CN105111504A - Modified calcium carbonate with excellent acid resistance and preparation method thereof - Google Patents
Modified calcium carbonate with excellent acid resistance and preparation method thereof Download PDFInfo
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- CN105111504A CN105111504A CN201510515508.XA CN201510515508A CN105111504A CN 105111504 A CN105111504 A CN 105111504A CN 201510515508 A CN201510515508 A CN 201510515508A CN 105111504 A CN105111504 A CN 105111504A
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Abstract
The invention discloses modified calcium carbonate with the excellent acid resistance and a preparation method thereof. The modified calcium carbonate is characterized by comprising, by weight, 100 parts to 150 parts of calcium carbonate, 30 parts to 50 parts of sodium oleate, 0.3 part to 0.7 part of sodium dodecyl benzene sulfonate, 1 part to 3 parts of sodium bicarbonate, 4 parts to 8 parts of styrene, 0.02 part to 0.05 part of potassium persulfate, 3 parts to 5 parts of fumed silica, 2 parts to 3 parts of organobentonite, 2 parts to 3 parts of zirconium tetrafluoride, 1 part to 3 parts of epoxy castor oil, 2 parts to 3 parts of sodium tripolyphosphate, 3 parts to 5 parts of shell powder and a proper amount of deionized water. According to the modified calcium carbonate, as the added zirconium tetrafluoride, the added epoxy castor oil, the added sodium tripolyphosphate and the added shell powder are cooperatively used, the calcium carbonate is good in acid resistance and adsorbability, resistant to bacteria, capable of achieving bacteriostasis, resistant to ultraviolet rays and good in heat resistance and light resistance; the modified calcium carbonate can be crosslinked with film forming matter in rubber, plastics and coatings to generate the good surface decoration effect, the performance of a product can be improved, and the modified calcium carbonate is green, safe and worthy of popularization.
Description
Technical field
The present invention relates to industrial filler field, particularly a kind of modified calcium carbonate and preparation method thereof of acid-proof.
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 modified calcium carbonate of a kind of acid-proof and preparation method thereof.In order to realize object of the present invention, the present invention is by following scheme implementation:
Modified calcium carbonate of a kind of acid-proof 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, zirconium tetrafluoride 2-3, epoxy castor oil 1-3, tripoly phosphate sodium STPP 2-3, oyster shell whiting 3-5, deionized water are appropriate;
Modified calcium carbonate of a kind of acid-proof 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, and the present invention is also by aerosil and organobentonite activation aftertreatment modified calcium carbonate, and make silicon-dioxide stick to the surface of calcium carbonate, not free settling, is uniformly dispersed, and suspension stability is good, and further enhancing the oilness of calcium carbonate, water tolerance and high thermal resistance, make calcium carbonate have a wide range of applications in the industry, the zirconium tetrafluoride of interpolation, epoxy castor oil, between tripoly phosphate sodium STPP and oyster shell whiting with the use of, make calcium carbonate acidproof, excellent adsorption, antibacterial bacteriostatic, uvioresistant, heat-resisting, photostabilization is good, can at rubber, plastics, with filmogen crosslinked action in coating, produce good surface decoration effect, improve the performance of product self, green safety, is worthy to be popularized.
Specific embodiments
Below by specific examples, the present invention is described in detail.
Modified calcium carbonate of a kind of acid-proof and preparation method thereof, is made up of the raw material of following weight part (kilogram): calcium carbonate 150, sodium oleate 46, Sodium dodecylbenzene sulfonate 0.5, sodium bicarbonate 2, vinylbenzene 7, Potassium Persulphate 0.03, aerosil 4, organobentonite 3, zirconium tetrafluoride 2, epoxy castor oil 2, tripoly phosphate sodium STPP 2, oyster shell whiting 4, deionized water are appropriate;
Modified calcium carbonate of a kind of acid-proof 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 4h, 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 50 ° 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 52.4% than unmodified calcium carbonate oil-absorption(number), settling volume reduces 61.3%, viscosity reduces 64.2%, and tap density reduces 18.3%, 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. the modified calcium carbonate and preparation method thereof of an acid-proof, 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, zirconium tetrafluoride 2-3, epoxy castor oil 1-3, tripoly phosphate sodium STPP 2-3, oyster shell whiting 3-5, deionized water are appropriate.
2. the modified calcium carbonate and preparation method thereof of a kind of acid-proof 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107280983A (en) * | 2017-06-27 | 2017-10-24 | 徐剑霞 | A kind of preparation method of modified calcium carbonate used for cosmetic |
| CN107383951A (en) * | 2017-08-04 | 2017-11-24 | 成都硕屋科技有限公司 | The preparation method of hydrophobic dispersion |
| CN107418254A (en) * | 2017-08-04 | 2017-12-01 | 成都硕屋科技有限公司 | A kind of hydrophobic solid powder dispersion and its application |
| CN107445187A (en) * | 2017-06-27 | 2017-12-08 | 徐剑霞 | A kind of preparation method of oyster shell whiting modified calcium carbonate |
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| JP3358833B2 (en) * | 1992-10-12 | 2002-12-24 | 日本化学工業株式会社 | Rust prevention pigment |
| CN104497637A (en) * | 2014-12-16 | 2015-04-08 | 湖北羿廷化工科技有限公司 | Modified calcium carbonate and preparation method thereof |
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2015
- 2015-08-21 CN CN201510515508.XA patent/CN105111504A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3358833B2 (en) * | 1992-10-12 | 2002-12-24 | 日本化学工業株式会社 | Rust prevention pigment |
| CN104497637A (en) * | 2014-12-16 | 2015-04-08 | 湖北羿廷化工科技有限公司 | Modified calcium carbonate and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 盛野: ""功能性纳米碳酸钙复合材料的合成研究"", 《中国优秀硕士学位论文全文数据库（博士）》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107280983A (en) * | 2017-06-27 | 2017-10-24 | 徐剑霞 | A kind of preparation method of modified calcium carbonate used for cosmetic |
| CN107445187A (en) * | 2017-06-27 | 2017-12-08 | 徐剑霞 | A kind of preparation method of oyster shell whiting modified calcium carbonate |
| CN107383951A (en) * | 2017-08-04 | 2017-11-24 | 成都硕屋科技有限公司 | The preparation method of hydrophobic dispersion |
| CN107418254A (en) * | 2017-08-04 | 2017-12-01 | 成都硕屋科技有限公司 | A kind of hydrophobic solid powder dispersion and its application |
| CN107418254B (en) * | 2017-08-04 | 2020-02-14 | 成都硕屋科技有限公司 | Hydrophobic solid powder dispersion material and application thereof |
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