CN101733028A - Dispersing method of nano particles in silicone rubber membrane casting solution - Google Patents

Dispersing method of nano particles in silicone rubber membrane casting solution Download PDF

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Publication number
CN101733028A
CN101733028A CN 200910217995 CN200910217995A CN101733028A CN 101733028 A CN101733028 A CN 101733028A CN 200910217995 CN200910217995 CN 200910217995 CN 200910217995 A CN200910217995 A CN 200910217995A CN 101733028 A CN101733028 A CN 101733028A
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Prior art keywords
silicone rubber
casting solution
nano particle
weight portions
nano particles
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CN 200910217995
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Chinese (zh)
Inventor
孙德
马立国
李然
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Changchun University of Technology
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Changchun University of Technology
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Priority to CN 200910217995 priority Critical patent/CN101733028A/en
Publication of CN101733028A publication Critical patent/CN101733028A/en
Pending legal-status Critical Current

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Abstract

The invention provides a rapid dispersing method of nano particles in a silicone rubber membrane casting solution. The method comprises the following steps of: adding a dispersing agent in the silicon rubber membrane casting solution, wherein the dispersing agent is a cross-linking agent for a silicon rubber membrane; and mechanically stirring and pre-dispersing, and then putting into an ultrasonoscope and carrying out ultrasonic dispersion, wherein the rapid dispersion of the nano particles just needs about 20 minutes, the nano particles are evenly dispersed in the membrane casting solution, an added auxiliary agent is an auxiliary agent for silicon rubber membrane formation, and the silicon rubber membrane has no other impurities. In the silicon rubber composite membrane prepared by the dispersing method, the nano particles are in single-particle dispersion by the determination of a scanning electronic microscope, the nano particles are evenly dispersed, and the tensile strength is improved up to 1.828MPa.

Description

The method that nano particle disperses in silicone rubber membrane casting solution
Technical field
The present invention relates to the method that a kind of nano particle disperses in silicone rubber membrane casting solution.
Background technology
Nano material is because particle diameter is little, and specific area is big, and therefore the free energy height exists with aggregating state generally speaking, thereby can not embody the nanoscale effect well.When nano material was used for the matrix material modification, this agglomeration caused nano particle to be difficult to disperse in matrix, has improved the dispersion cost, has increased the consumption of nano material, and modified effect also is difficult to embody.
Silicone rubber membrane is owing to its good hear resistance, cold resistance, thermal conductivity, anti-flammability, chemical stability, close organic matter hydrophobic performance, the difficult separating mixture mesentery that can be widely used in fields such as sealing, insulation, chemical industry, environmental protection, analysis separates, but, often need to add inorganic nano-particle and carry out modification because its mechanical performance is relatively poor.
But methods such as the mechanical agitation of CN200510112112 report, grinding are difficult to realize the quick dispersion of nano particle, generally need more than a few hours, and dispersion effect are also unsatisfactory; CN1332203A adopts ultrasonic wave to disperse to be greatly improved, but jitter time is still very long, needs about 1 hour approximately.
Summary of the invention
The objective of the invention is deficiency, the method that provides a kind of nano particle in silicone rubber membrane casting solution, to disperse at prior art.Be characterized in adding dispersant in nano particle silicon rubber casting solution, this dispersant is silicon rubber film forming crosslinking agent, and is earlier pre-dispersed through mechanical agitation, places then to carry out the ultrasonic wave dispersion in the ultrasonoscope.
The step and the condition of the method that a kind of nano particle disperses in silicone rubber membrane casting solution are as follows:
Take by weighing silicon rubber 10~35 weight portions, nano particle 1~10 weight portion, solvent 50~85 weight portions, dispersant 1~5 weight portion places in the reactor in turn, under the room temperature, carries out mechanical agitation 5~10 minutes at 600~1000 rev/mins; Then, this mixed liquor being placed power again is 500~1000W, and frequency is 2 * 10 6~2 * 10 8In the ultrasonoscope of Hz, ultrasonic 5~10 minutes, obtain the finely dispersed casting solution of nano particle;
Described nano particle is a kind of in carbon black, silica, calcium carbonate and the titanium dioxide;
Described silicon rubber is room temperature vulcanized silicone rubber, a kind of in dimethyl silicone rubber, methyl vinyl silicone rubber and the methyl phenyl vinyl silicone rubber;
Described solvent is a kind of in n-hexane, normal heptane, normal octane, chloroform, carbon tetrachloride and the dichloroethylene;
Described dispersant is a kind of in ethyl orthosilicate, poly-methyl methoxy radical siloxane, VTES, vinyltrimethoxy silane and the γ-chloropropyl triethoxysilane.
The usage of the finely dispersed casting solution of nano particle provided by the invention is as follows: get casting solution 85 weight portions, add the used dispersant of the above-mentioned casting solution of 12 weight portions in turn as crosslinking agent, the dibutyl tin laurate of 3 weight portions can be made film as catalyst.
Beneficial effect: by the composite silicone rubber membrane of process for dispersing preparation of the present invention, measure nano particle through ESEM and be the single particle dispersion, nano particle is uniformly dispersed (as shown in Figure 1), and hot strength can reach 1.828MPa.
The present invention can realize the quick dispersion of nano particle, only needs about 10~20 minutes; Nano particle is uniformly dispersed in casting solution; Institute's adding assistant is a silicon rubber film forming used additives, and made silicone rubber membrane does not have other impurity components.
Description of drawings
Fig. 1 is for adding white carbon composite silicone rubber membrane surface scan electromicroscopic photograph.
The specific embodiment
Embodiment 1
Take by weighing dimethyl silicone rubber 10 weight portions, the silica of 10 weight portion particle diameters, 0.5 nanometer, solvent normal heptane 75 weight portions, dispersant ethyl orthosilicate 5 weight portions place in the reactor, under the room temperature, carry out mechanical agitation 10 minutes at 600 rev/mins; Then, this mixed liquor being placed power again is 1000W, and frequency is 2 * 10 8In the ultrasonoscope of Hz, ultrasonic 7 minutes, can obtain the finely dispersed casting solution of nano particle.
The usage of the finely dispersed casting solution of nano particle that obtains is as follows: get casting solution 85 weight portions, add crosslinking agent ethyl orthosilicate 12 weight portions, catalyst dibutyl tin laurate 3 weight portions in turn, can make film.
Embodiment 2:
Take by weighing methyl vinyl silicone rubber 20 weight portions, the titanium dioxide of 5 weight portion particle diameters, 50 nanometers, solvent chloroform 72 weight portions, dispersant gathers methyl methoxy radical siloxane 3 weight portions, places in the reactor, under the room temperature, carries out mechanical agitation 5 minutes at 800 rev/mins; Then, this mixed liquor being placed power again is 700W, and frequency is 2 * 10 7In the ultrasonoscope of Hz, ultrasonic 10 minutes, can obtain the finely dispersed casting solution of nano particle.
The usage of the finely dispersed casting solution of nano particle that obtains is as follows: get casting solution 85 weight portions, add poly-methyl methoxy radical siloxane 12 weight portions of crosslinking agent, catalyst dibutyl tin laurate 3 weight portions in turn, can make film.
Embodiment 3:
Take by weighing methyl phenyl vinyl silicone rubber 35 weight portions, the calcium carbonate of 1 weight portion particle diameter, 100 nanometers, solvent normal octane 63 weight portions, dispersant VTES 1 weight portion, place in the reactor, under the room temperature, carried out mechanical agitation 7 minutes at 1000 rev/mins; Then, this mixed liquor being placed power again is 500W, and frequency is 2 * 10 6In the ultrasonoscope of Hz, ultrasonic 5 minutes, can obtain the finely dispersed casting solution of nano particle.
The usage of the finely dispersed casting solution of nano particle that obtains is as follows: get casting solution 85 weight portions, add crosslinking agent VTES 12 weight portions, catalyst dibutyl tin laurate 3 weight portions in turn, can make film.
Embodiment 4:
Take by weighing dimethyl silicone rubber 10 weight portions, the carbon black of 2 weight portion particle diameters, 80 nanometers, solvent carbon tetrachloride 85 weight portions, dispersant vinyltrimethoxy silane 3 weight portions place in the reactor, under the room temperature, carry out mechanical agitation 10 minutes at 600 rev/mins; Then, this mixed liquor being placed power again is 1000W, and frequency is 2 * 10 8In the ultrasonoscope of Hz, ultrasonic 7 minutes, can obtain the finely dispersed casting solution of nano particle.
The usage of the finely dispersed casting solution of nano particle that obtains is as follows: get casting solution 85 weight portions, add crosslinking agent vinyltrimethoxy silane 12 weight portions, catalyst dibutyl tin laurate 3 weight portions in turn, can make film.
Embodiment 5:
Take by weighing dimethyl silicone rubber 35 weight portions, the silica of 10 weight portion particle diameters, 50 nanometers, solvent n-hexane 50 weight portions, dispersant γ-chloropropyl triethoxysilane 5 weight portions place in the reactor, under the room temperature, carry out mechanical agitation 10 minutes at 600 rev/mins; Then, this mixed liquor being placed power again is 1000W, and frequency is 2 * 10 8In the ultrasonoscope of Hz, ultrasonic 7 minutes, can obtain the finely dispersed casting solution of nano particle.
The usage of the finely dispersed casting solution of nano particle that obtains is as follows: get casting solution 85 weight portions, add crosslinking agent γ-chloropropyl triethoxysilane 12 weight portions, catalyst dibutyl tin laurate 3 weight portions in turn, can make film.
Embodiment 6:
Replace normal heptane among the embodiment 1 with dichloroethylene, all the other are with embodiment 1.

Claims (1)

1. the step and the condition of nano particle process for dispersing in silicone rubber membrane casting solution are as follows:
Take by weighing silicon rubber 10~35 weight portions, nano particle 1~10 weight portion, solvent 50~85 weight portions, dispersant 1~5 weight portion places in the reactor in turn, under the room temperature, carries out mechanical agitation 5~10 minutes at 600~1000 rev/mins; Then, this mixed liquor being placed power again is 500~1000W, and frequency is 2 * 10 6~2 * 10 8In the ultrasonoscope of Hz, ultrasonic 5~10 minutes, obtain the finely dispersed casting solution of nano particle;
Described nano particle is a kind of in carbon black, silica, calcium carbonate and the titanium dioxide;
Described silicon rubber is room temperature vulcanized silicone rubber, a kind of in dimethyl silicone rubber, methyl vinyl silicone rubber and the methyl phenyl vinyl silicone rubber;
Described solvent is a kind of in n-hexane, normal heptane, normal octane, chloroform, carbon tetrachloride and the dichloroethylene;
Described dispersant is a kind of in ethyl orthosilicate, poly-methyl methoxy radical siloxane, VTES, vinyltrimethoxy silane and the γ-chloropropyl triethoxysilane.
CN 200910217995 2009-12-14 2009-12-14 Dispersing method of nano particles in silicone rubber membrane casting solution Pending CN101733028A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103464006A (en) * 2013-09-06 2013-12-25 长春工业大学 Preparation of PDMS/PVDF (polydimethylsiloxane/polyvinylidene fluoride) blended microporous film
CN104084059A (en) * 2014-07-28 2014-10-08 陈雄 Preparation method for hydrophobic modified nano-calcium carbonate filled silicone rubber composite membrane
CN106731906A (en) * 2015-11-20 2017-05-31 中国石油化工股份有限公司 A kind of preparation method of nanometer particle-modified composite silicone rubber membrane
EP3258750A1 (en) * 2016-06-17 2017-12-20 Nano Shield Technology Co., Ltd. Method for coating a device and devices having nanofilm thereon
CN108525514A (en) * 2018-04-19 2018-09-14 南京信息工程大学 A kind of sulfur resistive water resistant dedusting denitration demercuration multifunctional filter material and preparation method thereof
US10271435B2 (en) 2016-06-17 2019-04-23 Nanoshield Technology Co., Ltd. Method for coating devices and resulting products

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103464006A (en) * 2013-09-06 2013-12-25 长春工业大学 Preparation of PDMS/PVDF (polydimethylsiloxane/polyvinylidene fluoride) blended microporous film
CN104084059A (en) * 2014-07-28 2014-10-08 陈雄 Preparation method for hydrophobic modified nano-calcium carbonate filled silicone rubber composite membrane
CN104084059B (en) * 2014-07-28 2016-08-24 陈雄 A kind of preparation method of hydrophobically modified nanon calcium carbonatefilled composite silicone rubber membrane
CN106731906A (en) * 2015-11-20 2017-05-31 中国石油化工股份有限公司 A kind of preparation method of nanometer particle-modified composite silicone rubber membrane
CN106731906B (en) * 2015-11-20 2019-08-06 中国石油化工股份有限公司 A kind of preparation method of nanometer particle-modified composite silicone rubber membrane
EP3258750A1 (en) * 2016-06-17 2017-12-20 Nano Shield Technology Co., Ltd. Method for coating a device and devices having nanofilm thereon
CN107520105A (en) * 2016-06-17 2017-12-29 盔甲奈米科技股份有限公司 A kind of nano-solution, on device formed nano coating method and with nano coating device
US10271435B2 (en) 2016-06-17 2019-04-23 Nanoshield Technology Co., Ltd. Method for coating devices and resulting products
US10327338B2 (en) 2016-06-17 2019-06-18 Nanoshield Technology Co., Ltd. Method for coating a device and devices having nanofilm thereon
CN107520105B (en) * 2016-06-17 2020-05-19 盔甲奈米科技股份有限公司 Nano-solution, method for forming nano-coating on device and device with nano-coating
CN108525514A (en) * 2018-04-19 2018-09-14 南京信息工程大学 A kind of sulfur resistive water resistant dedusting denitration demercuration multifunctional filter material and preparation method thereof
CN108525514B (en) * 2018-04-19 2021-03-30 南京信息工程大学 Multifunctional filter material with sulfur resistance, water resistance, dust removal, denitration and demercuration functions and preparation method thereof

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Application publication date: 20100616