材料有限公司 | Method for preparing nanometer calcium carbonate special for water soluble ink by wet method |
| CN101723429A (en) * | 2008-10-16 | 2010-06-09 | 上海华明高技术（集团）有限公司 | Method for manufacturing nano calcium carbonate from high-concentration carbon dioxide industrial exhaust gases |
| CN101734705A (en) * | 2009-11-26 | 2010-06-16 | 南召鑫泰钙业有限公司 | Method for preparing micro-control super fine calcium carbonate slurry |
| CN101967298A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Novel nano calcium carbonate used for plastic film and preparation method thereof |
| CN101967310A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Method for preparing nano calcium carbonate with low viscosity and medium thixotropic property |
| CN101967308A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Method for preparing nano calcium carbonate for high-temperature resistant polymers |
| CN102167915A (en) * | 2011-03-03 | 2011-08-31 | 淄博嘉泽纳米材料有限公司 | Preparation method of medium/low-viscosity high-thixotropy nano calcium carbonate for aqueous system |
| CN102491397A (en) * | 2011-12-09 | 2012-06-13 | 广东嘉维化工实业有限公司 | Preparation method of nano-calcium carbonate SCC-2 special for silicone sealant |
| CN102491395A (en) * | 2011-11-22 | 2012-06-13 | 曾庆铭 | Preparation method of nano-grade calcium carbonate |
-
2013
- 2013-10-22 CN CN201310498210.3A patent/CN103509378A/en active Pending
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1330039A (en) * | 2001-08-03 | 2002-01-09 | 上海卓越纳米新材料股份有限公司 | Industrial process for preparing nm-class active calcium carbonate |
| CN1631789A (en) * | 2003-12-24 | 2005-06-29 | 上海华明高技术（集团）有限公司 | Method for preparing nano calcium carbonate particle |
| CN101723429A (en) * | 2008-10-16 | 2010-06-09 | 上海华明高技术（集团）有限公司 | Method for manufacturing nano calcium carbonate from high-concentration carbon dioxide industrial exhaust gases |
| CN101475759A (en) * | 2009-01-21 | 2009-07-08 | 山东海泽纳米材料有限公司 | Practical method for preparing high thixotropy surface treating nano calcium carbonate |
| CN101565198A (en) * | 2009-05-26 | 2009-10-28 | 建德市双超钙业有限公司 | Production method of nano calcium carbonate special for organosilicon |
| CN101570343A (en) * | 2009-06-11 | 2009-11-04 | 福建省万旗非金属材料有限公司 | Method for preparing nanometer calcium carbonate special for water soluble ink by wet method |
| CN101734705A (en) * | 2009-11-26 | 2010-06-16 | 南召鑫泰钙业有限公司 | Method for preparing micro-control super fine calcium carbonate slurry |
| CN101967298A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Novel nano calcium carbonate used for plastic film and preparation method thereof |
| CN101967310A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Method for preparing nano calcium carbonate with low viscosity and medium thixotropic property |
| CN101967308A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Method for preparing nano calcium carbonate for high-temperature resistant polymers |
| CN102167915A (en) * | 2011-03-03 | 2011-08-31 | 淄博嘉泽纳米材料有限公司 | Preparation method of medium/low-viscosity high-thixotropy nano calcium carbonate for aqueous system |
| CN102491395A (en) * | 2011-11-22 | 2012-06-13 | 曾庆铭 | Preparation method of nano-grade calcium carbonate |
| CN102491397A (en) * | 2011-12-09 | 2012-06-13 | 广东嘉维化工实业有限公司 | Preparation method of nano-calcium carbonate SCC-2 special for silicone sealant |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556184A (en) * | 2014-12-12 | 2015-04-29 | 安徽雪城超细碳酸钙有限公司 | Method for producing industrial precipitation-type nano calcium carbonate |
| CN105175686A (en) * | 2015-10-01 | 2015-12-23 | 常州市奥普泰科光电有限公司 | Preparation method of epoxy resin modified by ultra-dispersed nano calcium carbonate |
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Application publication date: 20140115 |