CN1358803A - Method for surface modifying inorganic particle - Google Patents

Method for surface modifying inorganic particle Download PDF

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Publication number
CN1358803A
CN1358803A CN 00132081 CN00132081A CN1358803A CN 1358803 A CN1358803 A CN 1358803A CN 00132081 CN00132081 CN 00132081 CN 00132081 A CN00132081 A CN 00132081A CN 1358803 A CN1358803 A CN 1358803A
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inorganic particle
inorganic particulate
inorganic
particle
solvent
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CN 00132081
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CN1210353C (en
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何光健
雷景新
李启满
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Sichuan University
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Sichuan University
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Abstract

The inorganic particle surface modification method is characterized by that using solvent to dissolve and dilute the monomers which can be polymerized, then stirring to make them uniformly distribute in inorganic particle dsurface, grain size of inorganic particle is 0.1-10 micrometer, then making solvent completely volatilize at 50-150 deg.C, making the inorganic particle undergo the process of UV light radiation at 0-150 deg.c (light intensity is 300-1000 w. wavelength is 280-400 nm) to initiate monomers to make polymerization reaction for 10-120 min., making polymer tightly combine with inorganic particle in grafting or settling mode. The inorganic particle whose surface is covered with a layer of polymer can be used for filling polymer matrix, can obviously improve compatibility of two-phase interface, and can raise the performance of composite material.

Description

The method of surface modifying inorganic particle
The present invention relates to a kind of method of surface modifying inorganic particle.The modified inorganic particle is used for the filled polymer matrix, can obviously improve the consistency of inorganic particulate and polymkeric substance, and obtained performance is matrix material preferably.
Inorganic particulate is widely used in the weighting agent or the toughener of macromolecular material, not only can reduce cost significantly, and can give the performance of the various preciousnesses of material, for Application Areas that enlarges macromolecular material and reduction material cost big meaning is arranged.Yet because the chemical constitution and the configuration of surface structure of inorganic particulate and organic polymer exist great difference, must to inorganic particulate carry out that surface modification can be improved and polymkeric substance between consistency.The surface modification of inorganic particulate adopts the surface of coupling agent treatment particle more, and coupling agent commonly used has silane, metatitanic acid fat, organic chromium and zirconium class coupling agent, and the use range of wherein preceding two kinds of coupling agents is the widest.The processing mode of coupling agent treatment inorganic particulate has two kinds: a kind of is method for pretreating; Another kind is the integral blend method.Method for pretreating is with solvent coupling agent to be diluted earlier, make it to be uniformly distributed in the inorganic particulate surface by stirring at a certain temperature then, because the effect of heating, solvent is volatilized, chemical reaction takes place in coupling agent and inorganic particulate surface, thereby reaches the effect that covers the inorganic particulate surface; The integral blend method is that coupling agent is incorporated in inorganic particulate filler and the resin matrix, the mixing together link coupled effect that reaches.Adopt the coupling agent treatment inorganic filler surface, mature technical route, and obtained using widely.Yet the coupling agent treatment mode is strict to treating processes, needs CONTROL PROCESS condition such as temperature, solvent and mixing time etc. comparatively complicated, and is empirical strong, must grope rule in practice gradually.
The objective of the invention is to provide a kind of method of surface modifying inorganic particle at the deficiencies in the prior art, be characterized in polymerisable monomer is dissolved in the solvent, make it to be evenly distributed on the inorganic particulate surface by stirring, the reaction of employing uv-light polymerization, polymkeric substance is combined closely with grafting or sedimentary mode and inorganic particulate, reaches the effect of modification.
Purpose of the present invention is realized by following technical measures.
The method of surface modifying inorganic particle
1, with 100 parts of polymerisable monomers, behind solvent 500-1500 part dissolved dilution, make it to be evenly distributed on the inorganic particulate surface by stirring, inorganic particulate particle diameter 0.1-10 μ m volatilizees solvent in temperature 50-150 ℃ fully.
2, carry out ultraviolet light irradiation through above-mentioned surface-treated inorganic particulate in temperature 0-150 ℃, power is 300-1000 watt, wavelength 280-400nm, and trigger monomer polyreaction 5-120 minute, polymkeric substance is combined closely with grafting or sedimentary mode and inorganic particulate.
3, inorganic particulate 5-40 part of surface parcel one layer of polymeric is used for filled polymer matrix 95-60 part, improves performance of composites significantly.
Polymerisable monomer is that acrylamide, vinylformic acid, maleic anhydride, vinyl cyanide are or/and vinylbenzene is at least a.
Solvent is that water, acetone, ethanol, methyl alcohol are or/and tetrahydrofuran (THF) is at least a.
Inorganic particulate is that lime carbonate, talcum powder, kaolin, mica powder, potter's clay are or/and aluminium hydroxide is at least a.
Polymeric matrix is that nylon 6, nylon 66, polyethylene, polypropylene, polyvinyl chloride, polystyrene are or/and polycarbonate is at least a.
The present invention compares with the coupling agent treatment mode, and it is simple to have technological process, and easy control of process conditions can easier realize serialization.Simultaneously, the present invention also can freely select different monomer modified inorganic particulates at different macromolecule matrixes, and handiness is big, better effects if.
Embodiment
Below by embodiment the present invention is carried out concrete description, be necessary to be pointed out that at this following examples only are used for the present invention is further specified, can not be interpreted as limiting the scope of the invention.The person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
1, with acrylamide 1.5g, be dissolved in 25 milliliters of acetone, after treating to dissolve fully, add in the 100g calcium carbonate particles calcium carbonate particles particle diameter 1.2 μ m.Start stirrer, calcium carbonate particles stirred 10-20 minute, make it uniform distribution after, in 60 ℃ of temperature oven dry 30 minutes, acetone is volatilized fully.Again the calcium carbonate particles of handling well is placed under the UV-light (500 watts of light intensity, wavelength 365nm) 70 ℃ of temperature and carry out irradiation, 120 minutes time, obtain the calcium carbonate particles modified product.
2, with the 1.5g vinyl cyanide, be dissolved in 25 milliliters of ethanol, after treating to dissolve fully, pour in the 100g kaolin particle, particle diameter is 4.9 μ m, starts stirrer, and the kaolin particle was stirred 10-20 minute, after making it uniform distribution,, ethanol is volatilized fully in 90 ℃ of oven dry of temperature 30 minutes.Again the above-mentioned kaolin particle of handling well is placed under the UV-light (500 watts of light intensity, wavelength 365nm) 70 ℃ of temperature and carry out irradiation, 120 minutes time, obtain the particle modified product of kaolin.
3, with 1g maleic anhydride and 1g vinylbenzene, be dissolved in jointly in 25 milliliters of acetone, after treating to dissolve fully, to pour in the 100g talcum powder particle, the talcum powder particle diameter is 0.19 μ m.Start stirrer, the talcum powder particle stirred 10-20 minute, make it uniform distribution after, in 60 ℃ of oven dry of temperature 30 minutes, acetone is volatilized fully.Again the above-mentioned talcum powder of handling well is placed under the UV-light (500 watts of light intensity, wavelength 365nm) at 70 ℃ and carry out irradiation, 120 minutes time.Obtain talcum powder improving particle surface product.
4, the method for surface modifying inorganic particle provided by the invention adopts acrylamide to handle behind the calcium carbonate particles and filled nylon-6, and its mechanical property is detailed to be shown in Table 1.Experimental result shows, the matrix material of filled nylon-6, and its shock strength is significantly improved, and tensile strength remains unchanged.
The mechanical property of the calcium carbonate-filled nylon 6 of table 1 *
AAM content in the lime carbonate, % Shock strength kJ/m 2 Tensile strength MPa Tensile modulus MPa Elongation %
????0 ????8.80 ????84.2 ????3972 ????4
????0.5 ????8.94 ????80.2 ????4417 ????3
????1 ????10.61 ????84.4 ????3871 ????9
????1.5 ????11.60 ????86.0 ????4043 ????7
????2 ????9.78 ????83.1 ????4197 ????5
????5 ????8.36 ????85.1 ????3741 ????7
*Calcium carbonate content is 16% in the nylon 6

Claims (5)

1, the method of inorganic particulate surface surface modification, it is characterized in that: a, with 100 parts of polymerisable monomers, behind solvent 500-1500 part dissolved dilution, make it to be evenly distributed on the inorganic particulate surface by stirring action, inorganic particulate particle diameter 0.1-10 μ m, in temperature 50-150 ℃ solvent is volatilized fully, b, pass through ultraviolet light irradiation through above-mentioned surface-treated inorganic particulate for 0~150 ℃ in temperature, 300~1000 watts of light intensity, wavelength 280-400nm, trigger monomer polyreaction 10-120 minute, polymkeric substance is combined closely with grafting or sedimentary mode and inorganic particulate, c, inorganic particulate 5-40 part of surface parcel one layer of polymeric is used for filled polymer matrix 95-60 part, improves performance of composites significantly.
2,, it is characterized in that polymerisable monomer is that acrylamide, vinylformic acid, maleic anhydride, vinylbenzene are or/and vinyl cyanide is at least a according to the method for the described surface modifying inorganic particle of claim 1.
3,, it is characterized in that solvent is that water, acetone, ethanol, methyl alcohol are or/and tetrahydrofuran (THF) is at least a according to the method for the described surface modifying inorganic particle of claim 1.
4,, it is characterized in that inorganic particulate is that lime carbonate, talcum powder, kaolin, mica powder, potter's clay are or/and aluminium hydroxide is at least a according to the method for the described surface modifying inorganic particle of claim 1.
5,, it is characterized in that polymeric matrix is that nylon 6, nylon 66, polyethylene, polypropylene, polyvinyl chloride, polystyrene are or/and polycarbonate is at least a according to the method for the described surface modifying inorganic particle of claim 1.
CN 00132081 2000-12-15 2000-12-15 Method for surface modifying inorganic particle Expired - Fee Related CN1210353C (en)

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Application Number Priority Date Filing Date Title
CN 00132081 CN1210353C (en) 2000-12-15 2000-12-15 Method for surface modifying inorganic particle

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CN1210353C CN1210353C (en) 2005-07-13

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1322200C (en) * 2005-06-20 2007-06-20 上海东升新材料有限公司 Preparation method of modified extrafine talc powder used as paper making filler and paint
CN100412126C (en) * 2006-09-05 2008-08-20 武汉理工大学 Composite material of similar fluid inorganic nano particle and polymer and preparation thereof
CN102585567A (en) * 2012-01-05 2012-07-18 四川大学 Method for preparing ultrafine inorganic powder dispersion
CN103275482A (en) * 2013-05-21 2013-09-04 苏州旭光聚合物有限公司 PP (Propene Polymer)/PA (Polyamide) composite material
US20150331315A1 (en) * 2013-11-08 2015-11-19 Boe Technology Group Co., Ltd. Functional material and preparation method thereof, display structure forming material, color film substrate, display device
CN106674596A (en) * 2016-11-16 2017-05-17 新疆维吾尔自治区产品质量监督检验研究院 Method for modifying surface of magnesium hydroxide flame retardant
CN107286307A (en) * 2017-07-28 2017-10-24 中广核达胜加速器技术有限公司 A kind of preparation method of polymeric adsorbent base material
CN108795106A (en) * 2018-06-21 2018-11-13 安徽雪城超细碳酸钙有限公司 A kind of activated earth and preparation method thereof
CN110272642A (en) * 2019-06-18 2019-09-24 武汉工程大学 A kind of chelated surface method of modifying of inorganic particulate

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1322200C (en) * 2005-06-20 2007-06-20 上海东升新材料有限公司 Preparation method of modified extrafine talc powder used as paper making filler and paint
CN100412126C (en) * 2006-09-05 2008-08-20 武汉理工大学 Composite material of similar fluid inorganic nano particle and polymer and preparation thereof
CN102585567A (en) * 2012-01-05 2012-07-18 四川大学 Method for preparing ultrafine inorganic powder dispersion
CN103275482A (en) * 2013-05-21 2013-09-04 苏州旭光聚合物有限公司 PP (Propene Polymer)/PA (Polyamide) composite material
US20150331315A1 (en) * 2013-11-08 2015-11-19 Boe Technology Group Co., Ltd. Functional material and preparation method thereof, display structure forming material, color film substrate, display device
US9598308B2 (en) * 2013-11-08 2017-03-21 Boe Technology Group Co., Ltd. Functional material and preparation method thereof, display structure forming material, color film substrate, display device
CN106674596A (en) * 2016-11-16 2017-05-17 新疆维吾尔自治区产品质量监督检验研究院 Method for modifying surface of magnesium hydroxide flame retardant
CN107286307A (en) * 2017-07-28 2017-10-24 中广核达胜加速器技术有限公司 A kind of preparation method of polymeric adsorbent base material
CN107286307B (en) * 2017-07-28 2019-10-22 中广核达胜加速器技术有限公司 A kind of preparation method for adsorbing resin base material
CN108795106A (en) * 2018-06-21 2018-11-13 安徽雪城超细碳酸钙有限公司 A kind of activated earth and preparation method thereof
CN110272642A (en) * 2019-06-18 2019-09-24 武汉工程大学 A kind of chelated surface method of modifying of inorganic particulate

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