CN1631791A - Superfine active calcium carbonate and its preparation process and application - Google Patents
Superfine active calcium carbonate and its preparation process and application Download PDFInfo
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- CN1631791A CN1631791A CN 200410084715 CN200410084715A CN1631791A CN 1631791 A CN1631791 A CN 1631791A CN 200410084715 CN200410084715 CN 200410084715 CN 200410084715 A CN200410084715 A CN 200410084715A CN 1631791 A CN1631791 A CN 1631791A
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- active calcium
- calcium carbide
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Abstract
Disclosed is a technique for preparing super-slim active calcium carbonate and the application of it, in the course of preparing calcium carbonate, carbonization and modification are done synchronously, the calcium carbonate particle prepared according to the technical method is cubic, its diameter is 70-150 nm, oil absorption number is 25-32, whiteness is 90-93, which can be applied in production of silicone adhesive whose sealant has remarkable cleanliness, thixotropy and strength. The invention has simple productive technique, short technical time, needs fewer equipments, with low cost.
Description
Technical field
The present invention relates to a kind of preparation technology of super-fine active calcium carbide and the treated carbonates that makes of technology and the application in silicone adhesive thereof thus.
Background technology
The present domestic technology of bubbling carbonizing method production at intermittence super-fine active calcium carbide that adopts is:
The Wingdale refuel calcined make CaO, add water and digest and make Ca (OH)
2Slurries carry out carbonization with carbonic acid gas then and make CaCO
3Slurries add surface-modifying agent again and activate and make active CaCO
3Slurries, dehydration makes CaCO
3Filter cake makes CaCO after the drying
3Dried cake is pulverized then and is finally made CaCO
3Fine powder.
The carbonation process devices needed is carburizing reagent still (strap clamp cover, an agitator), and the modification devices needed is modification still (strap clamp cover, an agitator).Because this method carbonization and modification are in two steps, make its complex manufacturing, the time is long, and equipment is many, and manufacturing cost is than higher.
Summary of the invention
At the deficiency that prior art exists, the object of the present invention is to provide that a kind of production technique is simple, the time is short, equipment is few, the preparation technology of the super-fine active calcium carbide of low cost of manufacture;
Another object of the present invention is to provide super-fine active calcium carbide obtained by this method;
Another object of the present invention is to provide the application of this super-fine active calcium carbide.
Goal of the invention of the present invention is achieved by the following technical solution:
A kind of preparation technology of super-fine active calcium carbide in turn includes the following steps:
A, with after the Wingdale refuel calcining, add hot water digestion, the Ca after sieving (OH)
2Concentration of slurry transfers to 8%-12%;
B, be the Ca (OH) that 8%-12%, temperature are with concentration
2Slurries are put into jacket reactor, after stirring, cooling off, feed carbonic acid gas and carry out carbonization, and the flow of carbonic acid gas is 300-600ml/min, adds Ca (OH) at the initial stage of carbonization
2The white sugar of the 0.2%-1.0% of quality and Ca (OH)
2The citric acid of the 0.2%-1.0% of quality, when carbonization 1-2 as a child after, add the surface-modifying agent of 1%-4%, on one side carbonization modification on one side, whole process need not heated;
The slurries that C, negate are answered phenolphthalein reagent titration, the phenolphthalein bleach then is reacted to terminal point, and the slurries that reaction is good make super-fine active calcium carbide through dehydration, drying, pulverizing.
Described surface-modifying agent is the mixture of being made up of sodium hydroxide, stearic acid, Oleum Cocois, and wherein stearic acid is the 1%-3% of calcium hydroxide solid content, and sodium hydroxide is stearic 25%-35%, and Oleum Cocois is the 1%-3% of calcium hydroxide solid content.
Slurries Ca (OH) in the described B step
2Temperature be 10-40 ℃.
According to the prepared calcium carbonate granule type of above-mentioned processing method looks is cubes, and size is the 70-150 nanometer, and oil-absorption(number) is 25-32, and whiteness is 90-93.
Smooth finish is good in the silicone sealant of working it out with calcium carbonate product of the present invention, and thixotropy is good, and intensity is good.
A kind of technology for preparing super-fine active calcium carbide of the present invention, because this method carbonization and modification are carried out simultaneously, it is simple therefore to have production technique, equipment is few, advantages such as low cost of manufacture, the calcium carbonate product produced of this processing method is used in the silicone sealant field in addition
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
How further specify the present invention below in conjunction with specific embodiment realizes:
Embodiment 1
Lime 3000 gram is put into the 20L bucket and is added hot water digestion, with 200 purpose sieve, the concentration of slurry after sieving is transferred to 11% after 1 hour, gets solid content and be 11% Ca (OH)
2Slurries 2000 grams, slurries are put into the reactor (strap clamp cover) of 5L, start agitator on the reactor, open the cooling water switch of reactor, make the temperature of slurries be reduced to 30 degree, open the flow valve of carbonic acid gas, regulating concentration of carbon dioxide is 30%, the flow of carbonic acid gas is transferred to 400ml/min, and the beginning carbonization is pressed Ca (OH) at the initial stage of carbonization
2Quality add 0.5% white sugar and citric acid, the purpose of white sugar is the size and the pattern of control calcium carbonate superfine powder, the purpose of citric acid is to reduce the concentration of calcium hydroxide slurry; After carbonization 1.5 as a child, add 4% surface-modifying agent, surface-modifying agent is by sodium hydroxide, stearic acid, Oleum Cocois synthetic, and the carbonation rate of this moment is about 30-50%, continues the modification on one side of carbonization on one side, and whole process need not heated.The terminal point of reaction is judged with phenolphthalein indicator.Concrete grammar: the slurries that negate is answered phenolphthalein reagent titration, look explanation reaction is not finished if phenolphthalein reddens, if the phenolphthalein bleach illustrates to be reacted to terminal point.Entire reaction is controlled to be finished in 3-4 hour.The slurries that reaction is good go dehydration again, and drying is pulverized.Hour finish.The slurries that reaction is good go dehydration again, and drying is pulverized.
Get lime 3000 gram and put into the 20L bucket and add hot water digestion, with 200 purpose sieve, the concentration of slurry after sieving is transferred to 9% after 1 hour, get solid content and be 9% Ca (OH)
2Slurries 2000 grams, slurries are put into the reactor (strap clamp cover) of 5L, start agitator on the reactor, open the cooling water switch of reactor, make the temperature of slurries be reduced to 20 degree, open the flow valve of carbonic acid gas, regulating concentration of carbon dioxide is 30%, the flow of carbonic acid gas is transferred to 300ml/min, and the beginning carbonization is pressed Ca (OH) at the initial stage of carbonization
2Quality add 0.3% white sugar and citric acid, the purpose of white sugar is the size and the pattern of control calcium carbonate superfine powder, the purpose of citric acid is to reduce the concentration of calcium hydroxide slurry; After carbonization 1.5 as a child, add 4% surface-modifying agent, surface-modifying agent is by sodium hydroxide, stearic acid, Oleum Cocois synthetic, and the carbonation rate of this moment is about 30-50%, continues the modification on one side of carbonization on one side, and whole process need not heated.The terminal point of reaction is judged with phenolphthalein indicator.Concrete grammar: the slurries that negate is answered phenolphthalein reagent titration, look explanation reaction is not finished if phenolphthalein reddens, if the phenolphthalein bleach illustrates to be reacted to terminal point.Entire reaction is controlled to be finished in 3-4 hour.The slurries that reaction is good go dehydration again, and drying is pulverized.
Making technical target of the product by above-mentioned technology is
| Index name | Index |
| ????CaCO 3Content % | ????96 |
| Granule-morphology | Cubes |
| Particle diameter nm | ????80～100 |
| Whiteness | ????92 |
| Oil-absorption(number) gDop/100gCaCO 3 | ????28 |
| Water ratio % | ????0.30 |
| The pH value | ????8.5 |
Smooth finish is good in the silicone sealant of working it out with this product, and thixotropy is good, and intensity is good.
Claims (6)
1, a kind of preparation technology of super-fine active calcium carbide in turn includes the following steps:
A, with after the Wingdale refuel calcining, add hot water digestion, the Ca after sieving (OH)
2Concentration of slurry transfers to 8%-12%;
B, be the Ca (OH) of 8%-12% with concentration
2Slurries are put into jacket reactor, after stirring, cooling off, feed carbonic acid gas and carry out carbonization, and the flow of carbonic acid gas is 300-600ml/min, adds Ca (OH) at the initial stage of carbonization
2The white sugar of the 0.2%-1.0% of quality and Ca (OH)
2The citric acid of the 0.2%-1.0% of quality, when carbonization 1-2 as a child after, add the surface-modifying agent of 1%-4%, on one side carbonization modification on one side, whole process need not heated;
The slurries that C, negate are answered phenolphthalein reagent titration, the phenolphthalein bleach then is reacted to terminal point, and the slurries that reaction is good make super-fine active calcium carbide through dehydration, drying, pulverizing.
2, the preparation technology of a kind of super-fine active calcium carbide according to claim 1 is characterized in that: the mixture of described surface-modifying agent for being made by sodium hydroxide, stearic acid, Oleum Cocois reaction.
3, the preparation technology of a kind of super-fine active calcium carbide according to claim 2 is characterized in that: stearic acid is the 1%-3% of calcium hydroxide solid content, and sodium hydroxide is stearic 25%-35%, and Oleum Cocois is the 1%-3% of calcium hydroxide solid content.
4, the preparation technology of a kind of super-fine active calcium carbide according to claim 1 is characterized in that: slurries Ca (OH) in the described B step
2Temperature be 10-40 ℃.
5, the super-fine active calcium carbide that makes by claim 1,2,3 or 4 described super-fine active calcium carbide preparation technologies, it is characterized in that: calcium carbonate granule type looks are cubes, and size is the 70-150 nanometer, and oil-absorption(number) is 25-32, and whiteness is 90-93.
6, super-fine active calcium carbide according to claim 5 is used for silicone sealant.
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| CN 200410084715 CN1631791A (en) | 2004-11-30 | 2004-11-30 | Superfine active calcium carbonate and its preparation process and application |
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| CN 200410084715 CN1631791A (en) | 2004-11-30 | 2004-11-30 | Superfine active calcium carbonate and its preparation process and application |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323947C (en) * | 2005-12-29 | 2007-07-04 | 上海耀华纳米科技有限公司 | Tech. for preparing super fine actived calcium carbonate with low oil absorpsion value |
| 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 |
| CN102796401A (en) * | 2012-08-17 | 2012-11-28 | 山东宝龙达胶业有限公司 | Preparation method of nanometer calcium carbonate with silica-stearic acid composite coating and special for silicone sealant |
| CN102910661A (en) * | 2012-09-14 | 2013-02-06 | 芮城新泰纳米材料有限公司 | Preparation method of high-reinforcement nanometer CaCO3 for silicone sealant |
| CN102936025A (en) * | 2012-10-26 | 2013-02-20 | 四川中际磁业有限责任公司 | Micro and nano-grade active light calcium carbonate automated production system |
| CN103011224A (en) * | 2012-12-07 | 2013-04-03 | 池州凯尔特纳米科技有限公司 | Preparation method of superfine active calcium carbonate functional filler special for PVC |
| CN104609453A (en) * | 2014-11-25 | 2015-05-13 | 广西华纳新材料科技有限公司 | Preparation method for cubic precipitated calcium carbonate |
| CN105233965A (en) * | 2015-11-06 | 2016-01-13 | 宣城新威华化工科技有限公司 | Powder disaggregation device |
| CN105329928A (en) * | 2015-12-10 | 2016-02-17 | 湖南化工职业技术学院 | Activation method for nanometer calcium carbonate |
| WO2020113964A1 (en) * | 2018-12-06 | 2020-06-11 | 东北大学 | Method for preparing nano calcium carbonate for enhancing yield of pvc automobile primer coating |
| CN111620359A (en) * | 2020-05-18 | 2020-09-04 | 河南鑫泰钙业有限公司 | Novel ultra-pure ultra-white large-sediment light calcium carbonate and production equipment and method thereof |
| CN111874934A (en) * | 2020-08-14 | 2020-11-03 | 王权广 | Process for preparing regular cubic crystal form nano calcium carbonate |
-
2004
- 2004-11-30 CN CN 200410084715 patent/CN1631791A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323947C (en) * | 2005-12-29 | 2007-07-04 | 上海耀华纳米科技有限公司 | Tech. for preparing super fine actived calcium carbonate with low oil absorpsion value |
| 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 |
| CN102796401A (en) * | 2012-08-17 | 2012-11-28 | 山东宝龙达胶业有限公司 | Preparation method of nanometer calcium carbonate with silica-stearic acid composite coating and special for silicone sealant |
| CN102910661A (en) * | 2012-09-14 | 2013-02-06 | 芮城新泰纳米材料有限公司 | Preparation method of high-reinforcement nanometer CaCO3 for silicone sealant |
| CN102936025A (en) * | 2012-10-26 | 2013-02-20 | 四川中际磁业有限责任公司 | Micro and nano-grade active light calcium carbonate automated production system |
| CN103011224A (en) * | 2012-12-07 | 2013-04-03 | 池州凯尔特纳米科技有限公司 | Preparation method of superfine active calcium carbonate functional filler special for PVC |
| CN104609453A (en) * | 2014-11-25 | 2015-05-13 | 广西华纳新材料科技有限公司 | Preparation method for cubic precipitated calcium carbonate |
| CN105233965A (en) * | 2015-11-06 | 2016-01-13 | 宣城新威华化工科技有限公司 | Powder disaggregation device |
| CN105329928A (en) * | 2015-12-10 | 2016-02-17 | 湖南化工职业技术学院 | Activation method for nanometer calcium carbonate |
| WO2020113964A1 (en) * | 2018-12-06 | 2020-06-11 | 东北大学 | Method for preparing nano calcium carbonate for enhancing yield of pvc automobile primer coating |
| CN111620359A (en) * | 2020-05-18 | 2020-09-04 | 河南鑫泰钙业有限公司 | Novel ultra-pure ultra-white large-sediment light calcium carbonate and production equipment and method thereof |
| CN111620359B (en) * | 2020-05-18 | 2024-04-26 | 河南鑫泰钙业有限公司 | Ultra-pure ultra-white heavy body light calcium carbonate and production equipment and method thereof |
| CN111874934A (en) * | 2020-08-14 | 2020-11-03 | 王权广 | Process for preparing regular cubic crystal form nano calcium carbonate |
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