CN105176092A - Preparation method for epoxy resin compound organic silicon thermal-insulation material - Google Patents

Preparation method for epoxy resin compound organic silicon thermal-insulation material Download PDF

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Publication number
CN105176092A
CN105176092A CN201510704834.5A CN201510704834A CN105176092A CN 105176092 A CN105176092 A CN 105176092A CN 201510704834 A CN201510704834 A CN 201510704834A CN 105176092 A CN105176092 A CN 105176092A
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epoxy resin
preparation
silicone oil
mixing
agent
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CN105176092B (en
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张世钦
吕树申
张锦芳
符远翔
李晓彬
谢金明
王虹丽
莫冬传
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Sun Yat Sen University
Greatoo Intelligent Equipment Inc
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Sun Yat Sen University
Greatoo Intelligent Equipment Inc
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Abstract

The invention discloses a preparation method for an epoxy resin compound organic silicon thermal-insulation material. The preparation method includes the steps that 1, a calculated amount of epoxy resin and organic silicon oil are weighed, heated inside a constant-temperature device, stirred and mixed evenly; 2, flame retardant, foaming agents, nanometer silicon dioxide and modifying agents are added into a resin system obtained through the step1, stirred and mixed evenly; 3, a mixed resin system obtained through the step2 is transferred and injected into a PTFE mold or a steel mold and then transferred into a high-temperature furnace to be subjected to constant-temperature expansion, and then the thermal-insulation and flame-retardant epoxy resin compound organic silicon material is obtained through demolding. The method can be used for preparing the controllable thermal-insulation flame-retardant material, is simple in preparation technology and can be applied to industrial thermal insulation easily.

Description

A kind of preparation method of epoxy resin composite organic lagging material
Technical field
The invention belongs to the preparing technical field of epoxy resin composite material, specifically, relate to a kind of preparation method of epoxy resin composite organic lagging material.
Background technology
Lagging material tool in the production and life of people plays a very important role, and can be used as the protecting materials of various instrument, valuables and precision instrument etc.Foaming thermal-insulating normally in one or several basic substances mixed foaming agent prepare after adding thermal expansion.Epoxy resin is a kind of base mateiral often selected in actual applications, and it has the widespread uses in a lot of field such as high resistance toheat, excellent adhesive property and mechanical property.Epoxy resin can prepare apparent low density foam material through foaming, form lightweight and structure is hard, and there is better electrical property, insulativity, the performance such as corrosion-resistant and high temperature resistant, the people such as Zhang Chun (CN201010242589.8) are by filling inorganic nano-particle (silicon-dioxide and polynite) has prepared a kind of epoxy resin composite foam material with better expansion character in the epoxy; The people such as Yu Yi (CN20101217986.X) report a kind of method at the foamable epoxy resin composite of room temperature, the mechanical property that the sample of preparation has had.But because of the intrinsic fragility of epoxide resin material itself, usual needs carry out adding dissimilar material and carry out modification, this research considers that the material of preparation can be incubated use in about 200 DEG C and following environment, and the organic silicone oil that have selected different viscosity carries out modification.Organic silicone oil is a kind of organopolysiloxane of different polymerization degree chain-like structure, and what it had high resistance toheat, high viscosity stability, excellent chemical stability and an excellence is generally used for the fields such as electronic apparatus, material of construction, petrochemical complex and medical and health, Aeronautical R&D and military technique to performances such as the corrosive effects of material are little.Epoxy resin and organic silicone oil mix by the mode by stirring in preparation process, in order to prevent the generation by sweat layer phenomenon, with the addition of the resin system energy stable existence that nano silicon carries out regulating epoxy resin and the organic silicone oil mixing making to prepare, and there is good swelling property and demolding performace.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, stablize high temperature system with nano-silicon dioxide modified epoxy resin and organic silicone oil System forming, provide a kind of preparation method of epoxy resin organosilicon expansion lagging material.
The technical solution used in the present invention is by epoxy resin and organic silicone oil mixing, add nano silicon and carry out resin system modification, then the performance modifier of swelling agent and fire retardant and other type is added, obtain a kind of method of the epoxy resin composite organic lagging material that can use at about 200 DEG C environment, concrete preparation process is as follows:
(1) prepare uniform resin system: the epoxy resin and the organic silicone oil that weigh calculated amount, then heat in thermostat and be uniformly mixed;
(2) the epoxy resin organosilicon material mixed is prepared: in the resin system of above-mentioned steps (1) gained, add fire retardant, whipping agent, nano silicon and properties-correcting agent and be uniformly mixed;
(3) the epoxy resin silicone body based material of high-temperature molding is prepared: gained hybrid resin system in above-mentioned steps (2) turned and be injected in polytetrafluoroethylene PTFE mould or steel die, then transfer to thermostatic expansion in High Temperature Furnaces Heating Apparatus, then obtain a kind of insulation of epoxy resin composite organic and the material of flame retardant properties with heat-insulating property through the demoulding.
The present invention, the weight of raw and auxiliary material used is: epoxy resin 10 ~ 40; 5 ~ 30 parts, bi-component epoxide-resin solidifying agent; Organic silicone oil 20 ~ 55 parts; Fire retardant 5 ~ 20 parts; Whipping agent 0.5 ~ 10 part; Aerosil 0.1 ~ 2 part; Properties-correcting agent is silane coupling agent 0.1 ~ 2 part and toughner 1 ~ 10 part.
The present invention, described epoxy resin can adopt high temperature resistant single component epoxy, also can adopt one or several the mixing in the bisphenol A type epoxy resin of general type, glycidyl ether type epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic based epoxy resin and alicyclic based epoxy resin.When selecting high temperature resistant single component epoxy, the bi-component epoxide-resin solidifying agent in formula is 0.
The present invention, described organic silicone oil comprises the mixing of one or more in methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, methyl phenyl silicone oil, methyl vinyl silicon oil, ethyl containing hydrogen silicone oil and hydroxyl hydrogen silicone oil, can select the used in combination of viscosity a kind of or not of the same race in concrete use.
The present invention, described fire retardant is the mixing of one or more in aluminium hydroxide, magnesium hydroxide, non-halogen organism NP-300, melamine cyanurate salt MCA and silicon-series five-retardant.
The present invention, described whipping agent is the mixing of one or more in Cellmic C 121 (AC whipping agent), polymer tiny balloon (microballoon whipping agent) and carbonate foaming agent (as calcium carbonate, magnesiumcarbonate, sodium bicarbonate).
The present invention, described aerosil is the granularity that laboratory is prepared by Stober method is the SiO 2 powder of 80 ~ 200nm, or the aerosil powder of business-like oleophylic type.
The present invention, described silane coupling agent is the mixing of one or more in KH-550, KH560, KH-570, KH-580 and KH-620; Described toughner is styrene-butadiene rubber(SBR), polyamide resin and Nano-meter CaCO3 3in the mixing of one or more.
The present invention, thermostat described in step (1) is constant temperature water bath apparatus or oil bath device, control temperature is at 75 ~ 110 DEG C, constant temperature time is 30 ~ 40min, hybrid mode is that mechanical stirring or three-roller stir, wherein churned mechanically speed is 150 ~ 1000rpm, and three-roller is constant speed 200rpm.
The present invention, in step (3), the temperature of constant temperature is 130 ~ 200 DEG C, and constant temperature time is 60 ~ 240min.
The present invention, owing to adopting the organic silicone oil of different viscosity, modification is carried out to epoxy resin, epoxy resin and organic silicone oil mix by the mode by stirring in preparation process, in order to prevent the generation by sweat layer phenomenon, with the addition of the resin system energy stable existence that nano silicon carries out regulating epoxy resin and the organic silicone oil mixing making to prepare, and there is good swelling property and demolding performace, material prepared therefrom can be incubated use in 200 DEG C and following environment.Its preparation technology is simple, can easily be generalized in industrial heat preservation application.
Accompanying drawing explanation
The silicon-dioxide SEM that Fig. 1 is prepared in laboratory schemes;
Fig. 2 prepares the photo of epoxy resin composite organic material;
Fig. 3 prepares the SEM figure of epoxy resin composite organic material;
Fig. 4 prepares the insulating pipe photo of epoxy resin composite organic material.
Embodiment
Explain the present invention further below in conjunction with specific embodiment, but embodiment does not limit in any form to invention
Embodiment 1: the High temp. epoxy resins 80g of the silicone oil 50g and single-component that take 1000cst is placed in container, is fixed in constent temperature heater and regulates temperature to be 80 DEG C, and the speed regulating stirrer is 300rpm, stirs the resin system that 30min obtains mixing.Then 10g Cellmic C 121 (AC whipping agent) is taken, the nano silicon 0.5g that laboratory is prepared by Stober method, aluminium hydroxide 15g, non-halogen organism (NP-300) 15g, styrene-butadiene rubber(SBR) 10g and 1gKH-550 adds in the resin system mixed respectively, after the speed of 100rpm stirs, again through the high-speed mixing of 800rpm, the resin system mixed is transferred in the mould of PTFE, then mould is placed in the baking oven of temp. controllable, controlling expansion temperature is 190 DEG C, period is 1.2 hours, then with furnace temperature cool to room temperature, obtain the organosilyl lagging material of foamable epoxy resin, the thermal conductivity obtaining the sample of this example preparation through thermal conductivity test is 0.052W/m*K.The SEM figure of Fig. 1 silicon-dioxide, Fig. 2 is the photo preparing sample, and Fig. 3 is the SEM figure preparing small sample, and Fig. 4 is the photo of the heat-preservation cylinder preparing sample.
Embodiment 2: the silicone oil 70g taking 12500cst, bisphenol A type epoxy resin 60g and solidifying agent 25g is placed in container, be fixed in constent temperature heater and regulate temperature to be 85 DEG C, the speed regulating stirrer is 250rpm, stirs the resin system that 40min obtains mixing.Then 20g polymer tiny balloon (microballoon whipping agent), nano silicon 1g, the magnesium hydroxide 20g of business, melamine cyanurate salt (MCA) 25g, Nano-meter CaCO3 is taken 315g and 2gKH-570 adds in the resin system mixed respectively, after the speed of 150rpm stirs, again through the high-speed mixing of 750rpm, the resin system mixed is transferred in steel die, then mould is placed in the baking oven of temp. controllable, controlling expansion temperature is 170 DEG C, period is 2 hours, then with furnace temperature cool to room temperature, obtain the organosilyl lagging material of foamable epoxy resin, the thermal conductivity obtaining the sample of this example preparation through thermal conductivity test is 0.050W/m*K.
Embodiment 3: taking 1000cst and 12500cst mixing silicone oil 60g(mass ratio is 2:1) and the High temp. epoxy resins 75g of single-component be placed in container, be fixed in constent temperature heater and regulate temperature to be 90 DEG C, the speed regulating stirrer is 250rpm, stirs the resin system that 25min obtains mixing.Then 10g Cellmic C 121 (AC whipping agent) and 10g sodium bicarbonate is taken, the nano silicon 1.5g that laboratory is prepared by Stober method, aluminium hydroxide 15g, magnesium hydroxide 15g, styrene-butadiene rubber(SBR) 10g and polyamide resin 5g, and the mixture of 1.5gKH-560 and KH-620 (mass ratio is 1:1) adds in uniform resin system respectively, after the speed of 80rpm stirs, again through the high-speed mixing 30min of 900rpm, the resin system mixed is transferred in the mould of PTFE, then mould is placed in the baking oven of temp. controllable, controlling expansion temperature is 185 DEG C, period is 1.5 hours, then with furnace temperature cool to room temperature, obtain the organosilyl lagging material of foamable epoxy resin, the thermal conductivity obtaining the sample of this example preparation through thermal conductivity test is 0.048W/m*K.

Claims (10)

1. a preparation method for epoxy resin composite organic lagging material, is characterized in that comprising the steps:
(1) prepare uniform resin system: the epoxy resin and the organic silicone oil that weigh calculated amount, then heat in thermostat and be uniformly mixed;
(2) the epoxy resin organosilicon material mixed is prepared: in the resin system of above-mentioned steps (1) gained, add fire retardant, whipping agent, nano silicon and properties-correcting agent and be uniformly mixed;
(3) the epoxy resin silicone body based material of high-temperature molding is prepared: gained hybrid resin system in above-mentioned steps (2) turned and be injected in polytetrafluoroethylene PTFE mould or steel die, then transfer to thermostatic expansion in High Temperature Furnaces Heating Apparatus, then obtain a kind of insulation of epoxy resin composite organic and the material of flame retardant properties with heat-insulating property through the demoulding.
2. preparation method according to claim 1, is characterized in that, the weight of raw and auxiliary material used is: epoxy resin 10 ~ 40; 5 ~ 30 parts, bi-component epoxide-resin solidifying agent; Organic silicone oil 20 ~ 55 parts; Fire retardant 5 ~ 20 parts; Whipping agent 0.5 ~ 10 part; Aerosil 0.1 ~ 2 part; Properties-correcting agent is silane coupling agent 0.1 ~ 2 part and toughner 1 ~ 10 part.
3. preparation method according to claim 1 and 2, it is characterized in that, described epoxy resin comprises high temperature resistant single component epoxy, or one or several the mixing in the bisphenol A type epoxy resin of general type, glycidyl ether type epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic based epoxy resin and alicyclic based epoxy resin.
4. preparation method according to claim 1 and 2, it is characterized in that, described organic silicone oil comprises the mixing of one or more in methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, methyl phenyl silicone oil, methyl vinyl silicon oil, ethyl containing hydrogen silicone oil and hydroxyl hydrogen silicone oil, in concrete use, select the used in combination of viscosity a kind of or not of the same race.
5. preparation method according to claim 1 and 2, is characterized in that, described fire retardant is the mixing of one or more in aluminium hydroxide, magnesium hydroxide, non-halogen organism NP-300, melamine cyanurate salt MCA and silicon-series five-retardant.
6. preparation method according to claim 1 and 2, is characterized in that, described whipping agent is the mixing of one or more in Cellmic C 121, polymer tiny balloon and carbonate foaming agent.
7. preparation method according to claim 1 and 2, is characterized in that, described aerosil is the granularity that laboratory is prepared by Stober method is the SiO 2 powder of 80 ~ 200nm, or the aerosil powder of business-like oleophylic type.
8. preparation method according to claim 2, is characterized in that, described silane coupling agent is the mixing of one or more in KH-550, KH560, KH-570, KH-580 and KH-620; Described toughner is styrene-butadiene rubber(SBR), polyamide resin and Nano-meter CaCO3 3in the mixing of one or more.
9. preparation method according to claim 1, it is characterized in that, thermostat described in step (1) is constant temperature water bath apparatus or oil bath device, control temperature is at 75 ~ 110 DEG C, constant temperature time is 30 ~ 40min, hybrid mode is that mechanical stirring or three-roller stir, and wherein churned mechanically speed is 150 ~ 1000rpm, and three-roller is constant speed 200rpm.
10. preparation method according to claim 1, is characterized in that, in step (3), the temperature of constant temperature is 130 ~ 200 DEG C, and constant temperature time is 60 ~ 240min.
CN201510704834.5A 2015-10-27 2015-10-27 A kind of preparation method of epoxy resin composite organic insulation material Active CN105176092B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106084525A (en) * 2016-06-27 2016-11-09 林春梅 A kind of novel light adiabator and preparation method thereof
CN106673509A (en) * 2016-12-09 2017-05-17 广西北海浩邦新能源科技有限公司 Heat insulating material with good flame retardant property
CN106673581A (en) * 2016-12-09 2017-05-17 广西北海浩邦新能源科技有限公司 Flame retardant heat insulating material
CN107739441A (en) * 2017-09-30 2018-02-27 烟台德邦先进硅材料有限公司 A kind of synthetic method of novel organosilicon modified epoxy
CN111908945A (en) * 2019-05-10 2020-11-10 南通联鑫新材料科技有限公司 Lightweight epoxy resin composite board and preparation method thereof
CN115073744A (en) * 2022-06-17 2022-09-20 中国科学院长春应用化学研究所 High-cohesiveness silicone rubber and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101319085A (en) * 2008-07-22 2008-12-10 上海材料研究所 Light-high-strength epoxy foam material and preparation method thereof
CN102863747A (en) * 2012-09-25 2013-01-09 中国工程物理研究院化工材料研究所 High-temperature-resistance high-strength epoxy foam plastic and preparation method thereof
CN103910974A (en) * 2014-04-22 2014-07-09 济南大学 Hollow-microsphere-filled epoxy resin composite foam material and preparation method thereof
CN104629361A (en) * 2015-02-09 2015-05-20 中国工程物理研究院化工材料研究所 High-temperature-resistant foamed plastic composition and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101319085A (en) * 2008-07-22 2008-12-10 上海材料研究所 Light-high-strength epoxy foam material and preparation method thereof
CN102863747A (en) * 2012-09-25 2013-01-09 中国工程物理研究院化工材料研究所 High-temperature-resistance high-strength epoxy foam plastic and preparation method thereof
CN103910974A (en) * 2014-04-22 2014-07-09 济南大学 Hollow-microsphere-filled epoxy resin composite foam material and preparation method thereof
CN104629361A (en) * 2015-02-09 2015-05-20 中国工程物理研究院化工材料研究所 High-temperature-resistant foamed plastic composition and preparation method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106084525A (en) * 2016-06-27 2016-11-09 林春梅 A kind of novel light adiabator and preparation method thereof
CN106673509A (en) * 2016-12-09 2017-05-17 广西北海浩邦新能源科技有限公司 Heat insulating material with good flame retardant property
CN106673581A (en) * 2016-12-09 2017-05-17 广西北海浩邦新能源科技有限公司 Flame retardant heat insulating material
CN107739441A (en) * 2017-09-30 2018-02-27 烟台德邦先进硅材料有限公司 A kind of synthetic method of novel organosilicon modified epoxy
CN111908945A (en) * 2019-05-10 2020-11-10 南通联鑫新材料科技有限公司 Lightweight epoxy resin composite board and preparation method thereof
CN115073744A (en) * 2022-06-17 2022-09-20 中国科学院长春应用化学研究所 High-cohesiveness silicone rubber and preparation method thereof
CN115073744B (en) * 2022-06-17 2023-12-05 中国科学院长春应用化学研究所 High-cohesiveness silicon rubber and preparation method thereof

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