CN105176092B - A kind of preparation method of epoxy resin composite organic insulation material - Google Patents

A kind of preparation method of epoxy resin composite organic insulation material Download PDF

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CN105176092B
CN105176092B CN201510704834.5A CN201510704834A CN105176092B CN 105176092 B CN105176092 B CN 105176092B CN 201510704834 A CN201510704834 A CN 201510704834A CN 105176092 B CN105176092 B CN 105176092B
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epoxy resin
preparation
silicone oil
organic
mixing
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CN105176092A (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 kind of preparation method of epoxy resin composite organic insulation material, including(1)The epoxy resin and organic silicone oil of amount of calculation are weighed, then heats and is uniformly mixed in thermostat;(2)In step(1)Fire retardant, foaming agent, nano silicon and modifying agent are added in the resin system of gained and is uniformly mixed;(3)By step(2)Middle gained hybrid resin system turns to be injected into polytetrafluoroethylene PTFE mould or steel mold, is then transferred into thermostatic expansion in high temperature furnace, then obtain a kind of insulation of epoxy resin composite organic with heat-insulating property and the material of fire resistance by the demoulding.This method can prepare a kind of controllable heat-insulating fireproof material, simple with preparation technology, and can easily be generalized in industrial heat preservation application.

Description

A kind of preparation method of epoxy resin composite organic insulation material
Technical field
The invention belongs to the preparing technical field of epoxy resin composite material, specifically, is related to a kind of epoxy resin and answers Close the preparation method of organosilicon insulation material.
Background technology
Insulation material has in the production and life of people to play a very important role, and can be used as various instrument, valuables And the protection materials of precision instrument etc..Foaming thermal-insulating is typically the mixed foaming agent in one or several kinds of basic substances Prepared after heating expands.Epoxy resin is a kind of basic material being often selected in actual applications, and it is that have height The extensive use in many fields such as heat resistance, excellent adhesive property and mechanical property.Epoxy resin is by foaming It can prepare the low expanded material of apparent density, form lightweight and structure is hard, and with more preferable electrical property, insulating properties, resistance to The performance, Zhang Chun et al. such as corrosion and high temperature resistant(CN 201010242589.8)By filling inorganic nano-particle in the epoxy Son(Silica and montmorillonite)It is prepared for a kind of epoxy resin composite foam material with preferable expansion character;Yu Yi etc. People(CN 20101217986.X)Report a kind of method in the foamable epoxy resin composite of room temperature, the sample tool of preparation The mechanical performance having had.The but intrinsic fragility because of epoxide resin material in itself, it usually needs be added different types of Material is modified, and the material that this research is considered to prepare can be incubated use in about 200 DEG C and following environment, have selected not Organic silicone oil with viscosity is modified.Organic silicone oil is a kind of polysiloxane of different polymerization degree chain structure, and it has There are high heat resistance, high viscosity stability, excellent chemical stability and the excellent corrosive effects to material small It is generally used for the neck such as electronic apparatus, construction material, petrochemical industry and medical and health, Aeronautical R&D and military technology etc. performance Domain.Epoxy resin and organic silicone oil are mixed by way of stirring in preparation process, in order to prevent by sweat layer phenomenon Generation, with the addition of nano silicon be adjusted enable prepare epoxy resin and organic silicone oil mixing resin system It is stabilized, and there is good dilatancy and demolding performace.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, with nano-silicon dioxide modified epoxy resin and organic silicone oil A kind of stable high temperature system of System forming, there is provided preparation method of epoxy resin organosilicon expansion insulation material.
The technical solution adopted by the present invention is to mix epoxy resin and organic silicone oil, adds nano silicon tree Resin system is modified, and then adds swelling agent and fire retardant and other types of performance modifier, obtaining one kind can be on 200 DEG C of left side The method for the epoxy resin composite organic insulation material that right environment uses, specific preparation process are as follows:
(1)Prepare uniform resin system:The epoxy resin and organic silicone oil of amount of calculation are weighed, then in thermostat Heat and be uniformly mixed;
(2)Prepare well mixed epoxy resin organosilicon material:In above-mentioned steps(1)Added in the resin system of gained Fire retardant, foaming agent, nano silicon and modifying agent are simultaneously uniformly mixed;
(3)Prepare the epoxy resin silicone body based material of high-temperature molding:By above-mentioned steps(2)Middle gained hybrid resin body System turns to be injected into polytetrafluoroethylene PTFE mould or steel mold, is then transferred into thermostatic expansion in high temperature furnace, then by de- Mould obtains a kind of insulation of epoxy resin composite organic with heat-insulating property and the material of fire resistance.
The present invention, the weight of raw and auxiliary material used are:High temperature resistant single component epoxy 10 ~ 40;Organic silicone oil 20 ~ 55 parts;5 ~ 20 parts of fire retardant;0.5 ~ 10 part of foaming agent;0.1 ~ 2 part of nano silicon;Modifying agent is silane coupler 0.1 ~ 2 parts and 1 ~ 10 part of toughener.
The present invention, the epoxy resin can use high temperature resistant single component epoxy, can also use the bisphenol-A of general type Type epoxy resin, glycidyl ether type epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, line One or several kinds of mixing in type aliphatic category epoxy resin and alicyclic based epoxy resin.When from high temperature resistant one-component During epoxy resin, the bi-component epoxide-resin curing agent in formula is 0.
The present invention, the organic silicone oil include methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, methyl phenyl silicone oil, methyl second One or more of mixing in alkenyl silicone oil, ethyl containing hydrogen silicone oil and hydroxyl hydrogen silicone oil, one may be selected in specifically used Kind or viscosity not of the same race be used in mixed way.
The present invention, the fire retardant are aluminium hydroxide, magnesium hydroxide, non-halogen organic matter NP-300, melamine cyanurate One or more of mixing in salt MCA and silicon-series five-retardant.
The present invention, the foaming agent are azodicarbonamides(AC foaming agents), macromolecule tiny balloon(Microballoon foaming agent) And carbonate foaming agent(Such as calcium carbonate, magnesium carbonate, sodium acid carbonate)In one or more of mixing.
The present invention, the nano silicon are that the granularity that laboratory is prepared by Stober methods is the two of 80 ~ 200 nm Silicon oxide powder, or the nano grade silica particles of commercialized oleophylic type.
The present invention, the silane coupler are one kind or several in KH-550, KH560, KH-570, KH-580 and KH-620 The mixing of kind;Described toughener is butadiene-styrene rubber, polyamide and Nano-meter CaCO33In one or more of mixing.
The present invention, step(1)Described in thermostat be constant temperature water bath apparatus or oil bath device, control temperature is 75 ~ 110 DEG C, constant temperature time is 30 ~ 40 min, and hybrid mode is that mechanical agitation or three-roller stir, wherein churned mechanically speed It is the rpm of constant speed 200 to spend for 150 ~ 1000 rpm, three-roller.
The present invention, step(3)The temperature of middle constant temperature is 130 ~ 200 DEG C, and constant temperature time is 60 ~ 240 min.
The present invention, due to being modified using the organic silicone oil of different viscosities to epoxy resin, by stirring in preparation process The mode mixed is mixed epoxy resin and organic silicone oil, in order to prevent by sweat layer phenomenon, with the addition of nanometer two Silica, which is adjusted, enables the epoxy resin prepared and the resin system of organic silicone oil mixing to be stabilized, and with good Dilatancy and demolding performace, material prepared therefrom use can be incubated in 200 DEG C and following environment.Its preparation technology letter It is single, can easily it be generalized in industrial heat preservation application.
Brief description of the drawings
Silica SEM figures prepared by Fig. 1 laboratories;
Fig. 2 prepares the photo of epoxy resin composite organic material;
Fig. 3 prepares the SEM figures of epoxy resin composite organic material;
Fig. 4 prepares the insulating tube photo of epoxy resin composite organic material.
Embodiment
The present invention is explained further below in conjunction with specific embodiment, but embodiment does not limit in any form to invention
Embodiment 1:The g of silicone oil 50 and one-component that weigh 1000 the cst g of High temperature epoxy resinses 80 are placed in container, Gu It is 80 DEG C to be scheduled in constent temperature heater and adjust temperature, and the speed for adjusting mixer is 300 rpm, and it is equal that 30 min of stirring obtain mixing Even resin system.Then 10 g azodicarbonamides are weighed(AC foaming agents), the nanometer that is prepared by Stober methods of laboratory The g of silica 0.5, the g of aluminium hydroxide 15, non-halogen organic matter(NP-300)15 g, the g of butadiene-styrene rubber 10 and 1 g KH-550 It is separately added into well mixed resin system, after 100 rpm speed stirs, then the high speed by 800 rpm Mixing, well mixed resin system is transferred in PTFE mould, then mould is placed in the baking oven of temperature controllable, controlled Expansion temperature processed is 190 DEG C, and control time is 1.2 hours, is then cooled to room temperature with furnace temperature, obtains foamable asphalt mixtures modified by epoxy resin The insulation material of fat organosilicon, the thermal conductivity factor that the sample of this preparation is obtained by thermal conductivity test is 0.052 W/m*K.Fig. 1 The SEM figures of silica, Fig. 2 are the photos for preparing sample, and Fig. 3 is the SEM figures for preparing small sample, and Fig. 4 is the guarantor for preparing sample The photo of warm cylinder.
Embodiment 2:Weigh 1000 cst and the g of 12500 cst mixing silicone oil 60(Mass ratio is 2:1)With the height of one-component The g of temperature epoxy resin 75 is placed in container, and it is 90 DEG C to be fixed in constent temperature heater and adjust temperature, and the speed for adjusting mixer is 250 rpm, 25 min of stirring obtain well mixed resin system.Then 10 g azodicarbonamides are weighed(AC foaming agents)With The g of nano silicon 1.5, the g of aluminium hydroxide 15, the magnesium hydroxide 15 that 10g sodium acid carbonates, laboratory are prepared by Stober methods G, the g of the butadiene-styrene rubber 10 and g of polyamide 5, and 1.5 g KH-560 and KH-620 mixture(Mass ratio is 1:1)Point Do not add in uniform resin system, after 80 rpm speed stirs, then the mixed at high speed 30 by 900 rpm Min, well mixed resin system is transferred in PTFE mould, then mould is placed in the baking oven of temperature controllable, controlled Expansion temperature processed is 185 DEG C, and control time is 1.5 hours, is then cooled to room temperature with furnace temperature, obtains foamable asphalt mixtures modified by epoxy resin The insulation material of fat organosilicon, the thermal conductivity factor that the sample of this preparation is obtained by thermal conductivity test is 0.048W/m*K.

Claims (6)

  1. A kind of 1. preparation method of epoxy resin composite organic insulation material, it is characterised in that:The weight of raw and auxiliary material used Part matches:High temperature resistant single component epoxy 10 ~ 40;20 ~ 55 parts of organic silicone oil;5 ~ 20 parts of fire retardant;Foaming agent 0.5 ~ 10 Part;0.1 ~ 2 part of nano silicon;Modifying agent is 1 ~ 10 part of 0.1 ~ 2 part of silane coupler and toughener, and its preparation method includes Following steps:
    (1)Prepare uniform resin system:The epoxy resin and organic silicone oil of amount of calculation are weighed, is then heated in thermostat And be uniformly mixed, wherein, thermostat is constant temperature water bath apparatus or oil bath device, and control temperature is permanent at 75 ~ 110 DEG C The warm time is 30 ~ 40 min, and hybrid mode is that mechanical agitation or three-roller stir, wherein churned mechanically speed be 150 ~ 1000 rpm, three-roller are the rpm of constant speed 200;
    (2)Prepare well mixed epoxy resin organosilicon material:In above-mentioned steps(1)Added in the resin system of gained fire-retardant Agent, foaming agent, nano silicon and modifying agent are simultaneously uniformly mixed;
    (3)Prepare the epoxy resin silicone body based material of high-temperature molding:By above-mentioned steps(2)Middle gained hybrid resin system turns It is injected into polytetrafluoroethylene PTFE mould or steel mold, is then transferred into thermostatic expansion in high temperature furnace, then by being stripped To a kind of insulation of epoxy resin composite organic with heat-insulating property and the material of fire resistance, wherein, the temperature of constant temperature It it is 130 ~ 200 DEG C, constant temperature time is 60 ~ 240 min.
  2. 2. preparation method according to claim 1, it is characterised in that the organic silicone oil includes methyl-silicone oil, ethyl silicon Oil, phenyl silicone oil, methyl phenyl silicone oil, methyl vinyl silicon oil, ethyl containing hydrogen silicone oil and one kind in hydroxyl hydrogen silicone oil or Several mixing, a kind of or viscosity not of the same race it is used in mixed way in specifically used middle selection.
  3. 3. preparation method according to claim 1, it is characterised in that the fire retardant is aluminium hydroxide, magnesium hydroxide, non- One or more of mixing in halogen organic matter NP-300, melamine cyanurate salt MCA and silicon-series five-retardant.
  4. 4. preparation method according to claim 1, it is characterised in that the foaming agent is azodicarbonamide, macromolecule One or more of mixing in tiny balloon and carbonate foaming agent.
  5. 5. preparation method according to claim 1, it is characterised in that the nano silicon is laboratory by Stober The SiO 2 powder that the granularity of method preparation is 80 ~ 200 nm, or the nano-silica powder of commercialized oleophylic type End.
  6. 6. preparation method according to claim 1, it is characterised in that the silane coupler is KH-550, KH560, KH- 570th, one or more of mixing in KH-580 and KH-620;Described toughener is butadiene-styrene rubber, polyamide and received Rice CaCO3In one or more of mixing.
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 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
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
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
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
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

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

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