CN1375456A - Nano level active calcium carbonate for special use - Google Patents
Nano level active calcium carbonate for special use Download PDFInfo
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- CN1375456A CN1375456A CN 02110801 CN02110801A CN1375456A CN 1375456 A CN1375456 A CN 1375456A CN 02110801 CN02110801 CN 02110801 CN 02110801 A CN02110801 A CN 02110801A CN 1375456 A CN1375456 A CN 1375456A
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- calcium carbonate
- special use
- nano level
- slurry
- level active
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Abstract
The preparation method of nano active special-purpose calcium carbonate includes the following steps: making CO2 and Ca(OH)2 product synthesis reaction at 28 plus or minus 1 deg.C; adding crystal growth inhibitor, when the slurry reaches to PH 6.7-7.0, heating, ageing and carbonizing at low speed rate; adding CO2 to calcium carbonate slurry, stirring at high speed and retaining for a certain time at about 85 deg.C; adding surfactant; dewatering and drying; and adding again a certain quantity of surfactant in the course of pulverization, mixing, homogenizing, sieving and packaging to obtain the invented product.
Description
Technical field
Nano level active calcium carbonate for special use of the present invention relates to a kind of lime carbonate, preparation method and its usage.
Background technology
The lime carbonate preparation method has multiple, is by making calcium hydroxide after the carbonoxide hydrolysis, being made by calcium hydroxide and carbon dioxide reaction.But the operational path difference, the performance of crystalline texture difference, particle diameter difference, product is also different with purposes.
Summary of the invention
The objective of the invention is to: a kind of nano level active calcium carbonate for special use, method for making and purposes are provided.
Purpose of the present invention can be achieved through the following technical solutions: a kind of nano level active calcium carbonate for special use is characterized in that: lime carbonate is cubic granules shape breast, and particle diameter 60～90nm has thixotropic behavior.
A kind of preparation method of nano level active calcium carbonate for special use is finished by multinomial step, the first step, carbonic acid gas (CO
2) and calcium hydroxide (Ca (OH)
2) carry out building-up reactions, temperature is at 28 ℃ ± 1 ℃; Second step, drop into the crystal growth inhibitor, slurry reaches PH6.7～7.0 and o'clock begins to add thermal aging, low rate carbonization; In the 3rd step, the calcium carbonate slurry after the carbonization adds CO
2High-speed stirring keeps certain hour about 85 ℃; In the 4th step, add synthetic good tensio-active agent; The 5th step, dehydration, drying; In the 6th step, in crushing process, mix a certain amount of surface treatment agent once more, mix sieve powder packing after the homogenizing.
Wherein, synthetic good tensio-active agent is to inject clear water earlier in still, and the ratio of the water yield and active material is 25: 1, and active material is 200
#Stearic acid and sodium stearate, stearic consumption are to be 1～3% of lime carbonate total amount in the slurry.The ratio of stearic acid and sodium stearate is 1: 0.3～2, and water temperature is 90 ℃ ± 1 ℃ during reaction, drops into sodium stearate and stearic acid successively, and is stirred.
Described crystal growth inhibitor is sucrose or other crystal growth modifiers that is fit to.
Nano level active calcium carbonate for special use of the present invention can be widely used in multiple plastisol.
Product cut size of the present invention is evenly distributed, and the granule-morphology cubes has thixotropic behavior.
Description of drawings
Accompanying drawing 1, process flow sheet of the present invention.
Embodiment:
A kind of nano level active calcium carbonate for special use is cubic granules shape breast, and particle diameter 60～90nm has thixotropic behavior.Shown in figure process flow sheet of the present invention, its preparation method branch multistep is carried out suddenly:
At first carry out raw material and prepare, select fat lime for use, its activity degree is greater than 300ml/4HCl, with 50 ℃ ± 1 ℃ hot water, water and lime (CaCO
3) in digester, clear up into lime slurry in 10: 1 ratios, lime slurry filters through three grade of 200 eye mesh screen filtration, wet cyclone, one-level 325 mesh sieve orders and flows into the mediation groove, is formulated into Ca (OH) in the mediation groove
2Concentration 8～11% is cooled off standby.
Lime slurry after the preparation is flowed into the carbonization still begin to stir through scale tank metering back, and begin to cool down or heat its Ca of titration (OH) that takes a sample when being controlled at 28 ℃ ± 1 ℃
2Concentration is measured CO
2Concentration.
Nano level active calcium carbonate for special use preparation method: the first step, CO
2With Ca (OH)
2Carry out building-up reactions, 28 ℃ ± 1 ℃ of temperature is according to CO
2With Ca (OH)
2Concentration and 3.46 * 10
-3Mol/1.min carbonization speed is determined CO
2Flow, carburizing reagent 60 minutes; Second step, drop into crystal growth inhibitor AR grade cane sugar, input amount is pressed Ca (OH)
2Concentration of being measured and CO
2The CaCO that complete reaction is produced
31～3% of weight, CO is closed in low rate continuous carbonization 15 minutes then
2Air valve, when slurry reaction during to PH6.7～7.0, in the whole carbonation reaction, slurry temperature is controlled between 28 ℃ ± 1 ℃ all the time; In the 3rd step, the slurry after the carbonization flows into and coats still, and coat still and adopt the heating of steam spacer, high-speed stirring, and in heat-processed, inject CO
2, 1/5th when injection rate is carbonization is heated to 85 ℃, keeps 2 hours; The 4th step, inject synthetic good tensio-active agent, slurry continues to keep temperature and stirred 2 hours, enters the homogenizing that homogenization groove carries out slurry then; The 5th step, adopt chamber-type press filter to dewater after the homogenizing to advance baking oven static dry to filter cake solid content 65～60%, drying temperature is dried to water ratio below 1% below 105 ℃, and outlet is pulverized, and disintegrating apparatus is an air-flow spiral mill; The 6th goes on foot, and sprays into the silicone grease 295-3 of surface treatment agent desaturation in crushing process by 0.1～1% of powder weight, enters 15M then
3Homogenizer, homogenizing was discharged in 20 minutes, sieve powder packing after vane powder shifter sieve powder packing, detection, mixing homogenizing.
Wherein, synthesizing in synthesis reactor of tensio-active agent finished, and synthesis reactor adopts the steam coils type of heating, and is furnished with whipping appts, the preparation method: inject clear water earlier in still, the ratio of the water yield and active material is 25: 1, and active material is 200
#One-level stearic acid and sodium stearate, stearic consumption are to be 1～3% of lime carbonate total amount in the slurry.The ratio of stearic acid and sodium stearate is 1: 0.3～2.Heat water to 90 ℃ ± 1 ℃ (and remaining to discharge) earlier, drop into sodium stearate and stearic acid successively, and stirred.
Final indicator powder:
Granule-morphology: cubes
Bingham viscosity: 0.45～0.5Pa.s
Yield value: 150～180Pa
The rheology anchor ring is long-pending: greater than 2.0 * 10
4Pa/S
Claims (5)
1, a kind of nano level active calcium carbonate for special use is characterized in that: lime carbonate is cubic granules shape breast, and particle diameter 60～90nm has thixotropic behavior.
2, a kind of preparation method of nano level active calcium carbonate for special use is characterized in that: the first step, CO
2With Ca (OH)
2Carry out building-up reactions, 28 ℃ ± 1 ℃ of temperature; Second step, drop into the crystal growth inhibitor, slurry reaches PH6.7～7.0 and o'clock begins to add thermal aging, low rate carbonization; In the 3rd step, the calcium carbonate slurry after the carbonization adds CO
2High-speed stirring keeps certain hour about 85 ℃; In the 4th step, add synthetic good tensio-active agent; The 5th step, dehydration, drying; In the 6th step, in crushing process, mix a certain amount of surface treatment agent once more, mix sieve powder packing after the homogenizing.
3, the preparation method of nano level active calcium carbonate for special use according to claim 2 is characterized in that: described synthetic good tensio-active agent is to inject clear water earlier in still, and the ratio of the water yield and active material is 25: 1, and active material is 200
#Stearic acid and sodium stearate, stearic consumption are to be 1～3% of lime carbonate total amount in the slurry.The ratio of stearic acid and sodium stearate is 1: 0.3～2, and water temperature is 90 ℃ ± 1 ℃ during reaction, drops into sodium stearate and stearic acid successively, and is stirred.
4, the preparation method of nano level active calcium carbonate for special use according to claim 2 is characterized in that: described crystal growth inhibitor is a sucrose.
5, a kind of purposes of nano level active calcium carbonate for special use is characterized in that: be used for multiple plastisol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02110801 CN1375456A (en) | 2002-02-07 | 2002-02-07 | Nano level active calcium carbonate for special use |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02110801 CN1375456A (en) | 2002-02-07 | 2002-02-07 | Nano level active calcium carbonate for special use |
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| CN1375456A true CN1375456A (en) | 2002-10-23 |
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ID=4741261
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| CN 02110801 Pending CN1375456A (en) | 2002-02-07 | 2002-02-07 | Nano level active calcium carbonate for special use |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006067144A1 (en) | 2004-12-22 | 2006-06-29 | Solvay (Société Anonyme) | Acid resistant particles of an alkaline earth metal carbonate |
| CN1331755C (en) * | 2005-12-29 | 2007-08-15 | 上海耀华纳米科技有限公司 | Process for preparing high thixotropic nano calcium carbonate |
| CN101913640A (en) * | 2010-08-20 | 2010-12-15 | 常州碳酸钙有限公司 | Method for preparing superfine activated calcium carbonate |
| CN102583483A (en) * | 2012-02-22 | 2012-07-18 | 常州碳酸钙有限公司 | Preparation method of micrometer spindle composite nano-calcium carbonate |
| CN102602973A (en) * | 2012-01-13 | 2012-07-25 | 中国中材国际工程股份有限公司 | Method for synthesizing ultrafine calcium carbonate by utilizing carbide slag |
| CN103265059A (en) * | 2013-06-09 | 2013-08-28 | 尤潘垦 | Nano calcium carbonate extruding device |
| CN104098928A (en) * | 2014-03-17 | 2014-10-15 | 福建省万旗非金属材料有限公司 | Preparation method and thixotropy test method of nano calcium carbonate with negative thixotropy |
| CN105329928A (en) * | 2015-12-10 | 2016-02-17 | 湖南化工职业技术学院 | Activation method for nanometer calcium carbonate |
| CN106673043A (en) * | 2017-01-06 | 2017-05-17 | 石家庄学院 | Toughening, anti-ultraviolet and anti-oxidization nano calcium carbonate for filling polyethersulfone resin as well as preparation method and application of toughening, anti-ultraviolet and anti-oxidization nano calcium carbonate |
| CN109399683A (en) * | 2018-12-06 | 2019-03-01 | 东北大学 | A kind of preparation method of PVC automobile bottom gluing surrender enhancing nanometer calcium carbonate |
| 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 |
| CN110643202A (en) * | 2019-08-07 | 2020-01-03 | 宜兴市涂门纳米新材料有限公司 | Special nanometer superfine calcium carbonate for wall |
| CN110817921A (en) * | 2019-10-24 | 2020-02-21 | 湖南金箭新材料科技有限公司 | Nano calcium carbonate aging, homogenizing and surface treatment integrated production process |
-
2002
- 2002-02-07 CN CN 02110801 patent/CN1375456A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1838789B1 (en) | 2004-12-22 | 2021-02-03 | Imertech Sas | Acid resistant particles of an alkaline earth metal carbonate |
| WO2006067144A1 (en) | 2004-12-22 | 2006-06-29 | Solvay (Société Anonyme) | Acid resistant particles of an alkaline earth metal carbonate |
| CN1331755C (en) * | 2005-12-29 | 2007-08-15 | 上海耀华纳米科技有限公司 | Process for preparing high thixotropic nano calcium carbonate |
| CN101913640A (en) * | 2010-08-20 | 2010-12-15 | 常州碳酸钙有限公司 | Method for preparing superfine activated calcium carbonate |
| CN101913640B (en) * | 2010-08-20 | 2012-12-26 | 常州碳酸钙有限公司 | Method for preparing superfine activated calcium carbonate |
| CN102602973A (en) * | 2012-01-13 | 2012-07-25 | 中国中材国际工程股份有限公司 | Method for synthesizing ultrafine calcium carbonate by utilizing carbide slag |
| CN102602973B (en) * | 2012-01-13 | 2014-06-18 | 中国中材国际工程股份有限公司 | Method for synthesizing ultrafine calcium carbonate by utilizing carbide slag |
| CN102583483A (en) * | 2012-02-22 | 2012-07-18 | 常州碳酸钙有限公司 | Preparation method of micrometer spindle composite nano-calcium carbonate |
| CN103265059A (en) * | 2013-06-09 | 2013-08-28 | 尤潘垦 | Nano calcium carbonate extruding device |
| CN104098928A (en) * | 2014-03-17 | 2014-10-15 | 福建省万旗非金属材料有限公司 | Preparation method and thixotropy test method of nano calcium carbonate with negative thixotropy |
| CN104098928B (en) * | 2014-03-17 | 2016-08-17 | 福建省万旗非金属材料有限公司 | The preparation method of a kind of nano-calcium carbonate with negative thixotroping and thixotropy method of testing thereof |
| CN105329928A (en) * | 2015-12-10 | 2016-02-17 | 湖南化工职业技术学院 | Activation method for nanometer calcium carbonate |
| CN106673043A (en) * | 2017-01-06 | 2017-05-17 | 石家庄学院 | Toughening, anti-ultraviolet and anti-oxidization nano calcium carbonate for filling polyethersulfone resin as well as preparation method and application of toughening, anti-ultraviolet and anti-oxidization nano calcium carbonate |
| 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 |
| CN109399683A (en) * | 2018-12-06 | 2019-03-01 | 东北大学 | A kind of preparation method of PVC automobile bottom gluing surrender enhancing nanometer calcium carbonate |
| CN109399683B (en) * | 2018-12-06 | 2020-12-01 | 东北大学 | Preparation method of nano calcium carbonate for yield enhancement of PVC (polyvinyl chloride) automobile primer |
| CN110643202A (en) * | 2019-08-07 | 2020-01-03 | 宜兴市涂门纳米新材料有限公司 | Special nanometer superfine calcium carbonate for wall |
| CN110817921A (en) * | 2019-10-24 | 2020-02-21 | 湖南金箭新材料科技有限公司 | Nano calcium carbonate aging, homogenizing and surface treatment integrated production process |
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