CN109422287A - A kind of preparation method of calcium carbonate-silica composite powder - Google Patents
A kind of preparation method of calcium carbonate-silica composite powder Download PDFInfo
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- CN109422287A CN109422287A CN201710730524.XA CN201710730524A CN109422287A CN 109422287 A CN109422287 A CN 109422287A CN 201710730524 A CN201710730524 A CN 201710730524A CN 109422287 A CN109422287 A CN 109422287A
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- calcium carbonate
- silica
- composite powder
- silica composite
- calcium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of calcium carbonate-silica composite powder preparation methods, comprising: (1) using ethyl orthosilicate as raw material, dehydrated alcohol is added, stirs 20~40min, adds ammonium hydroxide, continue 1~2h of stirring, obtain silica suspension；(2) deionized water is added in Xiang Shangshu silica suspension, calcium hydroxide powder is added under stirring conditions, stirs evenly, is passed through the carbon dioxide of certain volume ratio and the mixed gas of nitrogen, adjusting pH value is 8~10, obtains calcium carbonate-silica mixture；(3) calcium carbonate-silica mixture is aged to 1~3h under the conditions of 20~30 DEG C, is filtered, dehydrated alcohol is respectively adopted and deionized water is washed 3~5 times, dry, grinding obtains calcium carbonate-silica composite powder.In calcium carbonate made from method in the present invention-silica composite powder, by addition silica, it can be effectively prevent the reunion of calcium carbonate particle, meanwhile, the acid resistance of the composite powder greatly improves.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of calcium carbonate-silica composite powder preparation side
Method.
Background technique
Nm-class active calcium carbonate is widely applied in the industries such as coating, rubber, plastics as a kind of functional filler,
Main purpose is to improve the comprehensive performance and reduction production cost of product.
But there is also more problems in actual application for nm-class active calcium carbonate: first is that due to calcium carbonate
Surface characteristic determines, is preferably mainly stearic acid processing to this surface treatment effect, due to the unicity system of surface treating agent
The about expansion of application field；Second is that the product handled by stearic acid when silicon rubber etc. is used there are the bad dispersibility of product,
Reunite serious, does not give full play to the advantage of nano-powder；Third is that since calcium carbonate itself will decompose in micro acid medium
The characteristic for releasing carbon dioxide, constrains its use scope.
Therefore, people study calcium carbonate synthesis when particle size and pattern control while, be more concerned with surface treatment
In the process for the research of the acid resistance of product and dispersibility.How to improve calcium carbonate powder dispersibility and acid resistance at
For the target of people's research.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of calcium carbonate-silica composite powder,
It is able to solve problems of the prior art.
Summary of the invention
It is existing to overcome the purpose of the present invention is to provide a kind of calcium carbonate-silica composite powder preparation method
Deficiency in technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of calcium carbonate-silica composite powder, comprising:
(1) using ethyl orthosilicate as raw material, dehydrated alcohol is added, stirs 20~40min, adds ammonium hydroxide, continue stirring 1
~2h, obtains silica suspension；
(2) deionized water is added in Xiang Shangshu silica suspension, calcium hydroxide powder is added under stirring conditions,
It stirs evenly, is passed through the carbon dioxide of certain volume ratio and the mixed gas of nitrogen, adjusting pH value is 8~10, obtains calcium carbonate-
Silica mixture；
(3) calcium carbonate-silica mixture is aged to 1~3h under the conditions of 20~30 DEG C, filters, is respectively adopted
Dehydrated alcohol and deionized water are washed 3~5 times, dry, and grinding obtains calcium carbonate-silica composite powder.
Preferably, in step (1), the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:10
~15:10~20.
Preferably, in step (2), the ratio between volume of the silica suspension and the deionized water be 1:1.5~
2.5。
Preferably, in step (2), in the mixed gas, the ratio between volume of the carbon dioxide and the nitrogen is 1:1
~3.
Preferably, in the calcium carbonate-silica composite powder, the mass ratio of silicon and calcium is 3~10%.
Preferably, in the calcium carbonate-silica composite powder, the mass ratio of silicon and calcium is 3~8%.
Compared with the prior art, the advantages of the present invention are as follows: calcium carbonate-silica made from the method in the present invention is multiple
Close powder in, by be added silica, the reunion of calcium carbonate particle can be effectively prevent, meanwhile, the composite powder it is acidproof
Property greatly improves.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of calcium carbonate-silica composite powder, comprising:
(1) using ethyl orthosilicate as raw material, dehydrated alcohol is added, stirs 20~40min, adds ammonium hydroxide, continue stirring 1
~2h, obtains silica suspension；
(2) deionized water is added in Xiang Shangshu silica suspension, calcium hydroxide powder is added under stirring conditions,
It stirs evenly, is passed through the carbon dioxide of certain volume ratio and the mixed gas of nitrogen, adjusting pH value is 8~10, obtains calcium carbonate-
Silica mixture；
(3) calcium carbonate-silica mixture is aged to 1~3h under the conditions of 20~30 DEG C, filters, is respectively adopted
Dehydrated alcohol and deionized water are washed 3~5 times, dry, and grinding obtains calcium carbonate-silica composite powder.
In above-mentioned steps (1), the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:10~
15:10~20, it is preferred that the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:10:20.
In above-mentioned steps (2), the ratio between volume of the silica suspension and the deionized water is 1:1.5~2.5,
Preferably, the ratio between volume of the silica suspension and the deionized water is 1:2.
In above-mentioned steps (2), in the mixed gas, the ratio between volume of the carbon dioxide and the nitrogen be 1:1~
3, it is preferred that the ratio between volume of the carbon dioxide and the nitrogen is 1:2.
In the calcium carbonate according to made from the above method-silica composite powder, the mass ratio of silicon and calcium is 3~
10%, it is preferred that the mass ratio of silicon and calcium is 3~8%, it is furthermore preferred that the mass ratio of silicon and calcium is 5%.
Embodiment 1
(1) using ethyl orthosilicate as raw material, dehydrated alcohol is added, stirs 30min, adds ammonium hydroxide, continues to stir 2h, obtain
To silica suspension, wherein the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:10:
20；
(2) it is 1:2 according to the ratio between volume, deionized water is added in Xiang Shangshu silica suspension, in the condition of stirring
Lower addition calcium hydroxide powder, stirs evenly, and is passed through mixed gas of the certain volume than carbon dioxide and nitrogen for 1:2, adjusts
Saving pH value is 9, obtains calcium carbonate-silica mixture；
(3) calcium carbonate-silica mixture is aged 2h at 20 °C, filters, anhydrous second is respectively adopted
Pure and mild deionized water is washed 3~5 times, dry, and grinding obtains calcium carbonate-silica composite powder.
In the calcium carbonate according to made from the method in above-described embodiment-silica composite powder, the quality of silicon and calcium it
Than being 5%.
Embodiment 2
(1) using ethyl orthosilicate as raw material, dehydrated alcohol is added, stirs 30min, adds ammonium hydroxide, continues to stir 2h, obtain
To silica suspension, wherein the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:12:
15；
(2) it is 1:1.5 according to the ratio between volume, deionized water is added in Xiang Shangshu silica suspension, in the item of stirring
Calcium hydroxide powder is added under part, stirs evenly, is passed through mixed gas of the certain volume than carbon dioxide and nitrogen for 1:1,
Adjusting pH value is 9, obtains calcium carbonate-silica mixture；
(3) calcium carbonate-silica mixture is aged 2h at 20 °C, filters, anhydrous second is respectively adopted
Pure and mild deionized water is washed 3~5 times, dry, and grinding obtains calcium carbonate-silica composite powder.
In the calcium carbonate according to made from the method in above-described embodiment-silica composite powder, the quality of silicon and calcium it
Than being 10%.
Embodiment 3
(1) using ethyl orthosilicate as raw material, dehydrated alcohol is added, stirs 30min, adds ammonium hydroxide, continues to stir 2h, obtain
To silica suspension, wherein the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:15:
10。
(2) it is 1:2.5 according to the ratio between volume, deionized water is added in Xiang Shangshu silica suspension, in the item of stirring
Calcium hydroxide powder is added under part, stirs evenly, is passed through mixed gas of the certain volume than carbon dioxide and nitrogen for 1:3,
Adjusting pH value is 9, obtains calcium carbonate-silica mixture；
(3) calcium carbonate-silica mixture is aged 2h at 20 °C, filters, anhydrous second is respectively adopted
Pure and mild deionized water is washed 3~5 times, dry, and grinding obtains calcium carbonate-silica composite powder.
In the calcium carbonate according to made from the method in above-described embodiment-silica composite powder, the quality of silicon and calcium it
Than being 3%.
In calcium carbonate made from method in the present invention-silica composite powder, by the way that silica, Neng Gouyou is added
Effect prevents the reunion of calcium carbonate particle, meanwhile, the acid resistance of the composite powder greatly improves.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (6)
1. a kind of calcium carbonate-silica composite powder preparation method characterized by comprising
(1) using ethyl orthosilicate as raw material, be added dehydrated alcohol, stir 20~40min, add ammonium hydroxide, continue stirring 1~
2h obtains silica suspension；
(2) deionized water is added in Xiang Shangshu silica suspension, calcium hydroxide powder, stirring is added under stirring conditions
Uniformly, it is passed through the carbon dioxide of certain volume ratio and the mixed gas of nitrogen, adjusting pH value is 8~10, obtains calcium carbonate-dioxy
SiClx mixture；
(3) calcium carbonate-silica mixture is aged to 1~3h under the conditions of 20~30 DEG C, filters, is respectively adopted anhydrous
Ethyl alcohol and deionized water are washed 3~5 times, dry, and grinding obtains calcium carbonate-silica composite powder.
2. calcium carbonate according to claim 1-silica composite powder preparation method, which is characterized in that step (1)
In, the ethyl orthosilicate, the dehydrated alcohol, the ammonium hydroxide weight ratio be 1:10~15:10~20.
3. calcium carbonate according to claim 1-silica composite powder preparation method, which is characterized in that step (2)
In, the ratio between volume of the silica suspension and the deionized water is 1:1.5~2.5.
4. calcium carbonate according to claim 1-silica composite powder preparation method, which is characterized in that step (2)
In, in the mixed gas, the ratio between volume of the carbon dioxide and the nitrogen is 1:1~3.
5. calcium carbonate according to claim 1-silica composite powder preparation method, which is characterized in that the carbon
In sour calcium-silica composite powder, the mass ratio of silicon and calcium is 3~10%.
6. calcium carbonate according to claim 5-silica composite powder preparation method, which is characterized in that the carbon
In sour calcium-silica composite powder, the mass ratio of silicon and calcium is 3~8%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113350511A (en) * | 2021-03-01 | 2021-09-07 | 郎俊娜 | Novel sterile powder filling mixed protective gas for injection |
| CN114933763A (en) * | 2022-06-29 | 2022-08-23 | 立达超微科技(安徽青阳)有限公司 | Preparation method of polyolefin reinforced master batch |
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| JPH021527B2 (en) * | 1984-10-12 | 1990-01-11 | Osaka Packing | |
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| CN101637434A (en) * | 2009-08-27 | 2010-02-03 | 天津大学 | Preparation method of nuclear shell type CaCO3/SiO2 toothpaste abrasive |
| CN105417565A (en) * | 2015-11-13 | 2016-03-23 | 广西大学 | Cubic CaCO3 and SiO2 composite particles and preparing method thereof |
| CN105819484A (en) * | 2016-03-11 | 2016-08-03 | 广西大学 | Preparation method and dispersing method of nano CaCO3/SiO2 composite particle |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH021527B2 (en) * | 1984-10-12 | 1990-01-11 | Osaka Packing | |
| CN101225245A (en) * | 2008-01-31 | 2008-07-23 | 上海卓越纳米新材料股份有限公司 | Method for preparing core-shell silicon dioxide coated nano calcium carbonate |
| CN101637434A (en) * | 2009-08-27 | 2010-02-03 | 天津大学 | Preparation method of nuclear shell type CaCO3/SiO2 toothpaste abrasive |
| CN105417565A (en) * | 2015-11-13 | 2016-03-23 | 广西大学 | Cubic CaCO3 and SiO2 composite particles and preparing method thereof |
| CN105819484A (en) * | 2016-03-11 | 2016-08-03 | 广西大学 | Preparation method and dispersing method of nano CaCO3/SiO2 composite particle |
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| 赵兴等: "溶胶-凝胶法制备CaCO3 /SiO2复合粒子", 《人工晶体学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113350511A (en) * | 2021-03-01 | 2021-09-07 | 郎俊娜 | Novel sterile powder filling mixed protective gas for injection |
| CN113350511B (en) * | 2021-03-01 | 2024-01-02 | 郎俊娜 | Novel sterile powder filling mixed shielding gas for injection |
| CN114933763A (en) * | 2022-06-29 | 2022-08-23 | 立达超微科技(安徽青阳)有限公司 | Preparation method of polyolefin reinforced master batch |
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Application publication date: 20190305 |