CN105417565A - Cubic CaCO3 and SiO2 composite particles and preparing method thereof - Google Patents

Cubic CaCO3 and SiO2 composite particles and preparing method thereof Download PDF

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Publication number
CN105417565A
CN105417565A CN201510781047.0A CN201510781047A CN105417565A CN 105417565 A CN105417565 A CN 105417565A CN 201510781047 A CN201510781047 A CN 201510781047A CN 105417565 A CN105417565 A CN 105417565A
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composite particles
sio
caco
cube
calcium carbonate
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庞起
刘旭
郭豪
韩行健
杨昊
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Guangxi Co Ltd Of Calcium Carbonate Industrialization Chinese Academy Of Engineering
Guangxi University
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Guangxi Co Ltd Of Calcium Carbonate Industrialization Chinese Academy Of Engineering
Guangxi University
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Abstract

The invention discloses a preparing method for cubic CaCO3 and SiO2 composite particles. The preparing method includes the steps that nano calcium carbonate prepared through a carbonization method is used as a raw material, while calcium hydroxide is carbonized into calcium carbonate, surface modification is carried out by using sulfuric acid as a crystal form control agent, polyethylene glycol as a dispersing agent and silica sol as a surface modifier, the surface of calcium carbonate is coated with nano silica sol, and the cubic CaCO3 and SiO2 composite particles are prepared through one step. Compared with a traditional method, the preparing method adopts the one-step method and has the advantages of being short in time, high in efficiency, easy to operate, low in cost and the like. The obtained cubic CaCO3 and SiO2 composite particle product is uniform in size and crystal form, pure and free of impurities and is coated completely.

Description

Cube CaCO 3siO 2composite particles and preparation method thereof
Technical field
The invention belongs to silica modified nano calcium carbonate technical field, particularly relate to a kind of cube CaCO 3siO 2composite particles and preparation method thereof.
Background technology
Calcium carbonate is a kind of important inorganic materials, along with the development of nanotechnology, emerging nano-calcium carbonate, as the mineral filler that a kind of character is more excellent, is widely used in the fields such as rubber, plastics, papermaking, senior ink, coating, medicine, food, makeup.Calcium carbonate brightening, reinforcement, replacement reduce to compare in polymkeric substance total cost has obvious advantage with other fillers, calcium carbonate raw material sources are wide simultaneously, and preparation process is easy to control, and cost is low.Have data to show, current calcium carbonate as the usage quantity of polymer packing up to 80%.Industrial, often for preparing the main production process of nano-calcium carbonate, and wherein there is carbonic acid gas and disperse the shortcoming that inequality, utilization ratio are not high in the solution in carborization, and obtained calcium carbonate size is uneven, crystal formation is different.
Nano-calcium carbonate obtains Nano-meter CaCO3 after coated with silica 3siO 2composite particles, considerably increases its application in industries such as rubber, plastics, papermaking, coating and polymers.Through the nano calcium carbonate composite material of coated with silica, the characteristic of calcium carbonate and silicon-dioxide can be embodied simultaneously.Can be used in some field substituting white carbon black costly, increase economic efficiency.Prepare Nano-meter CaCO3 at present 3siO 2composite particles mainly carries out surface modification by silicon dioxide granule or water glass to the calcium carbonate prepared, and its technique is roughly divided into following three kinds:
One, Fang Jingnan etc. [1]with Yang Jinxin etc. [2]1 μm of calcium carbonate and 30-40nm silicon dioxide granule are stirred for some time with 1000rpm, obtains composite particles presoma, then add hmds (HMDS), in 140 DEG C of reaction 5h, obtain the CaCO of finishing 3/ SiO 2composite particles, CaCO 3particle and Nano-meter SiO_2 2particle.But this method operating process is divided into two steps, more complicated, finished product and containing CaCO in addition 3particle and Nano-meter SiO_2 2the non-targeted products such as particle.
Two, Liu Run waits quietly [3], Jiang Xiaoyi etc. [4]with Liu Guojun etc. [5]respectively to make calcium carbonate and 40-60nm finished product calcium carbonate by oneself for raw material, add water glass, under 80-85 DEG C of condition, use H 2sO 4regulate pH=5-9, ageing 2-4h, after filtration, washing, dry CaCO 3/ SiO 2composite particles, but the standby composite particles of this legal system is mainly with spherical or other irregularly shaped existence, and size of particles is uneven, also introduces SO in operating process 4 2-impurity.
Three, Ma Cuicui etc. [6], Hua Yimiao etc. [7]with Shi Qi etc. [8]respectively to make 50-70nm calcium carbonate and 70nm finished product calcium carbonate by oneself for raw material, under 80-90 DEG C of condition, drip water glass, pass into CO simultaneously 2to keep the pH=8-9 of system, last ageing 2-4h, through washing, filter, dry 60-80nmCaCO 3/ SiO 2composite particles, but this method is divided into two steps, complicated operation, and obtained composite particles size is uneven, and crystal formation is different, and introduces more Na in modifying process +.
[1] Fang Jingnan, Hong Biyuan, Tong Wei, etc. based on CaCO 3/ SiO 2super hydrophobic surface preparation [J] of composite particles. journal of Zhejiang university (Edition), 2011-3,38 (2): 189-193.
[2] Yang Jinxin, Wen Xiufang, Pi Pihui, waits .CaCO 3siO 2the surface tissue of composite particles coating and hydrophobic performance research [J] thereof. Journal of Inorganic Materials, 2009,24 (1): 91-96.
[3] Liu Runjing, Zou Haikui, Guo Fen, etc. nuclear-shell structure type Nano-meter CaCO3 3siO 2nH 2the preparation [J] of O composite particles. investigation of materials journal, 2001,15 (1): 61-64.
[4] Jiang Xiaoyi, Xie Gang, Geng Kai, etc. application CaCO 3siO 2the research [J] of nanometer composite technology modified polypropene. Heilongjiang University's natural science journal, 2010-2,27 (1): 96-125.
[5] Liu Guojun, once Chinese. Nano-meter CaCO3 3/ SiO 2the preparation [J] of nucleocapsid structure composite particles. aerospace material technique, 2003 (3): 57-61.
[6] Ma Cuicui, old snow plum. nuclear shell structured nano-CaCO 3siO 2the preparation [J] of composite particles. chemistry world, 2010, (4): 196-213.
[7] Hua Yimiao, Yuan Jun, Yue Linhai, waits .SiO 2coated CaCO 3crystallite analysis and XPS research [J]. Chinese Journal of Inorganic Chemistry, 2001-1,1:134-138.
[8] Shi Qi, Wu Sufang. precipitator method SiO 2clad nano CaCO 3performance of the adsorbent [J]. university of chemical technology's journal, 2009-2,60 (2): 507-513.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of cube CaCO 3siO 2composite particles and preparation method thereof, this method has that the time is short, efficiency is high, operation is simple, low cost and other advantages, gained cube CaCO 3siO 2composite particles product size is even, crystal formation is consistent, coated complete, pure nothing is mixed.
For solving the problems of the technologies described above, the present invention by the following technical solutions: cube CaCO 3siO 2the preparation method of composite particles, the nano-calcium carbonate obtained with carborization is for raw material, while calcium hydroxide carbonization becomes calcium carbonate, utilize that sulfuric acid is chemical additives, polyoxyethylene glycol is dispersion agent, silicon sol carries out surface modification for surface-modifying agent, Nano silica sol is coated on calcium carbonate surface, realizes a step and complete obtained cube CaCO 3siO 2composite particles.
The particle diameter of nano-calcium carbonate at 20-60nm, cube CaCO 3siO 2composite particles median size is 30-80nm.
Above-mentioned cube CaCO 3siO 2the preparation method of composite particles, comprises the following steps:
Unslaked lime drops in the water of 80 DEG C by <1>, in dispersion impeller, digest 2-4h with rotating speed 1000rpm; Gained calcium hydroxide suspension liquid is crossed 200 mesh standard sieves, then adds the suspension liquid that water is made into massfraction 4-12wt%, ageing 24h, stand-by;
<2> is by calcium hydroxide suspension liquid in step <1>, disperse with rotating speed 1000-1200rpm line cut in dispersion impeller, add sulphuric acid soln, control carbonization temperature 10-15 DEG C, pass into CO from bottom 2and N 2mixed gas carry out carbonization; After starting carburizing reagent 5min, add polyoxyethylene glycol and silicon sol solution, final carbonization, to pH=6.5-7.0, obtains nano-complex particle slurries;
Slurries water-bath in step <2> is heated to 80 DEG C by <3>, passes into CO in this process 2and N 2mixed gas keep pH=6.5-7.0, the calcium hydroxide carbonization that is wrapped by is complete, and be incubated ageing 1h, finally by filtration, washing, dry, to obtain final product.
The amount of the sulfuric acid added in step <2>, polyoxyethylene glycol and silicon sol is respectively 0.6-1.0wt%, 0.5-2.0wt%, 5-20wt% by the mass percent accounting for calcium carbonate theoretical yield.
Polyoxyethylene glycol is one or more in PEG-400, PEG-600, PEG-1000.
Nano silica sol median size in silicon sol solution is 5-20nm, pH=9.0-10.5.
The cube CaCO of above-mentioned preparation method's gained 3siO 2composite particles.
For current silica modified nano calcium carbonate Problems existing, we have established a kind of cube CaCO 3siO 2the preparation method of composite particles, the nano-calcium carbonate obtained with carborization is for raw material, while calcium hydroxide carbonization becomes calcium carbonate, utilize that sulfuric acid is chemical additives, polyoxyethylene glycol is dispersion agent, silicon sol carries out surface modification for surface-modifying agent, Nano silica sol is coated on calcium carbonate surface, realizes a step and complete obtained cube CaCO 3siO 2composite particles.Wherein, dispersion agent polyoxyethylene glycol mainly contains two kinds of effects: one is produce with sulfuric acid to act synergistically, and impels system to generate a large amount of nucleus at the carbonization initial stage, and stops calcium carbonate particles reunion to be grown up in carbonization process, and reaches the effect making particle thinner; Two be system when high speed line cut disperses, it promotes that mixed gas is dispersed into a large amount of tiny bubble, effectively improves utilization rate of carbon dioxide, shortens the reaction times, reaches and reduces the effect of production cost.Relative to traditional method, the present invention adopts single stage method, has that the time is short, efficiency is high, operation is simple, low cost and other advantages, gained cube CaCO 3siO 2composite particles product size is even, crystal formation is consistent, coated complete, pure nothing is mixed.
Accompanying drawing explanation
Fig. 1 is one of nm level CaCO_3 SiO2 composite particles transmission electron microscope picture (scale 100nm)
Fig. 2 is nm level CaCO_3 SiO2 composite particles transmission electron microscope picture two (scale 100nm)
Fig. 3 is nm level CaCO_3 SiO2 composite particles transmission electron microscope picture three (scale 500nm)
Embodiment
Embodiment 1
8.74g unslaked lime drops in the water of 280g80 DEG C by <1>, in dispersion impeller, digest 2h with rotating speed 1000rpm; Gained calcium hydroxide suspension liquid is crossed 200 mesh standard sieves, then adds the suspension liquid that water is made into massfraction 4wt%, ageing 24h, stand-by;
<2> is by calcium hydroxide suspension liquid in step <1>, disperse with rotating speed 1000rpm line cut in dispersion impeller, add 0.52g30% sulphuric acid soln, controlling carbonization temperature is 15 DEG C, passes into certain flow rate (60/120m from bottom 3.h -1.m -3suspension liquid) CO 2and N 2mixed gas carry out carbonization; After starting carburizing reagent 5min, add PEG-600 and 15.60g20% silicon sol solution (its SiO of 1.04g30% 2median size is 5-10nm, pH is 9.0-10.5), final carbonization, to pH=7.0, obtains nano-complex particle slurries;
Slurries water-bath in step <2> is heated to 80 DEG C by <3>, passes into a small amount of CO in this process 2and N 2mixed gas keep pH=6.5-7.0, the calcium hydroxide carbonization that is wrapped by is complete, and be incubated ageing 1h, finally by filtration, washing, dry, to obtain final product.
Result: after testing, the particle diameter of the not coated nano-calcium carbonate synthesized in intermediate steps <2> at 20-50nm, Surface coating SiO obtained in final step <3> 2caCO 3siO 2composite particles size evenly (40-60nm), crystal formation consistent (overwhelming majority is cube, other shapes on a small quantity), completely coated.
Embodiment 2
13.32g unslaked lime drops in the water of 280g80 DEG C by <1>, in dispersion impeller, digest 2h with rotating speed 1000rpm; Gained calcium hydroxide suspension liquid is crossed 200 mesh standard sieves, then adds the suspension liquid that water is made into massfraction 6wt%, ageing 24h, stand-by;
<2> is by calcium hydroxide suspension liquid in step <1>, disperse with rotating speed 1000rpm line cut in dispersion impeller, add 0.63g30% sulphuric acid soln, controlling carbonization temperature is 14 DEG C, passes into certain flow rate (60/120m from bottom 3.h -1.m -3suspension liquid) CO 2and N 2mixed gas carry out carbonization; After starting carburizing reagent 5min, add PEG-1000 and 17.83g20% silicon sol solution (its SiO of 1.19g30% 2median size is 10-20nm, pH is 9.0-10.5), final carbonization, to pH=7.0, obtains nano-complex particle slurries;
Slurries water-bath in step <2> is heated to 80 DEG C by <3>, passes into a small amount of CO in this process 2and N 2mixed gas keep pH=6.5-7.0, the calcium hydroxide carbonization that is wrapped by is complete, and be incubated ageing 1h, finally by filtration, washing, dry, to obtain final product.
Result: after testing, the particle diameter of the not coated nano-calcium carbonate synthesized in intermediate steps <2> at 20-50nm, Surface coating SiO obtained in final step <3> 2caCO 3siO 2composite particles size evenly (40-70nm), crystal formation consistent (overwhelming majority is cube, other shapes on a small quantity), completely coated.
Embodiment 3
32.21g unslaked lime drops in the water of 280g80 DEG C by <1>, in dispersion impeller, digest 2h with rotating speed 1000rpm; Gained calcium hydroxide suspension liquid is crossed 200 mesh standard sieves, then adds the suspension liquid that water is made into massfraction 8wt%, ageing 24h, stand-by;
<2> is by calcium hydroxide suspension liquid in step <1>, disperse with rotating speed 1000rpm line cut in dispersion impeller, add 0.64g30% sulphuric acid soln, controlling carbonization temperature is 11 DEG C, passes into certain flow rate (60/120m from bottom 3.h -1.m -3suspension liquid) CO 2and N 2mixed gas carry out carbonization; After starting carburizing reagent 5min, add PEG-600 and 16.11g10% silicon sol solution (its SiO of 1.07g30% 2median size is 5-10nm, pH is 9.0-10.5), final carbonization, to pH=6.7, obtains nano-complex particle slurries;
Slurries water-bath in step <2> is heated to 80 DEG C by <3>, passes into a small amount of CO in this process 2and N 2mixed gas keep pH=6.5-7.0, the calcium hydroxide carbonization that is wrapped by is complete, and be incubated ageing 1h, finally by filtration, washing, dry, to obtain final product.
Result: after testing, the particle diameter of the not coated nano-calcium carbonate synthesized in intermediate steps <2> at 20-40nm, Surface coating SiO obtained in final step <3> 2caCO 3siO 2composite particles size evenly (30-60nm), crystal formation consistent (overwhelming majority is cube, other shapes on a small quantity), completely coated.
Embodiment 4
27.97g unslaked lime drops in the water of 280g80 DEG C by <1>, in dispersion impeller, digest 2h with rotating speed 1000rpm; Gained calcium hydroxide suspension liquid is crossed 200 mesh standard sieves, then adds the suspension liquid that water is made into massfraction 12wt%, ageing 24h, stand-by;
<2> is by calcium hydroxide suspension liquid in step <1>, disperse with rotating speed 1000rpm line cut in dispersion impeller, add 1.0g30% sulphuric acid soln, controlling carbonization temperature is 10 DEG C, passes into certain flow rate (60/120m from bottom 3.h -1.m -3suspension liquid) CO 2and N 2mixed gas carry out carbonization; After starting carburizing reagent 5min, add PEG-400 and 24.97g5% silicon sol solution (its SiO of 0.83g30% 2median size is 5-10nm, pH is 9.0-10.5), final carbonization, to pH=6.5, obtains nano-complex particle slurries;
Slurries water-bath in step <2> is heated to 80 DEG C by <3>, passes into a small amount of CO in this process 2and N 2mixed gas keep pH=6.5-7.0, the calcium hydroxide carbonization that is wrapped by is complete, and be incubated ageing 1h, finally by filtration, washing, dry, to obtain final product.
Result: after testing, the particle diameter of the not coated nano-calcium carbonate synthesized in intermediate steps <2> at 30-60nm, Surface coating SiO obtained in final step <3> 2caCO 3siO 2composite particles size evenly (40-80nm), crystal formation consistent (overwhelming majority is cube, other shapes on a small quantity), completely coated.

Claims (7)

1. a cube CaCO 3siO 2the preparation method of composite particles, it is characterized in that: the nano-calcium carbonate obtained with carborization is for raw material, while calcium hydroxide carbonization becomes calcium carbonate, utilize that sulfuric acid is chemical additives, polyoxyethylene glycol is dispersion agent, silicon sol carries out surface modification for surface-modifying agent, Nano silica sol is coated on calcium carbonate surface, realizes a step and complete obtained cube CaCO 3siO 2composite particles.
2. cube CaCO according to claim 1 3siO 2the preparation method of composite particles, is characterized in that: the particle diameter of described nano-calcium carbonate at 20-60nm, described cube CaCO 3siO 2composite particles median size is 30-80nm.
3. cube CaCO according to claim 1 3siO 2the preparation method of composite particles, is characterized in that comprising the following steps:
Unslaked lime drops in the water of 80 DEG C by <1>, in dispersion impeller, digest 2-4h with rotating speed 1000rpm; Gained calcium hydroxide suspension liquid is crossed 200 mesh standard sieves, then adds the suspension liquid that water is made into massfraction 4-12wt%, ageing 24h, stand-by;
<2> is by calcium hydroxide suspension liquid in step <1>, disperse with rotating speed 1000-1200rpm line cut in dispersion impeller, add sulphuric acid soln, control carbonization temperature 10-15 DEG C, pass into CO from bottom 2and N 2mixed gas carry out carbonization; After starting carburizing reagent 5min, add polyoxyethylene glycol and silicon sol solution, final carbonization, to pH=6.5-7.0, obtains nano-complex particle slurries;
Slurries water-bath in step <2> is heated to 80 DEG C by <3>, passes into CO in this process 2and N 2mixed gas keep pH=6.5-7.0, the calcium hydroxide carbonization that is wrapped by is complete, and be incubated ageing 1h, finally by filtration, washing, dry, to obtain final product.
4. cube CaCO according to claim 3 3siO 2the preparation method of composite particles, is characterized in that the amount of sulfuric acid, polyoxyethylene glycol and the silicon sol added in step <2> is respectively 0.6-1.0wt%, 0.5-2.0wt%, 5-20wt% by the mass percent accounting for calcium carbonate theoretical yield.
5. cube CaCO according to claim 3 3siO 2the preparation method of composite particles, is characterized in that: described polyoxyethylene glycol is one or more in PEG-400, PEG-600, PEG-1000.
6. cube CaCO according to claim 3 3siO 2the preparation method of composite particles, is characterized in that: the Nano silica sol median size in described silicon sol solution is 5-20nm, pH=9.0-10.5.
7. the cube CaCO of arbitrary preparation method's gained described in claim 1 to 6 3siO 2composite particles.
CN201510781047.0A 2015-11-13 2015-11-13 Cubic CaCO3 and SiO2 composite particles and preparing method thereof Pending CN105417565A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105819484A (en) * 2016-03-11 2016-08-03 广西大学 Preparation method and dispersing method of nano CaCO3/SiO2 composite particle
CN105883882A (en) * 2016-04-19 2016-08-24 广西大学 Aqueous slurry of nano calcium carbonate as well as preparation method and application thereof
CN105907206A (en) * 2016-06-14 2016-08-31 东莞市联洲知识产权运营管理有限公司 Preparation method of high-hardness abrasion-resistant water-borne wood paint
CN106398448A (en) * 2016-06-14 2017-02-15 东莞市联洲知识产权运营管理有限公司 Preparation method for environment-friendly waterborne paint
CN109422287A (en) * 2017-08-23 2019-03-05 范佳晨 A kind of preparation method of calcium carbonate-silica composite powder
CN109796035A (en) * 2019-03-01 2019-05-24 燕卓君 A kind of preparation method of calcium carbonate superfine powder
CN111606345A (en) * 2020-05-28 2020-09-01 金三江(肇庆)硅材料股份有限公司 Preparation method of light calcium carbonate and silicon dioxide composite material
CN113861939A (en) * 2021-10-19 2021-12-31 兰州交通大学 Micro-nano calcium carbonate @ silicon dioxide composite material with super-hydrophobic property and preparation method and application thereof

Non-Patent Citations (2)

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郑岚等: ""立方形超细碳酸钙的制备研究"", 《无机盐工业》 *
马翠翠等: ""核-壳结构纳米CaCO3/SiO2复合粒子"", 《化学世界》 *

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105819484A (en) * 2016-03-11 2016-08-03 广西大学 Preparation method and dispersing method of nano CaCO3/SiO2 composite particle
CN105883882A (en) * 2016-04-19 2016-08-24 广西大学 Aqueous slurry of nano calcium carbonate as well as preparation method and application thereof
CN105883882B (en) * 2016-04-19 2019-02-22 广西大学 Water-soluble serous and preparation method thereof, the application of a kind of nanometer grade calcium carbonate
CN105907206A (en) * 2016-06-14 2016-08-31 东莞市联洲知识产权运营管理有限公司 Preparation method of high-hardness abrasion-resistant water-borne wood paint
CN106398448A (en) * 2016-06-14 2017-02-15 东莞市联洲知识产权运营管理有限公司 Preparation method for environment-friendly waterborne paint
CN109422287A (en) * 2017-08-23 2019-03-05 范佳晨 A kind of preparation method of calcium carbonate-silica composite powder
CN109796035A (en) * 2019-03-01 2019-05-24 燕卓君 A kind of preparation method of calcium carbonate superfine powder
CN109796035B (en) * 2019-03-01 2021-04-23 湖南金箭新材料科技有限公司 Preparation method of superfine calcium carbonate
CN111606345A (en) * 2020-05-28 2020-09-01 金三江(肇庆)硅材料股份有限公司 Preparation method of light calcium carbonate and silicon dioxide composite material
CN111606345B (en) * 2020-05-28 2020-12-15 金三江(肇庆)硅材料股份有限公司 Preparation method of light calcium carbonate and silicon dioxide composite material
CN113861939A (en) * 2021-10-19 2021-12-31 兰州交通大学 Micro-nano calcium carbonate @ silicon dioxide composite material with super-hydrophobic property and preparation method and application thereof
CN113861939B (en) * 2021-10-19 2023-09-12 兰州交通大学 Micro-nano calcium carbonate@silicon dioxide composite material with super-hydrophobic property and preparation method and application thereof

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