CN104927401A - Modified calcium carbonate and preparation method thereof - Google Patents
Modified calcium carbonate and preparation method thereof Download PDFInfo
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- CN104927401A CN104927401A CN201510302284.4A CN201510302284A CN104927401A CN 104927401 A CN104927401 A CN 104927401A CN 201510302284 A CN201510302284 A CN 201510302284A CN 104927401 A CN104927401 A CN 104927401A
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Abstract
The invention discloses modified calcium carbonate and a preparation method thereof. The modified calcium carbonate is characterized by being prepared from the following raw materials in parts by weight: 100-150 parts of calcium carbonate, 30-50 parts of sodium oleate, 0.3-0.7 part of sodium dodecyl benzene sulfonate, 1-3 parts of sodium bicarbonate, 4-8 parts of styrene, 0.02-0.05 part of potassium persulfate, 3-5 parts of fumed silica, 2-3 parts of organic bentonite, 2-3 parts of polyimide, 0.4-1 part of ammonium bicarbonate, 2-4 parts of high abrasion furnace black and a proper amount of deionized water. The added polyimide, ammonium bicarbonate and high abrasion furnace black are combined with calcium carbonate to enable calcium carbonate to be wear-resistant in surface, lipophilic and hydrophobic, and have the fire-extinguishing property and other properties, the modified calcium carbonate has relatively good compatibility with polymers, and the interface effect is enhanced. The modified calcium carbonate has the advantages of simple modification process, relatively low cost, zero pollution, easy popularization and wide application prospect.
Description
Technical field
The present invention relates to industrial filler field, particularly a kind of modified calcium carbonate and preparation method thereof.
Background technology
calcium carbonate is as rubber, the filler of plastics, the thermotolerance of goods can be improved, wear resistance, dimensional stability, rigidity and workability, and reduce the cost of goods, but the hydroxyl that its surface has wetting ability stronger, present stronger alkalescence, the affinity of the calcium carbonate that this hydrophilic thin oil properties makes and organic polymer is poor, easy formation aggregate, part in superpolymer is caused to disperse uneven, thus cause boundary defect between bi-material, direct effect is bad, and calcium carbonate is as filler, its acid resistance, slickness, the performances such as whiteness need further raising, therefore, in order to improve the physicals of the strengthening action of calcium carbonate and dispersing property in the composite and modified calcium carbonate filled composite materials, be necessary to adopt different surface-modifying agents and treatment process to carry out surface modification to calcium carbonate powders, and then widen the Application Areas of calcium carbonate.
Polymer/inorganic particle matrix material is a kind of type material, which overcome simple inorganic particulate not easily to process, organic polymer intensity is lower, the shortcomings such as less stable, under synergistic effect, can obtain upgrading than inorganic particulate and organic polymer, more excellent performance, improve the stability of composite prod and the dispersiveness in organic phase, the performances such as physical strength, the present invention adopts polymer overmold modified calcium carbonate, solve the hydrophilic oleophobic of carbonic acid carbon, dispersed bad, free settling, physical strength is not high, the problems such as enhancement cannot be reached with polymer compatibility difference, improve the range of application of calcium carbonate.
Summary of the invention
The object of this invention is to provide a kind of modified calcium carbonate and preparation method thereof.In order to realize object of the present invention, the present invention is by following scheme implementation:
A kind of modified calcium carbonate and preparation method thereof, is made up of the raw material of following weight part: calcium carbonate 100-150, sodium oleate 30-50, Sodium dodecylbenzene sulfonate 0.3-0.7, sodium bicarbonate 1-3, vinylbenzene 4-8, Potassium Persulphate 0.02-0.05, aerosil 3-5, organobentonite 2-3, polyimide 2-3, bicarbonate of ammonia 0.4-1, high wear-resistant carbon black 2-4, deionized water are appropriate;
A kind of modified calcium carbonate of the present invention and preparation method thereof, be made up of following concrete steps:
(1) sodium oleate is added the aqueous solution sodium oleate that deionized water dissolving makes 1%, electric stirring 10min raised temperature to 60 ° C, add calcium carbonate and stir 1.5h, stirred suction filtration after rear standing 4-6h, with deionized water wash, dry for standby under 80 ° of C in an oven;
(2) modified calcium carbonate obtained for step (1) is added in the four-necked bottle with driven stirring rod and reflux condensing tube, adding appropriate water stirring makes modified calcium carbonate become slurries, stirring is stopped to add Sodium dodecylbenzene sulfonate and sodium bicarbonate, vinylbenzene is added after stirring 0.5h in a nitrogen atmosphere, persulfate aqueous solution is dripped after mixture being warming up to 80 ° of C, constant temperature is centrifugal after keeping 80 ° of C8h, with dry under 80 ° of C in an oven after deionized water rinsing, after to be ground into 300-400 order for subsequent use;
(3) the methanol solution activation 0.5h of 3-5 times amount is added after organobentonite and aerosil being mixed, 5 μm are less than to particle diameter again at grinding machine for grinding 2-3h, add deionized water ultrasonic disperse more even, transfer in flask the product adding step (2) gained again, raised temperature is to 80-100 ° of C, the ultrasonic methyl alcohol that is back to volatilizees, and dries product;
(4) by remaining mixing of materials, stir when being heated to 40-60 ° of C, then the product adding step (3) gained is under the rotating speed of 1300-1500 rev/min, stirs 8-10min, naturally cool to room temperature after insulation 10-15min, grind to form nanometer powdery.
Advantage of the present invention is: the present invention's sodium oleate makes calcium carbonate surface organise as properties-correcting agent, calcium carbonate particles surface is made to have certain hydrophobicity, and double bond is introduced calcium carbonate surface, using modified calcium carbonate particle as seed, the method of letex polymerization has prepared polystyrene coated caco3 composite particles, enhance the consistency of calcium carbonate and polymkeric substance, and easily disperse, not easily reunite, physical strength is high, the present invention is also by aerosil and organobentonite activation aftertreatment modified calcium carbonate, silicon-dioxide is made to stick to the surface of calcium carbonate, not free settling, be uniformly dispersed, suspension stability is good, and further enhancing the oilness of calcium carbonate, water tolerance and high thermal resistance, calcium carbonate is had a wide range of applications in the industry, the polyimide added, bicarbonate of ammonia and high wear-resistant carbon black and calcium carbonate are formed and combine, make calcium carbonate surface wear-resisting, oleophilic drainage, the characteristics such as fire extinguishing, modified calcium carbonate and polymkeric substance have good consistency, enhance interface interaction, modified technique of the present invention is simple, cost is lower, pollution-free, be easy to promote, have a extensive future.
Specific embodiments
Below by specific examples, the present invention is described in detail.
A kind of modified calcium carbonate and preparation method thereof, is made up of the raw material of following weight part (kilogram): calcium carbonate 150, sodium oleate 47, Sodium dodecylbenzene sulfonate 0.7, sodium bicarbonate 2, vinylbenzene 6, Potassium Persulphate 0.05, aerosil 5, organobentonite 3, polyimide 3, bicarbonate of ammonia 0.8, high wear-resistant carbon black 3, deionized water are appropriate;
A kind of modified calcium carbonate of the present invention and preparation method thereof, be made up of following concrete steps:
(1) sodium oleate is added the aqueous solution sodium oleate that deionized water dissolving makes 1%, electric stirring 10min raised temperature to 60 ° C, add calcium carbonate and stir 1.5h, stirred suction filtration after rear standing 6h, with deionized water wash, dry for standby under 80 ° of C in an oven;
(2) modified calcium carbonate obtained for step (1) is added in the four-necked bottle with driven stirring rod and reflux condensing tube, adding appropriate water stirring makes modified calcium carbonate become slurries, stirring is stopped to add Sodium dodecylbenzene sulfonate and sodium bicarbonate, vinylbenzene is added after stirring 0.5h in a nitrogen atmosphere, persulfate aqueous solution is dripped after mixture being warming up to 80 ° of C, constant temperature is centrifugal after keeping 80 ° of C8h, with dry under 80 ° of C in an oven after deionized water rinsing, after to be ground into 400 orders for subsequent use;
(3) the methanol solution activation 0.5h of 5 times amount is added after organobentonite and aerosil being mixed, 5 μm are less than to particle diameter again at grinding machine for grinding 2h, add deionized water ultrasonic disperse more even, transfer in flask the product adding step (2) gained again, raised temperature to 100 ° C, the ultrasonic methyl alcohol that is back to volatilizees, and dries product;
(4) by remaining mixing of materials, stir when being heated to 60 ° of C, then the product adding step (3) gained is under the rotating speed of 1500 revs/min, stirs 8min, naturally cool to room temperature after insulation 10min, grind to form nanometer powdery.
The modified calcium carbonate produce the present invention and unmodified calcium carbonate performance compare, obtain modified calcium carbonate and reduce 54.7% than unmodified calcium carbonate oil-absorption(number), settling volume reduces 65.8%, viscosity reduces 58.5%, and tap density reduces 14.6%, and modified calcium carbonate oleophilic drainage is described, good with polymer compatibility, and tap density diminishes, illustrate that calcium carbonate dispersing property is good, not easily reunite.
Claims (2)
1. modified calcium carbonate and preparation method thereof, it is characterized in that, be made up of the raw material of following weight part: calcium carbonate 100-150, sodium oleate 30-50, Sodium dodecylbenzene sulfonate 0.3-0.7, sodium bicarbonate 1-3, vinylbenzene 4-8, Potassium Persulphate 0.02-0.05, aerosil 3-5, organobentonite 2-3, polyimide 2-3, bicarbonate of ammonia 0.4-1, high wear-resistant carbon black 2-4, deionized water are appropriate.
2. a kind of modified calcium carbonate and preparation method thereof according to claim 1, is characterized in that, be made up of following concrete steps:
(1) sodium oleate is added the aqueous solution sodium oleate that deionized water dissolving makes 1%, electric stirring 10min raised temperature to 60 ° C, add calcium carbonate and stir 1.5h, stirred suction filtration after rear standing 4-6h, with deionized water wash, dry for standby under 80 ° of C in an oven;
(2) modified calcium carbonate obtained for step (1) is added in the four-necked bottle with driven stirring rod and reflux condensing tube, adding appropriate water stirring makes modified calcium carbonate become slurries, stirring is stopped to add Sodium dodecylbenzene sulfonate and sodium bicarbonate, vinylbenzene is added after stirring 0.5h in a nitrogen atmosphere, persulfate aqueous solution is dripped after mixture being warming up to 80 ° of C, constant temperature is centrifugal after keeping 80 ° of C8h, with dry under 80 ° of C in an oven after deionized water rinsing, after to be ground into 300-400 order for subsequent use;
(3) the methanol solution activation 0.5h of 3-5 times amount is added after organobentonite and aerosil being mixed, 5 μm are less than to particle diameter again at grinding machine for grinding 2-3h, add deionized water ultrasonic disperse more even, transfer in flask the product adding step (2) gained again, raised temperature is to 80-100 ° of C, the ultrasonic methyl alcohol that is back to volatilizees, and dries product;
(4) by remaining mixing of materials, stir when being heated to 40-60 ° of C, then the product adding step (3) gained is under the rotating speed of 1300-1500 rev/min, stirs 8-10min, naturally cool to room temperature after insulation 10-15min, grind to form nanometer powdery.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106221294A (en) * | 2016-08-05 | 2016-12-14 | 中玺新材料（安徽）有限公司 | A kind of insulation composite calcium carbonate and preparation method thereof |
| CN106927494A (en) * | 2017-03-31 | 2017-07-07 | 贵州省化工研究院 | A kind of method that utilization ardealite directly prepares modified calcium carbonate |
| CN113943497A (en) * | 2020-07-17 | 2022-01-18 | 湖南磊鑫新材料科技有限公司 | Modified calcium carbonate and preparation method thereof |
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| CN104031417A (en) * | 2014-05-20 | 2014-09-10 | 凤台精兴生物科技有限公司 | Modified calcium carbonate with heat-isolating heat-insulating effect and preparation method thereof |
| CN104059392A (en) * | 2014-05-27 | 2014-09-24 | 池州凯尔特纳米科技有限公司 | Porous material modified calcium carbonate and preparation method thereof |
| CN104087025A (en) * | 2014-06-06 | 2014-10-08 | 凤台县精华助剂有限公司 | Modified calcium carbonate with enhanced wear resistance and preparing method thereof |
| CN104087027A (en) * | 2014-06-06 | 2014-10-08 | 凤台县精华助剂有限公司 | High-temperature-resistant modified calcium carbonate and preparation method thereof |
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Patent Citations (4)
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| CN104031417A (en) * | 2014-05-20 | 2014-09-10 | 凤台精兴生物科技有限公司 | Modified calcium carbonate with heat-isolating heat-insulating effect and preparation method thereof |
| CN104059392A (en) * | 2014-05-27 | 2014-09-24 | 池州凯尔特纳米科技有限公司 | Porous material modified calcium carbonate and preparation method thereof |
| CN104087025A (en) * | 2014-06-06 | 2014-10-08 | 凤台县精华助剂有限公司 | Modified calcium carbonate with enhanced wear resistance and preparing method thereof |
| CN104087027A (en) * | 2014-06-06 | 2014-10-08 | 凤台县精华助剂有限公司 | High-temperature-resistant modified calcium carbonate and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106221294A (en) * | 2016-08-05 | 2016-12-14 | 中玺新材料（安徽）有限公司 | A kind of insulation composite calcium carbonate and preparation method thereof |
| CN106927494A (en) * | 2017-03-31 | 2017-07-07 | 贵州省化工研究院 | A kind of method that utilization ardealite directly prepares modified calcium carbonate |
| CN113943497A (en) * | 2020-07-17 | 2022-01-18 | 湖南磊鑫新材料科技有限公司 | Modified calcium carbonate and preparation method thereof |
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