CN104016391A - Method for preparing nanometer calcium carbonate for organic silicone electronic sealant by adopting continuous carbonization device - Google Patents
Method for preparing nanometer calcium carbonate for organic silicone electronic sealant by adopting continuous carbonization device Download PDFInfo
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Abstract
The invention relates to a method for preparing nanometer calcium carbonate for an organic silicone electronic sealant by adopting a continuous carbonization device. The method comprises the steps of feeding fine slurry containing a crystal form control agent and a dispersant into a Ca (OH)2 slurry tank, and then enabling the blended slurry to pass through the upper part of a carbonization reactor and continuously feed the slurry to the bubbling layer of the reactor and simultaneously introducing the kiln gas, carrying out gas-liquid-solid reaction on the slurry in the process that the slurry flows on the tower plates in the reactor to produce calcium carbonate as a precipitate, flowing the reacted material out from the outlet located at the bottom of the reactor, and then carrying out a wet modification treatment to obtain nanometer calcium carbonate which is cubic, has regular crystal form, concentrated particle size distribution and the rheological properties and can be added in an organic silicone electronic sealant. The product derived from the method according to the invention can impart the high thixotropy and low viscosity to the organic silicon electronic sealant, and no cracking, no chalking and no yellowing are generated in the temperature range (-45)-350 DEG C and the bonding is not damaged after the organic silicone electronic sealant is irradiated by ultraviolet ray.
Description
Technical field
The present invention relates to a kind of nano-calcium carbonate production method, refer to especially a kind of method that adopts continuous carbonization device to prepare organosilicon electronic seal glue nano-calcium carbonate.
Background technology
Nanometer grade calcium carbonate is the product innovation of just developing the late nineteen eighties in last century, the product that it has been generally acknowledged that the following particle diameter of 100nm is nano level product, nanometer grade calcium carbonate is mainly used in coating, structure glue, seal gum, ink, rubber, automobile bottom coat, plastics, papermaking, food, the aspects such as makeup.
Organic silicon electronic seal gum is the expensive goods in organosilicon sealant; be mainly used in bonding, sealing and the protection of electronic component and photovoltaic module; its purposes determines that it has special performance, i.e. good dielectric insulation performance, anti-ozone and ultraviolet ray, good cementability and good chemical stability, adaptive temperature wide ranges etc.The performance of organosilicon material can meet above-mentioned requirements substantially, so organic silicon electronic seal gum becomes one of important kind of electronic seal glue, but also there is obvious shortcoming in organosilicon sealant, intensity is low, thixotropy is poor, expensive, therefore need to add filler to carry out reinforcement, reduce costs and improve thixotropy.
Nm-class active calcium carbonate becomes one of filler of organic silicon electronic seal gum because having certain reinforcement.Organic silicon electronic seal gum has higher requirement to nano-calcium carbonate: 1) Nano particles of calcium carbonate regular crystal forms, centralized particle diameter, good dispersity; 2) different batches constant product quality; 3) there is good high-and low-temperature resistance performance and uvioresistant performance; 4) while interpolation, give organic silicon electronic seal gum high thixotropic and low viscous feature in organosilicon system.But there are following 2 shortcomings in existing explained hereafter nano calcium carbonate special for organosilicon: 1) existing explained hereafter nano-calcium carbonate adopts multistage spray carbonation, gravity Method more, carbonization at low temperature and intermittently bubbling carbonizing etc., Nano particles of calcium carbonate particle size distribution range that above-mentioned carbonization method causes carbonization to obtain because of the limitation of equipment of itself and technique is wide and the fluctuation of different batches quality product is large; 2) the existing properties-correcting agent of nm-class active calcium carbonate is generally lipid acid and soap, sylvic acid and sylvate, water-soluble titanate coupling agent, when the nano-calcium carbonate of these modifier modifications adds in organosilicon system, high-and low-temperature resistance performance and uvioresistant performance are not good, and can not possess high thixotroping and low viscous characteristic simultaneously.
Simultaneously, the chemical additives of conventional carbon metallization processes mostly is carbohydrate, organic acid, inorganic acids, protein-based and taking magnesium salts, barium salt, aluminium salt and sodium salt as main inorganic salts, by increasing the degree of supersaturation of solution and controlling the crystal face direction of growth and realize the synthetic of different crystal forms nano-calcium carbonate, the contained functional group in Nano particles of calcium carbonate surface being obtained by above-mentioned chemical additives is Ca-OH, and reactive behavior is low.
Summary of the invention
The technical problem that the present invention need solve is to provide a kind of production method that overcomes the defect of the Nano calcium carbonate dedicated existence of organic silicon electronic seal gum in prior art.
Proposed a kind of continuous carbonization device that adopts according to the technical problem of above-mentioned required solution and prepared the organosilicon electronic seal glue method of nano-calcium carbonate, the method is taking following carbonizer device as basis,
Described carbonizer tank body is provided with Ca (OH)
2slurries input aperture, carbonic acid gas CO
2input aperture and bottom be provided with discharge port, below these two input apertures of this body interior to bottom even be provided with outlet mutual dislocation horizontal column plate, what between the outlet of adjacent tray, adopt is S shape or snakelike reverse-flow baffle layout, described Ca (OH)
2slurries input aperture and CO
2input aperture is all positioned at the top of this body, and entrance the first layer tray outlet is provided with the sieve plate of vertical column plate, and bubble level is positioned at the top of reactor;
The step that described method comprises is,
Step 1, sends refining liquid into Ca (OH)
2slurry tank, Ca (OH)
2the mass concentration 7-12% of slurries, slurry temperature 20-30 DEG C, chemical additives addition accounts for Ca (OH)
2the 0.1-0.3% of total mass, dispersion agent addition accounts for Ca (OH)
2the 1-3% of total mass;
Step 2, deployed Ca (OH)
2slurries are continuously sent into the bubble level of reactor, slurry flow 20-35m by the top of carbonization reactor
3/ h;
Meanwhile, pass into the kiln gas through purifying treatment from carbonic acid gas gas distribution pipe, kiln gas flow is 15-40m
3/ h, volume fraction>=20% of carbonic acid gas in kiln gas;
Ca (OH)
2on the column plate of slurries in reactor, in mobile process, carry out gas, liquid, solid phase reaction and generate precipitated chalk, reacted material flows out from the bottom outlet of reactor;
Step 3, the nano-calcium carbonate slurries that obtain carry out wet-process modified processing, the addition 2-4%CaCO of surface treatment agent
3total mass, modification is carried out in activation kettle, agitator speed 200-300 r/min, churning time 1-1.5h;
Step 4, by the modified nano calcium carbonate slurries press filtration obtaining, dry, depolymerization, packaging.
Wherein, described chemical additives is the water glass in silicate, one or more of potassium silicate.Described dispersion agent be alkylbenzene sulfonate, alkyl-sulphate, phosphatic one or more.Described surface treatment agent is one or more in methoxy silane coupling agent, Ethoxysilane coupling agent and other silane coupling agents in silane coupling agent.
According to the synthetic nm-class active calcium carbonate median size of the inventive method between 70-80nm, cubes, crystalline form is regular, centralized particle diameter, specific surface area 18-30m
2/ g, oil-absorption(number)≤30g/100g.Rheological characteristics (synthetic modified nano calcium carbonate, o-phthalic acid dibutyl ester and the calcium oxide of the present invention adds by a certain percentage and high speed shear mixes, and leaves standstill and carries out rheology testing for 24 hours): viscosity 380-430cp(shearing rate 316.7s
-1), structure recovery time 2.906-3.050s, yield value 1.36-1.50Pa.Rheological property shows that product of the present invention adds in organic silicon electronic seal gum, can give its high thixotroping and low viscous feature, and in-45 DEG C to 350 DEG C range of temperature seal gum without be full of cracks, without efflorescence, without xanthochromia, and after ultraviolet irradiation bonding without destroy.
Embodiment
The inventive method is to adopt the continuous carbonization reactor of the ZL201110159221 granted patent that has of the applicant to carry out the synthetic of nano-calcium carbonate.This carbonization reactor is made up of the horizontal pedal that exports mutual dislocation, Ca (OH)
2slurries input aperture is on the top of reactor, and entrance the first layer tray outlet is provided with the sieve plate of vertical column plate, and bubble level is positioned at the top of reactor.The top that carbonic acid gas gas distribution pipe is positioned at reactor is array arrangement, and carbon dioxide is covered with whole reactor cavity.Ca (OH)
2on the column plate of slurries in reactor, in mobile process, carry out gas, liquid, solid phase reaction and generate precipitated chalk, reacted material flows out from the bottom outlet of reactor.This reactor because of carbonization crystal nucleation phase and vegetative period separately, the nucleation reaction period is positioned at reactor upper tray region or bubbling region, be arranged in reactor, lower region vegetative period, nucleation areal pressure is large compared with growth district reaction pressure, temperature is low, carbon dioxide and Ca (OH)
2concentration is high, and nucleation quantity is large, flows out nucleation district and enter vitellarium after nucleation, because of the time period that particle stops in nucleation district, the titanium pillaring solution that the nucleation period generates time on the nucleus generating is short and consistent, therefore the nanoparticle regular crystal forms obtaining, particle size distribution range is narrow, constant product quality.
Utilizing on the basis of aforementioned continuous carbonization device, the inventive method realizes by controlling following processing condition.
1) refining liquid is sent into Ca (OH)
2slurry tank, Ca (OH)
2the mass concentration 7-12% of slurries, slurry temperature 20-30 DEG C, chemical additives addition 0.1-0.3% Ca (OH)
2total mass, dispersion agent addition 1-3% Ca (OH)
2total mass.
Said chemical additives is that potassium silicate in silicate is or/and one or more of water glass.The chemical additives of conventional carbon metallization processes mostly is carbohydrate, organic acid, inorganic acids, protein-based and inorganic salts, inorganic salts mainly contains magnesium salts, barium salt, aluminium salt and sodium salt, by increasing the degree of supersaturation of solution and controlling the crystal face direction of growth and realize the synthetic of different crystal forms nano-calcium carbonate, the contained functional group in Nano particles of calcium carbonate surface being obtained by above-mentioned chemical additives is Ca-OH, and reactive behavior is low.The present invention adopts silicate to do chemical additives, and effect has two: 1) by increasing solution degree of supersaturation and controlling crystal face direction of growth synthesis of cubic body Nano particles of calcium carbonate; 2) thus silicate issues unboiled water solution-condensation reaction in carbonic acid gas effect to be generated colloidal sol and is deposited in Nano particles of calcium carbonate surface, the Si-OH that makes Nano particles of calcium carbonate surface contain high reaction activity, in follow-up modification process, can generate more firmly chemical bond with organic modifiers generation dehydration condensation, and Nano particles of calcium carbonate and organic modifiers that Ca-OH is contained on surface are mainly coated on ion surface by physical force form, less stable.Said dispersion agent be alkylbenzene sulfonate, alkyl-sulphate, phosphatic one or more.
2) deployed Ca (OH)
2slurries are continuously sent into the bubble level of reactor, slurry flow 20-35m by the top of carbonization reactor
3/ h.By Different Ca (OH)
2the switching of slurry tank realizes slurry and successively inputs, and realizes continuous production truly.
3) pass into the kiln gas through purifying treatment from carbonic acid gas gas distribution pipe, flow is 15-40m
3/ h, volume fraction>=20% of carbonic acid gas in kiln gas.
4) the nano-calcium carbonate slurries that obtain carry out wet-process modified processing, and surface treatment agent is silane coupling agent, the addition 2-4%CaCO of surface treatment agent
3total mass, modification is carried out in activation kettle, agitator speed 200-300 r/min, churning time 1-1.5h.
Said silane coupling agent is one or more in methoxy silane coupling agent, Ethoxysilane coupling agent and other silane coupling agents.
Silane coupling agent contains hydrolysable group and organic group, can there is condensation reaction formation-Si-O-Si-key with the silicon hydroxyl on Nano particles of calcium carbonate surface (realizing Nano particles of calcium carbonate surface silanol group by the chemical additives of 1 step) in hydrolysising group, make silane coupling agent be wrapped in firmly the surface of nano-calcium carbonate, and organic group is arranged in the outside of calcium carbonate particles, can with polymer formation chemical bond, compare with conventional properties-correcting agent, silane coupler modified nano-calcium carbonate has better consistency and dispersiveness in organosilicon system, thereby give organosilicon sealant high thixotroping, low viscous feature, conventional properties-correcting agent is organic acid, high temperature meeting cracking, and the nano-calcium carbonate resistance to elevated temperatures that modification obtains is not good, and the not cracking of nano-calcium carbonate high temperature of process modification of the present invention have good high-and low-temperature resistance performance, and uvioresistant irradiation behaviour is better.
5) modified nano calcium carbonate slurries press filtration, dry, depolymerization, packaging.
The invention will be further described by the following examples.
Embodiment 1
1) toward Ca (OH)
2in slurry tank, pump into concentration and be 7.0% refining, open to stir and add 0.10% Ca (OH)
2total mass potassium silicate is or/and water glass adds 1.0% Ca (OH)
2the sodium alkyl benzene sulfonate of total mass, adjusts slurry temperature to 25 DEG C.
2) in carbonization reactor, input the kiln gas through purifying, carbonic acid gas volumetric concentration is 20%, kiln gas flow is 15m
3/ h, pumps into 1 after passing into kiln gas 5min) Ca (OH) in step
2slurries, slurry flow 20m
3/ h.
3) carbonization reactor exports the ripe slurry obtaining and continuously inputs in activation kettle, realizes the switching of entering slurry between different activation kettles by the liquid level control switch of activation kettle.The stirring of opening activation kettle, agitator speed 200r/min, adds 2.5%CaCO
3the methyltrimethoxy silane coupling agent of total mass, stirs 1h after properties-correcting agent adds.
4) the modified nano calcium carbonate slurries in step, through press filtration, dry, depolymerization, packaging, obtain finished product.
Embodiment 2
1) toward Ca (OH)
2in slurry tank, pump into concentration and be 8.0% refining, open to stir and add 0.15% Ca (OH)
2the potassium silicate of total mass is or/and water glass adds 1.5% Ca (OH)
2the Sodium hexametaphosphate 99 of total mass, adjusts slurry temperature to 23 DEG C.
2) in carbonization reactor, input the kiln gas through purifying, carbonic acid gas volumetric concentration is 25%, kiln gas flow is 20 m
3/ h, pumps into 1 after passing into kiln gas 5min) Ca (OH) in step
2slurries, slurry flow 25m
3/ h.
3) carbonization reactor exports the ripe slurry obtaining and continuously inputs in activation kettle, realizes the switching of entering slurry between different activation kettles by the liquid level control switch of activation kettle.Open the stirring of activation kettle, agitator speed 230r/min, adds the dimethyldimethoxysil,ne of 2.3%CaCO3 total mass, after properties-correcting agent adds, stirs 1.5h.
4) the modified nano calcium carbonate slurries in step, through press filtration, dry, depolymerization, packaging, obtain finished product.
Embodiment 3
1) toward Ca (OH)
2in slurry tank, pump into concentration and be 9.0% refining, open to stir and add 0.2% Ca (OH)
2the potassium silicate of total mass is or/and water glass adds 2.0% Ca (OH)
2the sodium alkyl benzene sulfonate of total mass, adjusts slurry temperature to 25 DEG C.
2) in carbonization reactor, input the kiln gas through purifying, carbonic acid gas volumetric concentration is 30%, kiln gas flow is 25 m
3/ h, pumps into 1 after passing into kiln gas 5min) Ca (OH) in step
2slurries, slurry flow 30m
3/ h.
3) carbonization reactor exports the ripe slurry obtaining and continuously inputs in activation kettle, realizes the switching of entering slurry between different activation kettles by the liquid level control switch of activation kettle.Open the stirring of activation kettle, agitator speed 260r/min, adds the aminopropyl trimethoxysilane properties-correcting agent of 2.0%CaCO3 total mass to stir 1.5h after adding.
4) the modified nano calcium carbonate slurries in step, through press filtration, dry, depolymerization, packaging, obtain finished product.
Embodiment 4
1) toward Ca (OH)
2in slurry tank, pump into concentration and be 10.0% refining, open to stir and add 0.25% Ca (OH)
2the potassium silicate of total mass is or/and water glass adds 2.5% Ca (OH)
2the Sodium hexametaphosphate 99 of total mass, adjusts slurry temperature to 28 DEG C.
2) in carbonization reactor, input the kiln gas through purifying, carbonic acid gas volumetric concentration is 33%, kiln gas flow is 30 m
3/ h, pumps into 1 after passing into kiln gas 5min) Ca (OH) in step
2slurries, slurry flow 32m
3/ h.
3) carbonization reactor exports the ripe slurry obtaining and continuously inputs in activation kettle, realizes the switching of entering slurry between different activation kettles by the liquid level control switch of activation kettle.Open the stirring of activation kettle, agitator speed 280r/min, add 3.0%CaCO3 total mass-aminopropyl triethoxysilane, after properties-correcting agent adds, stir 1.5h.
4) the modified nano calcium carbonate slurries in step, through press filtration, dry, depolymerization, packaging, obtain finished product.
Embodiment 5
1) toward Ca (OH)
2in slurry tank, pump into concentration and be 11.0% refining, open to stir and add 0.25% Ca (OH)
2the potassium silicate of total mass is or/and water glass adds 2.5% Ca (OH)
2the sodium alkyl benzene sulfonate of total mass, adjusts slurry temperature to 30 DEG C.
2) in carbonization reactor, input the kiln gas through purifying, carbonic acid gas volumetric concentration is 32%, kiln gas flow is 35 m
3/ h, pumps into 1 after passing into kiln gas 5min) Ca (OH) in step
2slurries, slurry flow 35m
3/ h.
3) carbonization reactor exports the ripe slurry obtaining and continuously inputs in activation kettle, realizes the switching of entering slurry between different activation kettles by the liquid level control switch of activation kettle.Open the stirring of activation kettle, agitator speed 280r/min, adds the isobutyl triethoxy silane of 2.8%CaCO3 total mass, after properties-correcting agent adds, stirs 1.5h.
4) the modified nano calcium carbonate slurries in step, through press filtration, dry, depolymerization, packaging, obtain finished product.
Embodiment 6
1) toward Ca (OH)
2in slurry tank, pump into concentration and be 12.0% refining, open to stir and add 0.3% Ca (OH)
2the potassium silicate of total mass is or/and water glass adds 3.0% Ca (OH)
2the Sodium hexametaphosphate 99 of total mass, adjusts slurry temperature to 30 DEG C.
2) in carbonization reactor, input the kiln gas through purifying, carbonic acid gas volumetric concentration is 35%, kiln gas flow is 40 m
3/ h, pumps into 1 after passing into kiln gas 5min) Ca (OH) in step
2slurries, slurry flow 35m
3/ h.
3) carbonization reactor exports the ripe slurry obtaining and continuously inputs in activation kettle, realizes the switching of entering slurry between different activation kettles by the liquid level control switch of activation kettle.Open the stirring of activation kettle, agitator speed 300r/min, adds the dimethyldiethoxysilane of 3.2%CaCO3 total mass, after properties-correcting agent adds, stirs 1.5h.
4) the modified nano calcium carbonate slurries in step, through press filtration, dry, depolymerization, packaging, obtain finished product.
Claims (4)
1. adopt continuous carbonization device to prepare the organosilicon electronic seal glue method of nano-calcium carbonate, the method is taking following carbonizer device as basis,
Described carbonizer tank body is provided with Ca (OH)
2slurries input aperture, carbonic acid gas CO
2the discharge port that input aperture and bottom are provided with, below two input apertures of this body interior to bottom even be provided with the horizontal column plate of outlet mutual dislocation, what between the outlet of adjacent tray, adopt is S shape or snakelike reverse-flow baffle layout, described Ca (OH)
2slurries input aperture and CO
2input aperture is all positioned at the top of this body, and entrance the first layer tray outlet is provided with the sieve plate of vertical column plate, and bubble level is positioned at the top of reactor;
The step that described method comprises is,
Step 1, sends refining liquid into Ca (OH)
2slurry tank, Ca (OH)
2the mass concentration 7-12% of slurries, slurry temperature 20-30 DEG C, chemical additives addition accounts for Ca (OH)
2the 0.1-0.3% of total mass, dispersion agent addition accounts for Ca (OH)
2the 1-3% of total mass;
Step 2, deployed Ca (OH)
2slurries are continuously sent into the bubble level of reactor, slurry flow 20-35m by the top of carbonization reactor
3/ h;
Meanwhile, pass into the kiln gas through purifying treatment from carbonic acid gas gas distribution pipe, kiln gas flow is 15-40m
3/ h, volume fraction>=20% of carbonic acid gas in kiln gas;
Ca (OH)
2on the column plate of slurries in reactor, in mobile process, carry out gas, liquid, solid phase reaction and generate precipitated chalk, reacted material flows out from the bottom outlet of reactor;
Step 3, the nano-calcium carbonate slurries that obtain carry out wet-process modified processing, the addition 2-4%CaCO of surface treatment agent
3total mass, modification is carried out in activation kettle, agitator speed 200-300 r/min, churning time 1-1.5h;
Step 4, by the modified nano calcium carbonate slurries press filtration obtaining, dry, depolymerization, packaging.
2. the method for preparing organosilicon electronic seal glue nano-calcium carbonate according to claim 1, is characterized in that, described chemical additives is the water glass in silicate, one or more of potassium silicate.
3. prepare the organosilicon electronic seal glue method of nano-calcium carbonate according to claim 1, it is characterized in that, described dispersion agent be alkylbenzene sulfonate, alkyl-sulphate, phosphatic one or more.
4. prepare the method for organosilicon electronic seal glue nano-calcium carbonate according to claim 1, it is characterized in that, described surface treatment agent is one or more in methoxy silane coupling agent, Ethoxysilane coupling agent and other silane coupling agents in silane coupling agent.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104497633A (en) * | 2014-11-25 | 2015-04-08 | 广西华纳新材料科技有限公司 | Nano calcium carbonate surface treatment method |
| CN104843757A (en) * | 2015-04-16 | 2015-08-19 | 四川海雅粉体科技有限责任公司 | Coil pipe type nano calcium carbonate carbonization system |
| CN104927398A (en) * | 2014-06-10 | 2015-09-23 | 池州市富华粉体科技有限公司 | Preparation method of active light calcium carbonate |
| CN105883883A (en) * | 2016-04-20 | 2016-08-24 | 广西平南县恒祥钙业有限公司 | Preparation method of special nano calcium carbonate for polyurethane sealant |
| CN106277015A (en) * | 2016-08-22 | 2017-01-04 | 连州市万仕达新材料有限公司 | The preparation method that a kind of polyurethane sealant is Nano calcium carbonate dedicated |
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| CN110028094A (en) * | 2018-07-31 | 2019-07-19 | 荆门市东宝区凯龙矿业股份有限公司 | A kind of production method of high thixotropic active nano-calcium carbonate |
| CN110127741A (en) * | 2019-04-21 | 2019-08-16 | 宣城新威华化工科技有限公司 | A kind of nm-class active calcium carbonate preparation method applied to pvc plastisol |
| CN112299465A (en) * | 2020-10-30 | 2021-02-02 | 广西大学 | Synthetic method of modified porous calcium carbonate |
| CN113307295A (en) * | 2021-06-25 | 2021-08-27 | 安徽前江超细粉末科技有限公司 | Method for producing nano calcium carbonate by using kiln gas with low carbon dioxide concentration |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5792440A (en) * | 1995-09-20 | 1998-08-11 | Chemical Lime Company | Method of manufacturing high purity calcium carbonate |
| CN101108741A (en) * | 2006-07-21 | 2008-01-23 | 北京市化工建材厂 | Industrial process for preparing nm-class active calcium carbonate |
| CN102295306A (en) * | 2011-06-14 | 2011-12-28 | 连州市凯恩斯纳米材料有限公司 | Carbonizer for continuously synthesizing calcium carbonate and production method of 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 |
| CN102701255A (en) * | 2012-06-21 | 2012-10-03 | 石家庄市红日钙业有限公司 | Method for high-concentration carbonization production of spherical nano calcium carbonate |
| CN102849771A (en) * | 2012-08-29 | 2013-01-02 | 池州凯尔特纳米科技有限公司 | Continuous carbonization reaction device, and method for preparing ultrafine calcium carbonate through applying it |
| CN103011226A (en) * | 2012-12-07 | 2013-04-03 | 池州凯尔特纳米科技有限公司 | Method for preparing nano calcium carbonate through nucleation and growth step by step |
-
2014
- 2014-04-10 CN CN201410141781.6A patent/CN104016391A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5792440A (en) * | 1995-09-20 | 1998-08-11 | Chemical Lime Company | Method of manufacturing high purity calcium carbonate |
| CN101108741A (en) * | 2006-07-21 | 2008-01-23 | 北京市化工建材厂 | Industrial process for preparing nm-class active calcium carbonate |
| CN102295306A (en) * | 2011-06-14 | 2011-12-28 | 连州市凯恩斯纳米材料有限公司 | Carbonizer for continuously synthesizing calcium carbonate and production method of 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 |
| CN102701255A (en) * | 2012-06-21 | 2012-10-03 | 石家庄市红日钙业有限公司 | Method for high-concentration carbonization production of spherical nano calcium carbonate |
| CN102849771A (en) * | 2012-08-29 | 2013-01-02 | 池州凯尔特纳米科技有限公司 | Continuous carbonization reaction device, and method for preparing ultrafine calcium carbonate through applying it |
| CN103011226A (en) * | 2012-12-07 | 2013-04-03 | 池州凯尔特纳米科技有限公司 | Method for preparing nano calcium carbonate through nucleation and growth step by step |
Non-Patent Citations (1)
| Title |
|---|
| 曾蕾等: ""纳米碳酸钙的制备、表面改性及应用进展"", 《精细化工中间体》 * |
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|---|---|---|---|---|
| CN104927398A (en) * | 2014-06-10 | 2015-09-23 | 池州市富华粉体科技有限公司 | Preparation method of active light calcium carbonate |
| CN104497633B (en) * | 2014-11-25 | 2017-04-19 | 广西华纳新材料科技有限公司 | Nano calcium carbonate surface treatment method |
| CN104497633A (en) * | 2014-11-25 | 2015-04-08 | 广西华纳新材料科技有限公司 | Nano calcium carbonate surface treatment method |
| CN104843757A (en) * | 2015-04-16 | 2015-08-19 | 四川海雅粉体科技有限责任公司 | Coil pipe type nano calcium carbonate carbonization system |
| US10676620B2 (en) | 2015-07-31 | 2020-06-09 | Omya International Ag | Precipitated calcium carbonate with improved resistance to structural breakdown |
| CN107848829A (en) * | 2015-07-31 | 2018-03-27 | Omya国际股份公司 | The winnofil destroyed with improved resistive connection structure |
| US11111388B2 (en) | 2015-07-31 | 2021-09-07 | Omya International Ag | Precipitated calcium carbonate with improved resistance to structural breakdown |
| CN105883883A (en) * | 2016-04-20 | 2016-08-24 | 广西平南县恒祥钙业有限公司 | Preparation method of special nano calcium carbonate for polyurethane sealant |
| CN106277015A (en) * | 2016-08-22 | 2017-01-04 | 连州市万仕达新材料有限公司 | The preparation method that a kind of polyurethane sealant is Nano calcium carbonate dedicated |
| CN110028094A (en) * | 2018-07-31 | 2019-07-19 | 荆门市东宝区凯龙矿业股份有限公司 | A kind of production method of high thixotropic active nano-calcium carbonate |
| CN110127741A (en) * | 2019-04-21 | 2019-08-16 | 宣城新威华化工科技有限公司 | A kind of nm-class active calcium carbonate preparation method applied to pvc plastisol |
| CN112299465A (en) * | 2020-10-30 | 2021-02-02 | 广西大学 | Synthetic method of modified porous calcium carbonate |
| CN113307295A (en) * | 2021-06-25 | 2021-08-27 | 安徽前江超细粉末科技有限公司 | Method for producing nano calcium carbonate by using kiln gas with low carbon dioxide concentration |
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