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CN1663992A - Method for preparing nano calcium carbonate/rubber composite materials - Google Patents

Method for preparing nano calcium carbonate/rubber composite materials Download PDF

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Publication number
CN1663992A
CN1663992A CN 200410097543 CN200410097543A CN1663992A CN 1663992 A CN1663992 A CN 1663992A CN 200410097543 CN200410097543 CN 200410097543 CN 200410097543 A CN200410097543 A CN 200410097543A CN 1663992 A CN1663992 A CN 1663992A
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China
Prior art keywords
calcium carbonate
composite materials
nano calcium
rubber
rubber composite
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Granted
Application number
CN 200410097543
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Chinese (zh)
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CN100343326C (en
Inventor
符新
王江
赵同建
符世泰
孙玉清
钟明霞
王大辉
符胥
曾海青
王琴
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Hainan Huatai Creation Research Institute Of Science And Technology
SOUTH-CHINA PROPICAL AGRICULTURAL UNIV
Original Assignee
Hainan Huatai Creation Research Institute Of Science And Technology
SOUTH-CHINA PROPICAL AGRICULTURAL UNIV
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Application filed by Hainan Huatai Creation Research Institute Of Science And Technology, SOUTH-CHINA PROPICAL AGRICULTURAL UNIV filed Critical Hainan Huatai Creation Research Institute Of Science And Technology
Priority to CNB2004100975436A priority Critical patent/CN100343326C/en
Publication of CN1663992A publication Critical patent/CN1663992A/en
Application granted granted Critical
Publication of CN100343326C publication Critical patent/CN100343326C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

The invention discloses a method for preparing nanocalcium carbonate /rubber composite material, which takes calcium oxide, carbon dioxide and rubber latex as main stock, combining the preparing technology for nanocalcium carbonate and rubber together. The method comprises preparing the calcium hydroxide from calcium oxide, then adding carbon dioxide for charring and getting suspending liquid, then mixing the suspending liquid with rubber latex, through coprecipitation/coagulate, dehydration, drying etc getting the nanocalcium carbonate /rubber composite material.The method is characterized by the simple preparing process and the low production cost, the high performance because of the high degree of scatter of the the flying-off loss and nanocalcium carbonate and the decrease of the environmental pollution.

Description

A kind of preparation method of nano calcium carbonate/rubber composite materials
Technical field
The present invention relates to a kind of preparation method of nano calcium carbonate/rubber composite materials.
Background technology
Existing nanometer CaCO 3The preparation method of/rubber composite adopts completion method, wherein is divided into compounding filled method and emulsion and fills coprecipitation method.The former is with nanometer CaCO on rubber mixing machine 3Prepare with the solid rubber blend; The latter is with nanometer CaCO 3Add latex and mix, prepare through processes such as coprecipitated, dryings.Adopt completion method to prepare nanometer CaCO 3/ rubber composite, nanometer CaCO 3Degree of scatter in rubber matrix is relatively poor, and the performance of material is lower, employed nanometer CaCO 3Powder all will be handled through preventing to focus on again with stability, moreover the latex coprecipitation method also will make nanometer CaCO 3Again dry for the second time, cause the preparation cost of matrix material higher.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of nano calcium carbonate/rubber composite materials, it can organically combine the preparation technology of nano-calcium carbonate and the preparation technology of rubber (dried glue).
The preparation method of the nano calcium carbonate/rubber composite materials that the present invention is designed is: earlier CaO is made Ca (OH) 2Emulsion then adds CO 2Carry out charing, can be prepared into nanometer CaCO 3Suspension; With rubber latex and nanometer CaCO 3Suspension mixes mutually, passes through coprecipitated or solidify to be separated into nanometer CaCO 3Rubber lump or wet micelle; Grumeleuse through slaking, dehydration, compressing tablet or granulation, drying, can be obtained nano calcium carbonate/rubber composite materials; The micelle convection drying that maybe will wet obtains nano calcium carbonate/rubber composite materials.
Preparation method's technology of nano calcium carbonate/rubber composite materials provided by the present invention is simple, and cost is low, because nanometer CaCO 3Degree of scatter in rubber matrix is higher, and prepared performance of composites is better, and has reduced nanometer CaCO 3Fly upward loss and mixing energy expenditure, reduction is to the pollution of environment.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
1,, makes Ca (OH) after filtration after the removal of impurities with CaO slaking wet-milling 2Emulsion at the crystal control agent and the dispersion agent that do not add or add below 5%, to prevent crystallization and to increase degree of scatter, then adds CO 2Carry out charing, carbonization temperature is 5 ℃-40 ℃, does not add or add the properties-correcting agent below 10% then, and preparation concentration is the nanometer CaCO of 2-70% 3Suspension, nanometer CaCO 3Particle dia is 40-90nm.Described crystal control agent is meant a kind of in sodium polyphosphate, zinc sulfate, aluminum chloride, the sodium-chlor; Described dispersion agent is meant disodium EDTA; Described properties-correcting agent is meant a kind of in hard acid ester salt, dodecane sulfonate, titanium, silicon, the aluminium.
2, with concentration be rubber latex and the nanometer CaCO of 5-60% 3Suspension mixes mutually, and stirs, and adds the thickening material below 10% when concentration is low, passes through or solidify being separated into nanometer CaCO then coprecipitated 3Rubber lump or wet micelle.Described rubber latex is meant a kind of of natural rubber latex, styrene-butadiene latex, nitrile rubber, polychloroprene latex, cis-butadiene cement breast, ethylene propylene rubber latex, acrylate adhesive Ruzhong and their mixture; Described thickening material is meant a kind of in polyacrylamide, polyvinyl alcohol, gum arabic, starch, a polyvalent salt; Described method of solidifying is meant a kind of in natural coagulation, biological coagulation, auxiliary biological coagulation, the salt rapid solidification.
3,,,, can obtain nano calcium carbonate/rubber composite materials through compressing tablet or granulating working procedure, drying process again with the ironed dehydration of grumeleuse with gained grumeleuse slaking 0-16h; Or with the wet micelle convection drying of gained, drying temperature is 60-150 ℃, can obtain nano calcium carbonate/rubber composite materials.
Embodiment 1
After the digestion of CaO water,, be made into 5%Ca (OH) through wet-milling, filtering and impurity removing 2Emulsion under stirring action, adds Ca (OH) 20.15% sodium polyphosphate of quality and 0.2% disodium ethylene diamine tetraacetate are adding CO 2Carry out charing, carbonization temperature is 20 ℃, obtains unmodified nanometer CaCO 3Suspension, and then add nanometer CaCO 32% sodium laurylsulfonate of quality carries out the wet method surface modification, obtains nanometer CaCO 3Suspension; Get concentration and be 30% fresh natural rubber latex, under stirring action, join nanometer CaCO 3In the suspension, add polyacrylamide again and mix, then add sucrose and solidify,, can obtain nanometer CaCO 100 ℃ of following dryings with the grumeleuse dehydration 3/ NR matrix material.
Embodiment 2
Press the prepared nanometer CaCO of embodiment 1 3Suspension is got concentration and is 30% styrene-butadiene latex, joins nanometer CaCO under stirring action 3In the suspension, add polyacrylamide again and mix, then add potassium alum and solidify,, can obtain nano-calcium carbonate/styrene-butadiene rubber composite material 100 ℃ of following dryings with the grumeleuse dehydration.

Claims (9)

1, a kind of preparation method of nano calcium carbonate/rubber composite materials is characterized in that: with CaO slaking wet-milling, make Ca (OH) after filtration after the removal of impurities 2Emulsion behind the crystal control agent and dispersion agent that do not add or add below 5%, then adds CO 2Carry out charing, do not add or add the properties-correcting agent below 10% then, preparation concentration is the nanometer CaCO of 2-70% 3Suspension, nanometer CaCO 3Particle dia is 40-90nm; With concentration is rubber latex and the nanometer CaCO of 5-60% 3Suspension mixes mutually, and stirs, and adds the thickening material below 10% when concentration is low, passes through or solidify being separated into nanometer CaCO then coprecipitated 3Rubber lump or wet micelle; With gained grumeleuse slaking 0-16h,,, can obtain nano calcium carbonate/rubber composite materials through compressing tablet or granulating working procedure, drying process again with the ironed dehydration of grumeleuse; Or, can obtain nano calcium carbonate/rubber composite materials with the wet micelle convection drying of gained.
2, according to the preparation method of the said nano calcium carbonate/rubber composite materials of claim 1, it is characterized in that: described crystal control agent is meant a kind of in sodium polyphosphate, zinc sulfate, aluminum chloride, the sodium-chlor.
3, according to the preparation method of the said nano calcium carbonate/rubber composite materials of claim 1, it is characterized in that: described dispersion agent is meant disodium EDTA.
4, according to the preparation method of the said nano calcium carbonate/rubber composite materials of claim 1, it is characterized in that: described carbonization temperature is 5 ℃-40 ℃.
5, according to the preparation method of the said nano calcium carbonate/rubber composite materials of claim 1, it is characterized in that: described properties-correcting agent is meant a kind of in hard acid ester salt, dodecane sulfonate, titanium, silicon, the aluminium.
6, according to the preparation method of the said nano calcium carbonate/rubber composite materials of claim 1, it is characterized in that: described rubber latex is meant a kind of of natural rubber latex, styrene-butadiene latex, nitrile rubber, polychloroprene latex, cis-butadiene cement breast, ethylene propylene rubber latex, acrylate adhesive Ruzhong and their mixture.
7, according to the preparation method of the said nano calcium carbonate/rubber composite materials of claim 1, it is characterized in that: described thickening material is meant a kind of in polyacrylamide, polyvinyl alcohol, gum arabic, starch, a polyvalent salt.
8, according to the preparation method of the said nano calcium carbonate/rubber composite materials of claim 1, it is characterized in that: described method of solidifying is meant a kind of in natural coagulation, biological coagulation, auxiliary biological coagulation, the salt rapid solidification.
9, according to the preparation method of the said nano calcium carbonate/rubber composite materials of claim 1, it is characterized in that: described drying temperature with the wet micelle convection drying of gained is 60-150 ℃.
CNB2004100975436A 2004-11-26 2004-11-26 Method for preparing nano calcium carbonate/rubber composite materials Expired - Fee Related CN100343326C (en)

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CN100343326C CN100343326C (en) 2007-10-17

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101456961B (en) * 2009-01-07 2011-01-19 中国热带农业科学院农产品加工研究所 Method for preparing reactive nano calcium carbonate-native rubber composite material
CN102321281A (en) * 2011-08-09 2012-01-18 上海华明高技术(集团)有限公司 Composition of calcium carbonate and organic elastomer and preparation method thereof
CN103059356A (en) * 2012-12-31 2013-04-24 安徽省佳宝玩具(集团)有限公司 Latex and plush combined toy and production process thereof
CN108794810A (en) * 2018-06-29 2018-11-13 钦州市宝业坭兴陶厂 A kind of method of modifying of nano-calcium carbonate and its application in Reinforced PVC tubing
CN110817922A (en) * 2019-12-11 2020-02-21 合肥工业大学 Inorganic/organic composite inducer and application thereof in induced synthesis of nano calcium carbonate

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1211286C (en) * 2001-08-03 2005-07-20 上海华明高技术(集团)有限公司 Industrial process for preparing nm-class active calcium carbonate
CN1188460C (en) * 2002-06-03 2005-02-09 骆天荣 Granular nano material as rubber stuffing and its prepn

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101456961B (en) * 2009-01-07 2011-01-19 中国热带农业科学院农产品加工研究所 Method for preparing reactive nano calcium carbonate-native rubber composite material
CN102321281A (en) * 2011-08-09 2012-01-18 上海华明高技术(集团)有限公司 Composition of calcium carbonate and organic elastomer and preparation method thereof
CN103059356A (en) * 2012-12-31 2013-04-24 安徽省佳宝玩具(集团)有限公司 Latex and plush combined toy and production process thereof
CN108794810A (en) * 2018-06-29 2018-11-13 钦州市宝业坭兴陶厂 A kind of method of modifying of nano-calcium carbonate and its application in Reinforced PVC tubing
CN110817922A (en) * 2019-12-11 2020-02-21 合肥工业大学 Inorganic/organic composite inducer and application thereof in induced synthesis of nano calcium carbonate
CN110817922B (en) * 2019-12-11 2021-06-29 合肥工业大学 Inorganic/organic composite inducer and application thereof in induced synthesis of nano calcium carbonate

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Granted publication date: 20071017

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