CN108641409A - A kind of precipitated calcium carbonate superfine powdery material and its application in layer/polyaniline conductive film - Google Patents

A kind of precipitated calcium carbonate superfine powdery material and its application in layer/polyaniline conductive film Download PDF

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CN108641409A
CN108641409A CN201810408361.8A CN201810408361A CN108641409A CN 108641409 A CN108641409 A CN 108641409A CN 201810408361 A CN201810408361 A CN 201810408361A CN 108641409 A CN108641409 A CN 108641409A
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calcium carbonate
precipitated calcium
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powdery material
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顾黎明
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Suzhou Zhirui Photoelectric Material Technology Co Ltd
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract

The invention belongs to superfine powdery material preparation fields, and in particular to a kind of precipitated calcium carbonate superfine powdery material and its application in layer/polyaniline conductive film.The powder body material is made by following steps：Take stearic acid, heating fusing, mixes with precipitated calcium carbonate, is added in the deionized water of 60 70 times of mixture weight, ultrasound 5 10 minutes, it mixes, is sent in reaction kettle with compound solution of silane, insulated and stirred, discharging cooling, it centrifuges, drying will be precipitated, up to precipitated calcium carbonate superfine powdery material after grinding.The present invention uses stearic acid to handle precipitated calcium carbonate first, it is acted on by stearic adsorption to improve the reactivity on precipitated calcium carbonate surface, then it is blended with the ethyl alcohol of silane coupling agent decentralized processing, lauryl mercaptan, pass through high temperature esterification, so as to improve dispersion compatibility of the calcium carbonate between organic polymer, the mechanical stability for improving finished films plays fine facilitation effect.

Description

A kind of precipitated calcium carbonate superfine powdery material and its in layer/polyaniline conductive film Using
Technical field
The invention belongs to superfine powdery material preparation fields, and in particular to a kind of precipitated calcium carbonate superfine powdery material and its Application in layer/polyaniline conductive film.
Background technology
Filler of the calcium carbonate as plastic products can improve heat resistance, wearability, dimensional stability, the rigidity of product And machinability, and the cost of product is reduced, but there is the stronger hydroxyl of hydrophily on its surface, and stronger alkalinity is presented, it is this The compatibility of calcium carbonate and organic polymer that hydrophilic and oleophobic property makes is poor, easily forms aggregation, causes inside high polymer Dispersion is uneven, to cause two kinds of storeroom boundary defects, direct application effect bad；In addition, calcium carbonate superfine powder grain size It is small, there is great specific surface area and higher specific surface energy, preparing and particle coagulation, group easily occur in last handling process It is poly-, offspring is formed, so that grain diameter is become larger, loses the function that superfine material has in application process, to influence Actually should effect, functional stuffing cannot be played the role of.Therefore, in order to improve the strengthening action of calcium carbonate and in composite wood The physical property of dispersion performance and modified calcium carbonate filled composite materials in material, it is necessary to using different surface modifiers and Processing method carries out surface modification to calcium carbonate powder, and then widens the application field of calcium carbonate.
Invention content
It is an object of the present invention in view of the drawbacks of the prior art and insufficient, a kind of precipitated calcium carbonate superfine powder is provided Body material.
Another object of the present invention is to provide a kind of precipitated calcium carbonate superfine powdery material in layer/polyaniline conductive film Using.
To realize that said one purpose, the present invention use following technical scheme：
A kind of precipitated calcium carbonate superfine powdery material, the precipitated calcium carbonate superfine powdery material are made by following steps：Take tristearin Acid, heating fusing, mixes with precipitated calcium carbonate, is added in the deionized water of 60-70 times of mixture weight, ultrasonic 5-10 points Clock is mixed with compound solution of silane, is sent in reaction kettle, and control reactor pressure is 0.9-1Mpa, and raising temperature is 90-95 DEG C, insulated and stirred 1-2 hours, discharging cooling centrifuges, will precipitate drying, up to precipitated calcium carbonate superfine powder after grinding Material；
Wherein, the compound solution of silane is made by following steps：Silane coupling agent kh560 is taken, its weight 10-13 is added to In absolute ethyl alcohol again, it is 55-60 DEG C to increase temperature, and lauryl mercaptan is added, and insulated and stirred 4-20 minutes obtains compound silane Solution.
To realize that another above-mentioned purpose, the present invention use following technical scheme：
A kind of application of precipitated calcium carbonate superfine powdery material in layer/polyaniline conductive film, application process are：1）By lightweight Calcium carbonate superfine powder body material is added in polyaniline solutions, is stirred evenly, and tributyl tin trichloride is added, at 80-90 DEG C Insulated and stirred 30-40 minutes is filtered, filter cake is washed, air drying obtains modified polyaniline；2）Modified polyaniline is added to It in wax solvent, stirs evenly, spin-coating film is to get layer/polyaniline conductive film.
Preferably, step 1）Described in polyaniline solutions be made by following steps：It takes tertiary butyl to biphenol, is added to It in the chloroform of 7-10 times of its weight, stirs evenly, dopant is added, it is 10-20 minutes ultrasonic, aniline is added, stirs evenly, is sent into Into reaction kettle, it is passed through nitrogen, it is 65-70 DEG C to adjust temperature of reaction kettle, addition initiator solution, insulated and stirred 4-5 hours, Discharging cooling, obtains polyaniline solutions；Wherein, the initiator solution is to be added to 25-30 times of its weight by initiator In deionized water, stir evenly to obtain the final product；
Step 2）Described in wax solvent be added in solvent by polytetrafluoroethylwax wax, after stirring evenly to obtain the final product；The solvent is body Product is than being 1:The acetone of 5-7 and the mixed solution of dimethylformamide.
Preferably, it counts in parts by weight, each raw material of the present invention is：3-4 parts of stearic acid, 120-140 parts of aniline, initiator 3- 5 parts, 1-2 parts of lauryl mercaptan, 1-2 parts of dopant, 0.3-0.5 parts of tributyl tin trichloride, 170-200 parts of solvent, tertiary fourth Base is to 0.8-1 parts of biphenol, 6-8 parts of precipitated calcium carbonate, 2-3 parts of polytetrafluoroethylwax wax, 0.7-1 parts of silane coupling agent kh560.
Preferably, the one kind of dopant of the present invention in p-methyl benzenesulfonic acid or citric acid.
Preferably, the one kind of initiator of the present invention in ammonium persulfate, potassium peroxydisulfate or sodium peroxydisulfate.
Advantages of the present invention：
The present invention uses stearic acid to handle precipitated calcium carbonate first, is acted on by stearic adsorption to improve lightweight carbonic acid Then the reactivity on calcium surface is blended with the ethyl alcohol of silane coupling agent decentralized processing, lauryl mercaptan, passes through high temperature ester Change, so as to improve dispersion compatibility of the calcium carbonate between organic polymer, the mechanical stability for improving finished films rises Fine facilitation effect is arrived.
The present invention introduces acid doping agent during aniline polymerization, and the conduction that can effectively improve polyaniline finished product is steady It is qualitative, while the tertiary butyl being added can then improve biphenol the bin stability of film, the present invention by adding in a solvent Enter polytetrafluoroethylwax wax, can effectively improve the tensile strength of polyaniline finished films, while promoting compound between each raw material Intensity.
Specific implementation mode
The present invention is further described through with reference to embodiment.
Embodiment 1
1) preparation of compound solution of silane
1 part of silane coupling agent kh560 is taken, is added in the absolute ethyl alcohol of 13 times of its weight, it is 60 DEG C to increase temperature, is added ten 2 parts of dialkyl group mercaptan, insulated and stirred 20 minutes, obtains compound solution of silane.
2）The preparation of precipitated calcium carbonate superfine powdery material
4 parts of stearic acid, heating fusing is taken to be mixed for 8 parts with precipitated calcium carbonate, be added to the deionized water of 70 times of mixture weight In, ultrasound 10 minutes is mixed with above-mentioned compound solution of silane, is sent in reaction kettle, and control reactor pressure is 1Mpa, is increased Temperature is 95 DEG C, insulated and stirred 2 hours, and discharging cooling centrifuges, will precipitate drying, obtain precipitated calcium carbonate superfine powder material Material.
Embodiment 2
1) preparation of compound solution of silane
0.7 part of silane coupling agent kh560 is taken, is added in the absolute ethyl alcohol of 10 times of its weight, it is 55 DEG C to increase temperature, is added 1 part of lauryl mercaptan, insulated and stirred 4 minutes, obtains compound solution of silane；
2）The preparation of precipitated calcium carbonate superfine powdery material
3 parts of stearic acid, heating fusing is taken to be mixed for 6 parts with precipitated calcium carbonate, be added to the deionized water of 60 times of mixture weight In, ultrasound 5 minutes is mixed with above-mentioned compound solution of silane, is sent in reaction kettle, and control reactor pressure is 0.9mpa, is risen High-temperature is 90 DEG C, insulated and stirred 1 hour, and discharging cooling centrifuges, will precipitate drying, obtain precipitated calcium carbonate superfine powder Material.
Embodiment 3
The preparation of layer/polyaniline conductive film：
1）5 parts of sodium peroxydisulfate is taken, is added in the deionized water of 30 times of its weight, is stirred evenly, obtain sodium persulfate aqueous solution；
2）3 parts of polytetrafluoroethylwax wax is taken, is added in 200 parts of solvent, stirs evenly, obtain wax solvent；Wherein solvent is volume ratio It is 1:7 acetone and the mixed solution of dimethylformamide；
3）It takes tertiary butyl to 1 part of biphenol, is added in the chloroform of 10 times of its weight, stirs evenly, p-methyl benzenesulfonic acid 2 is added Part, ultrasound 20 minutes is added 140 parts of aniline, stirs evenly, be sent in reaction kettle, is passed through nitrogen, adjusts temperature of reaction kettle and is 70 DEG C, above-mentioned sodium persulfate aqueous solution, insulated and stirred 5 hours is added, discharging cooling obtains polyaniline solutions；
4）Precipitated calcium carbonate superfine powdery material made from Example 1, is added in above-mentioned polyaniline solutions, stirs evenly, 0.5 part of tributyl tin trichloride is added, insulated and stirred 40 minutes at 90 DEG C filter, filter cake washed, air drying, must be changed Property polyaniline；
5）Above-mentioned modified polyaniline is taken, is added in wax solvent, stirs evenly, spin-coating film is thin to get the layer/polyaniline conductive Film.
Embodiment 4
The preparation of layer/polyaniline conductive film：
1）3 parts of ammonium persulfate is taken, is added in the deionized water of 25 times of its weight, is stirred evenly, obtain ammonium persulfate aqueous solution；
2）2 parts of polytetrafluoroethylwax wax is taken, is added in 170 parts of solvent, stirs evenly, obtain wax solvent；Wherein solvent is volume ratio It is 1:5 acetone and the mixed solution of dimethylformamide；
3）It takes tertiary butyl to 0.8 part of biphenol, is added in the chloroform of 7 times of its weight, stirs evenly, 1 part of citric acid is added, surpass Sound 10 minutes is added 120 parts of aniline, stirs evenly, be sent in reaction kettle, is passed through nitrogen, and it is 65 DEG C to adjust temperature of reaction kettle, Above-mentioned ammonium persulfate aqueous solution, insulated and stirred 4-5 hours is added, discharging cooling obtains polyaniline solutions；
4）Precipitated calcium carbonate superfine powdery material made from Example 2, is added in above-mentioned polyaniline solutions, stirs evenly, Tributyl tin trichloride is added, insulated and stirred 30 minutes at 80 DEG C filter, filter cake washed, air drying obtains modified polyphenyl Amine；
5）Above-mentioned modified polyaniline is taken, is added in wax solvent, stirs evenly, spin-coating film is thin to get the layer/polyaniline conductive Film.
Performance test：
The layer/polyaniline conductive film of embodiment 3：
Thickness 1.6mm；
Tensile strength 10.2Mpa；
Conductivity is tested using four probe method, result 0.80S/cm；
The layer/polyaniline conductive film of embodiment 4：
Thickness 1.7mm；
Tensile strength 11.3Mpa；
Conductivity is tested using four probe method, result 0.86S/cm.

Claims (6)

1. a kind of precipitated calcium carbonate superfine powdery material, it is characterised in that：The precipitated calcium carbonate superfine powdery material by walking as follows It is rapid to be made：Stearic acid, heating fusing is taken to be mixed with precipitated calcium carbonate, be added to the deionized water of 60-70 times of mixture weight In, it is 5-10 minutes ultrasonic, it mixes, is sent in reaction kettle with compound solution of silane, control reactor pressure is 0.9-1Mpa, is risen High-temperature is 90-95 DEG C, insulated and stirred 1-2 hours, and discharging cooling centrifuges, will precipitate drying, up to lightweight carbon after grinding Sour calcium superfine powdery material；
Wherein, the compound solution of silane is made by following steps：Silane coupling agent kh560 is taken, its weight 10-13 is added to In absolute ethyl alcohol again, it is 55-60 DEG C to increase temperature, and lauryl mercaptan is added, and insulated and stirred 4-20 minutes obtains compound silane Solution.
2. a kind of application of precipitated calcium carbonate superfine powdery material as described in claim 1 in layer/polyaniline conductive film, special Sign is：Application process is：1）Precipitated calcium carbonate superfine powdery material is added in polyaniline solutions, is stirred evenly, is added Tributyl tin trichloride is filtered, filter cake is washed, air drying insulated and stirred 30-40 minutes at 80-90 DEG C, must be modified poly- Aniline；2）Modified polyaniline is added in wax solvent, is stirred evenly, spin-coating film is to get layer/polyaniline conductive film.
3. application of a kind of precipitated calcium carbonate superfine powdery material in layer/polyaniline conductive film according to claim 2, It is characterized in that：Step 1）Described in polyaniline solutions be made by following steps：It takes tertiary butyl to biphenol, is added to its weight It in 7-10 times of chloroform, stirs evenly, dopant is added, it is 10-20 minutes ultrasonic, aniline is added, stirs evenly, is sent to reaction In kettle, it is passed through nitrogen, it is 65-70 DEG C to adjust temperature of reaction kettle, and initiator solution is added, and insulated and stirred 4-5 hours discharges cold But, polyaniline solutions are obtained；Wherein, the initiator solution is the deionization that 25-30 times of its weight is added to by initiator In water, stir evenly to obtain the final product；
Step 2）Described in wax solvent be added in solvent by polytetrafluoroethylwax wax, after stirring evenly to obtain the final product；The solvent is body Product is than being 1:The acetone of 5-7 and the mixed solution of dimethylformamide.
4. application of a kind of precipitated calcium carbonate superfine powdery material in layer/polyaniline conductive film according to claim 3, It is characterized in that：It counts in parts by weight, each raw material is：3-4 parts of stearic acid, 120-140 parts of aniline, 3-5 parts of initiator, dodecyl 1-2 parts of mercaptan, 1-2 parts of dopant, 0.3-0.5 parts of tributyl tin trichloride, 170-200 parts of solvent, tertiary butyl are to biphenol 0.8-1 parts, 6-8 parts of precipitated calcium carbonate, 2-3 parts of polytetrafluoroethylwax wax, 0.7-1 parts of silane coupling agent kh560.
5. application of a kind of precipitated calcium carbonate superfine powdery material in layer/polyaniline conductive film according to claim 4, It is characterized in that：The one kind of the dopant in p-methyl benzenesulfonic acid or citric acid.
6. application of a kind of precipitated calcium carbonate superfine powdery material in layer/polyaniline conductive film according to claim 4, It is characterized in that：The one kind of the initiator in ammonium persulfate, potassium peroxydisulfate or sodium peroxydisulfate.
CN201810408361.8A 2018-05-02 2018-05-02 A kind of precipitated calcium carbonate superfine powdery material and its application in layer/polyaniline conductive film Withdrawn CN108641409A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109504130A (en) * 2018-12-19 2019-03-22 安徽省宣城市华纳新材料科技有限公司 A kind of preparation of silane end capped polyurethane sealant nanometer calcium carbonate
WO2019210685A1 (en) * 2018-05-02 2019-11-07 苏州知瑞光电材料科技有限公司 Polyaniline conductive thin film
WO2022133526A1 (en) * 2020-12-21 2022-06-30 Commonwealth Scientific And Industrial Research Organisation Thermally stabilised conductive polymer coatings

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EP3050932A1 (en) * 2015-01-30 2016-08-03 Shin-Etsu Chemical Co., Ltd. Conductive polymer composition, coated article, patterning process, and substrate
CN107118555A (en) * 2017-06-22 2017-09-01 常州大学 The method that solution blended process prepares polyamideimide-based antistatic film
CN107418111A (en) * 2017-08-01 2017-12-01 中国科学技术大学 For strain and/or the preparation method of pressure sensing conductive polymer composite

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Publication number Priority date Publication date Assignee Title
CN102532892A (en) * 2012-01-20 2012-07-04 北京师范大学 Conductive polymer film and preparation method thereof
EP3050932A1 (en) * 2015-01-30 2016-08-03 Shin-Etsu Chemical Co., Ltd. Conductive polymer composition, coated article, patterning process, and substrate
CN107118555A (en) * 2017-06-22 2017-09-01 常州大学 The method that solution blended process prepares polyamideimide-based antistatic film
CN107418111A (en) * 2017-08-01 2017-12-01 中国科学技术大学 For strain and/or the preparation method of pressure sensing conductive polymer composite

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Publication number Priority date Publication date Assignee Title
WO2019210685A1 (en) * 2018-05-02 2019-11-07 苏州知瑞光电材料科技有限公司 Polyaniline conductive thin film
CN109504130A (en) * 2018-12-19 2019-03-22 安徽省宣城市华纳新材料科技有限公司 A kind of preparation of silane end capped polyurethane sealant nanometer calcium carbonate
CN109504130B (en) * 2018-12-19 2021-02-09 安徽省宣城市华纳新材料科技有限公司 Preparation of nano calcium carbonate for silane-terminated polyurethane sealant
WO2022133526A1 (en) * 2020-12-21 2022-06-30 Commonwealth Scientific And Industrial Research Organisation Thermally stabilised conductive polymer coatings

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Application publication date: 20181012