CN103788582A - Pouring type epoxy composite filling material and production method thereof - Google Patents
Pouring type epoxy composite filling material and production method thereof Download PDFInfo
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- CN103788582A CN103788582A CN201310730137.8A CN201310730137A CN103788582A CN 103788582 A CN103788582 A CN 103788582A CN 201310730137 A CN201310730137 A CN 201310730137A CN 103788582 A CN103788582 A CN 103788582A
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Abstract
The invention relates to a pouring type epoxy composite filling material and a production method thereof. The composite filling material comprises the following chemical components the following chemical components: 100 parts of the epoxy resin, 0-30 parts of the epoxy active diluting agent, 1-5 parts of the silane coupling agent, 1-3 parts of the organic siloxane de-foaming agent, 35-70 parts of the hollow glass micro-beads, 30-80 parts of the curing agent and 0-3 parts of the catalyst. The material provided by the invention has low viscosity, has good mobility and leveling property and is suitable for a vacuum pouring or high-pressure injection molding process; the density of the material provided by the invention is slightly lower than that of seawater; the solidified material has no air bubbles and does not crack; the pouring type epoxy composite filling material has high rigidity and high strength and can resist long-time seawater soaking.
Description
Technical field
The present invention relates to a kind of polymer matrix composite, be specifically related to a kind of casting type epoxy group(ing) composite filling material and manufacture method thereof.
Background technology
Polymer-based carbon composite filling material is the important supplementary material of ocean petroleum developing, and the industrial advanced countries such as American and Britain, day, Russia are since the development sixties in 20th century and for deep seafloor exploitation cause, in industrial circle widespread uses such as civilian, business, military affairs.The low-density and high-strength composite filling material of external development is to adopt high-intensity resin as matrix, fills buoyancy adjustment medium as matrix, adopts special process to process.Wherein prefabrication type solid buoyancy packing material preparation method reports morely, and U.S. Pat P 4829094, US P 4843104, US P 4902722, USP 4916173, US P 4595623, USP 6166109 have reported solid buoyancy packing materials that some adopt different methods to prepare.
Chinese patent CN201010176618.5 has reported a kind of by Yu Haiyang bottom observation platform composite filling material and manufacture method thereof.Formed by liquid bisphenol A epoxy resin, fourth cyanogen latex toughner, polyamide curing agent, r-glycidyl ether oxygen propyl trimethoxy silicane coupling agent, filling hollow glass micropearl, can invade for a long time bubble in seawater, safe and reliable.
There are a large amount of patent reports for electrical apparatus insulation encapsulated epoxy resin casting type matrix material, Chinese patent CN 1455799, CN 1516206, CN 200710134818, CN200510091147, CN O1819651, CN 200510006698 etc., conventionally adopt liquid bisphenol A epoxy resin, anhydride curing agent, tertiary amine catalyst, active micro silicon powder weighting agent is raw material, vacuum pouring or high-pressure injection technological forming.Chinese patent CN 200510019 has reported a kind of hollow glass micropearl reinforced epoxy matrix material and manufacture method thereof.Be made up of A material and B material, A expects by bisphenol A epoxide resin, diglycidyl ether of ethylene glycol reactive thinner, and TSL 8330 coupling agent, hollow glass micropearl and silicon powder filler form.B expects by methyl tetrahydrophthalic acid anhydride curing agent, dimethylbenzyl amine catalyst formation.Relevant naval vessel ballast tank has no report by the composite filled ballast material of epoxy group(ing) patent.
?
summary of the invention
The present invention overcomes the deficiencies in the prior art, a kind of casting type epoxy group(ing) composite filling material and manufacture method thereof are proposed, material viscosity of the present invention is low, there is good mobile, levelling property, be applicable to vacuum pouring or high pressure injection moulding technique, density is a little less than seawater, and cured article does not ftracture without bubble, high rigidity, high strength, long-term sea water resistance soaks.
Technical scheme of the present invention is, a kind of casting type epoxy group(ing) composite filling material and manufacture method thereof,
describedcomposite filling material comprises epoxy resin, epoxy active diluent, silane coupling agent, organo-siloxane defoamer, hollow glass micropearl, solidifying agent and catalyzer, and its chemical constitution is as follows:
Chemical constitution is by 100 mass parts epoxy resin: epoxy resin 100, epoxy active diluent 0--30, silane coupling agent 1--5, organo-siloxane defoamer 1--3, hollow glass micropearl 35--70, solidifying agent 30--80, catalyzer 0--3, manufacturing step is:
(1) preparation of blank piece: the materials such as epoxy resin, silane coupling agent, hollow glass micropearl, solidifying agent, catalyzer are solidified through premix, dispersion, injection, gradient, prepare blank piece;
(2) cutting, splicing, bonding: blank piece is through mechanical roughing, and excision adhesive surface top layer, binds splicing, preparation standard module;
(3) car, plane, saw, mill precision work: standard module, through precision work such as digital controlled lathes, is prepared cord wood composite filling material ballast module;
(4) outer protecting and application: carry out outer protecting and application according to design requirements.
Preparation technology is:
By in the epoxy resin of metering, epoxy active diluent, silane coupling agent, organo-siloxane defoamer, input mixing tank, with dispersion machine, material stirring is even.Drop into hollow glass micropearl, first low rate mixing makes microballon powder wetting in batches, and then middling speed stirring is even by powder lot dispersing, adds solidifying agent and catalyzer to stir.Be cast in stainless steel mould with high pressure injection moulding machine, gradient is solidified and is prepared blank, through roughing, gluing, solidify after, by digital controlled lathe precision work, prepare composite filling material standard module, carry out outer protecting and application according to design requirements, prepare ballast module.
Epoxy resin described above: bisphenol A epoxide resin, novolac epoxy, cycloaliphatic epoxy resin or its mixture; Wherein the epoxy equivalent (weight) of liquid bisphenol A epoxy resin is 184-225g/mol; Novolac epoxy is line style phenol formaldehyde (PF) epoxy resin, and its epoxy equivalent (weight) is 180-250g/mol; Cycloaliphatic epoxy resin be 3,4-epoxy-cyclohexane formic acid-3 ', 4 '-epoxy-cyclohexane methyl esters, its epoxy equivalent (weight) is 131-143g/mol.
Epoxy active diluent described above: n-butyl glycidyl ether (BGE), phenyl glycidyl ether (PGE), diglycidylether (DGE), diglycidylaniline (DGA) or trihydroxymethylpropanyltri diglycidyl ether (TMPGE);
Solidifying agent described above is: anhydride curing agent is selected from methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methyl carbic anhydride or its mixture; Polymeric amide (300#, 400#, 650#, 651#); Aromatic polyamine is selected from 3,3
,diethyl-4,4
,-diaminodiphenyl-methane, diamino cyclohexyl-methane; Polyetheramine (D-230, D--400, T--403) or phenolic aldehyde quadrol (T--31);
Catalyzer described above: 2,4,6 three (dimethylamino methyl) phenol, benzyldimethylamine, 2-ethyl-4-methylimidazole or nonyl phenol;
Silane coupling agent described above is: 3-(2,3-glycidoxy) propyl trimethoxy silicane (KH560), 3-aminopropyl trimethoxysilane (KH550) or r-methacryloxypropyl trimethoxy silane (KH570);
Hollow glass micropearl density range described above is 0.125-0.60g/cm
3, 0.22-0.51g/cm
3or 0.15-0.60g/cm
3.
the present invention has following beneficial effect:,
Material viscosity of the present invention is low, has good mobile, levelling property, is applicable to vacuum pouring or high pressure injection moulding technique, and density is a little less than seawater, and cured article does not ftracture without bubble, high rigidity, high strength, and long-term sea water resistance soaks.
Embodiment:
embodiment 1
Take 400 grams of epoxy resin, 100 grams of epoxy active diluents, 12 grams of silane coupling agents, 6 grams of organo-siloxane defoamers, drop in FS-D2.2 type rotating speed 0--1000r/min high speed dispersor agitation vat, low speed is even by material stirring, and drop into 150 grams of density is 0.4g/cm in batches
3hollow glass micropearl, first stirring at low speed makes hollow glass micropearl powder be soaked by liquid material, then middling speed dispersed with stirring is even, adds 120 gram 3,3
,-diethyl 4,4
,-diaminodiphenyl-methane and 20 grams of phenolic aldehyde quadrol solidifying agent, unload agitation vat after stirring and be placed in vacuum drying oven together with material, room temperature vacuum defoamation 30 minutes.Material is cast in inner cavity size 120
mm× 120
mmin × 50mm stainless steel mould, with mould together in Electric heat oven 80 ℃ solidify 2 hours, 100 ℃ solidify 2 hours, gradient curing molding, after the demoulding through 120 ℃ of after fixing 4 hours.After having solidified, take out again composite filling material blank after being slowly down to room temperature with baking oven naturally cooling.
Density of material 0.91g/cm
3, uniaxial compressive strength 115Mpa.
embodiment 2
Take 400 grams of epoxy resin, 100 grams of epoxy active diluents, 18 grams of silane coupling agents, 6 grams of organo-siloxane defoamers, drop in FS-D2.2 type rotating speed 0--1000r/min high speed dispersor agitation vat, low speed is even by material stirring, and drop into 280 grams of density is 0.6g/cm in batches
3hollow glass micropearl, first stirring at low speed makes hollow glass micropearl powder be soaked by liquid material, then middling speed dispersed with stirring is even, add 290 grams of methyl tetrahydrophthalic anhydride solidifying agent and 4 grams of benzyldimethylamine catalyzer, after stirring, unload agitation vat and be placed in vacuum drying oven together with material, room temperature vacuum defoamation 30 minutes.Material is cast in inner cavity size 120
mm× 120
mmin × 50mm stainless steel mould, with mould together in Electric heat oven 100 ℃ solidify 2 hours, 120 ℃ solidify 2 hours, gradient curing molding, after the demoulding through 150 ℃ of after fixing 4 hours.After having solidified, take out again composite filling material blank after being slowly down to room temperature with baking oven naturally cooling.
Density of material 0.94g/cm
3, uniaxial compressive strength 126Mpa.
embodiment 3
Take 400 grams of epoxy resin, 40 grams of epoxy active diluents, 8 grams of silane coupling agents, 6 grams of organo-siloxane defoamers, drop in FS-D2.2 type rotating speed 0--1000r/min high speed dispersor agitation vat, low speed is even by material stirring, and drop into 250 grams of density is 0.46g/cm in batches
3hollow glass micropearl, first stirring at low speed makes hollow glass micropearl powder be soaked by liquid material, then middling speed dispersed with stirring is even, add 200 grams of polyetheramine D-400 solidifying agent and 20 grams of nonyl phenol catalyzer, after stirring, unload agitation vat and be placed in vacuum drying oven together with material, room temperature vacuum defoamation 30 minutes.Material is cast in inner cavity size 120
mm× 120
mmin × 50mm stainless steel mould, with mould together in Electric heat oven 80 ℃ solidify 2 hours, 100 ℃ solidify 2 hours, gradient curing molding, after the demoulding through 130 ℃ of after fixing 4 hours.After having solidified, take out again composite filling material blank after being slowly down to room temperature with baking oven naturally cooling.
Density of material 0.87g/cm
3, uniaxial compressive strength 74Mpa.
embodiment 4
Take 5000 grams of epoxy resin, 180 grams of silane coupling agents, 60 grams of organo-siloxane defoamers, drop in mixing tank, and with rotating speed r/min 0-1460 hydraulic elevation type dispersion machine, material stirring is even, and drop into 2200 grams of density is 0.46g/cm in batches
3hollow glass micropearl, low rate mixing makes hollow glass micropearl powder be soaked by liquid material, then middling speed stir material dispersion is even.Add 3500 grams of methylhexahydrophthalic anhydride solidifying agent and 250 grams of 2-ethyl-4-methylimidazole catalyzer, stir.Be cast in inner cavity size 300 with high pressure injection moulding machine
mm× 300
mmin × 100mm stainless steel mould, arise from Electric heat oven 100 ℃ solidify 2 hours together with mould one, 120 ℃ solidified 2 hours, and curing molding, puts into baking oven at once after the demoulding, through 150 ℃ of after fixing 4 hours.After having solidified, take out again composite filling material blank after being slowly down to room temperature with oven temperature naturally cooling.
embodiment 5
Take 54.5Kg epoxy resin, 13.6Kg epoxy active diluent, 1.6Kg silane coupling agent, 1.08Kg organo-siloxane defoamer, drops in mixing tank, with rotating speed r/min 0-1460 hydraulic elevation type dispersion machine, material stirring is even, and drop into 17.6Kg density is 0.46g/cm in batches
3hollow glass micropearl, low rate mixing makes hollow glass micropearl powder be soaked by liquid material, then middling speed stir material dispersion is even.Add 16.5kg 3,3
,-diethyl 4,4
,-diaminodiphenyl-methane and 2.75Kg diethylenetriamine butylglycidyl ether solidifying agent are uniformly dispersed, and are cast in 5 cover inner cavity sizes 300 with high pressure injection moulding machine
mm× 300
mmin × 200mm stainless steel mould, arise from Electric heat oven 80 ℃ solidify 2 hours together with mould one, 100 ℃ solidified 2 hours, and gradient curing molding, puts into baking oven at once after the demoulding, through 120 ℃ of after fixing 4 hours.After having solidified, take out again composite filling material blank after being slowly down to room temperature with oven temperature naturally cooling.
embodiment 6
The composite filling material blank of embodiment 4#, 5#, preparation, exposes unsalted surface through mechanical roughing excision bonding plane top layer, and polishing makes its surfacing and removes dust greasy dirt, sticks with glue agent bonding curing.Composite filling material module through boning, size, through digital controlled lathe precision work, within be controlled at ± 0.5mm of machining precision, is prepared cord wood composite filling material ballast module by drawing, and carries out as requested outer protecting and application.
Composite filling material ballast module performance is as following table:
Table 1 embodiment parameter comparison sheet
Parameter name | Embodiment 4 | Embodiment 5 |
Density g/cm 3 | 0.932 | 0.945 |
? Uniaxial compressive strength Mpa | 124 | 132 |
Volume change % after solidifying | 0.8 | 1.5 |
Resistance to hydrostatic pressure Mpa/h | 20/8 | 20/8 |
Water-intake rate % | 0.08 | 0.09 |
Material surface is without cracking, without creep, undeformed, and sea water immersion is after 6 months, and material surface and bonding coat intensity are without considerable change.
Claims (3)
1. a casting type epoxy group(ing) composite filling material, it is characterized in that: described composite filling material comprises epoxy resin, epoxy active diluent, silane coupling agent, organo-siloxane defoamer, hollow glass micropearl, solidifying agent and catalyzer, and its chemical constitution is as follows:
Chemical constitution is by 100 mass parts epoxy resin: epoxy resin 100, epoxy active diluent 0--30, silane coupling agent 1--5, organo-siloxane defoamer 1--3, hollow glass micropearl 35--70, solidifying agent 30--80, catalyzer 0--3, manufacturing step is:
(1) preparation of blank piece: the materials such as epoxy resin, silane coupling agent, hollow glass micropearl, solidifying agent, catalyzer are solidified through premix, dispersion, injection, gradient, prepare blank piece;
(2) cutting, splicing, bonding: blank piece is through mechanical roughing, and excision adhesive surface top layer, binds splicing, preparation standard module;
(3) car, plane, saw, mill precision work: standard module, through precision work such as digital controlled lathes, is prepared cord wood composite filling material ballast module;
(4) outer protecting and application: carry out outer protecting and application according to design requirements.
2. casting type epoxy group(ing) composite filling material according to claim 1, is characterized in that: preparation technology is:
By the epoxy resin of metering, epoxy active diluent, silane coupling agent, organo-siloxane defoamer, drop in mixing tank, with dispersion machine, material stirring is even, drop into hollow glass micropearl in batches, first low rate mixing makes microballon powder wetting, then middling speed stirs powder lot dispersing is even, add solidifying agent and catalyzer to stir, be cast in stainless steel mould with high pressure injection moulding machine, the curing blank of preparing of gradient, through roughing, gluing, after solidifying, by digital controlled lathe precision work, prepare composite filling material standard module, carry out outer protecting and application according to design requirements, prepare ballast module.
3. casting type epoxy group(ing) composite filling material according to claim 1 and 2, is characterized in that:
Epoxy resin described above is, bisphenol A epoxide resin, novolac epoxy, cycloaliphatic epoxy resin or its mixture; Wherein the epoxy equivalent (weight) of liquid bisphenol A epoxy resin is 184-225g/mol; Novolac epoxy is line style phenol formaldehyde (PF) epoxy resin, and its epoxy equivalent (weight) is 180-250g/mol; Cycloaliphatic epoxy resin be 3,4-epoxy-cyclohexane formic acid-3 ', 4 '-epoxy-cyclohexane methyl esters, its epoxy equivalent (weight) is 131-143g/mol;
Epoxy active diluent described above: n-butyl glycidyl ether (BGE), phenyl glycidyl ether (PGE), diglycidylether (DGE), diglycidylaniline (DGA) or trihydroxymethylpropanyltri diglycidyl ether (TMPGE);
Solidifying agent described above is: anhydride curing agent is selected from methyl tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methyl carbic anhydride or its mixture; Polymeric amide (300#, 400#, 650#, 651#); Aromatic polyamine is selected from 3,3
,diethyl-4,4
,-diaminodiphenyl-methane, diamino cyclohexyl-methane; Polyetheramine (D-230, D--400, T--403) or phenolic aldehyde quadrol (T--31);
Catalyzer described above is: 2,4,6 three (dimethylamino methyl) phenol, benzyldimethylamine, 2-ethyl-4-methylimidazole or nonyl phenol;
Silane coupling agent described above is: 3-(2,3-glycidoxy) propyl trimethoxy silicane (KH560), 3-aminopropyl trimethoxysilane (KH550) or r-methacryloxypropyl trimethoxy silane (KH570);
Hollow glass micropearl density range described above is 0.125-0.60g/cm
3, 0.22-0.51g/cm
3or 0.15-0.60g/cm
3.
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CN104530650A (en) * | 2014-12-31 | 2015-04-22 | 青岛海洋新材料科技有限公司 | Submersible vehicle encapsulation composite foam filling materials and preparation method thereof |
WO2017157591A1 (en) * | 2016-03-15 | 2017-09-21 | Huntsman Advanced Materials Licensing (Switzerland) Gmbh | A process for the preparation of insulation systems for electrical engineering, the articles obtained therefrom and the use thereof |
CN107987483A (en) * | 2017-12-26 | 2018-05-04 | 天津康普斯特科技发展有限公司 | A kind of method of the hybrid resin for being used to quickly manufacture injection mold and quick manufacture injection mold |
CN108724832A (en) * | 2017-04-20 | 2018-11-02 | 乐陵市友谊体育器材有限责任公司 | Carbon porcelain arculae |
CN109483705A (en) * | 2018-12-14 | 2019-03-19 | 广西利升石业有限公司 | Temperature-adjusting type jade stone mold |
CN109514714A (en) * | 2018-12-14 | 2019-03-26 | 广西利升石业有限公司 | Jade stone mold |
CN111326298A (en) * | 2020-04-07 | 2020-06-23 | 华北电力大学(保定) | Inner-filling light extra-high voltage composite insulating cross arm |
CN112063118A (en) * | 2020-07-28 | 2020-12-11 | 艾达索高新材料芜湖有限公司 | Low-density flame-retardant epoxy SMC resin composition |
WO2021217551A1 (en) * | 2020-04-30 | 2021-11-04 | 淮阴工学院 | Composite material for preparing dumbbell and method for manufacturing dumbbell using same |
CN114561178A (en) * | 2022-02-25 | 2022-05-31 | 中国航空制造技术研究院 | Low-density flame-retardant filling adhesive and preparation method thereof |
CN115449188A (en) * | 2022-10-25 | 2022-12-09 | 台州市黄岩区武汉理工高性能复合材料技术研究院 | Preparation method of high-strength epoxy mould pressing material |
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WO2017157591A1 (en) * | 2016-03-15 | 2017-09-21 | Huntsman Advanced Materials Licensing (Switzerland) Gmbh | A process for the preparation of insulation systems for electrical engineering, the articles obtained therefrom and the use thereof |
CN109074902A (en) * | 2016-03-15 | 2018-12-21 | 亨斯迈先进化工材料许可(瑞士)有限公司 | Preparation is used for the method for the insulation system of electrical engineering, thus obtained product and application thereof |
CN108724832A (en) * | 2017-04-20 | 2018-11-02 | 乐陵市友谊体育器材有限责任公司 | Carbon porcelain arculae |
CN107987483A (en) * | 2017-12-26 | 2018-05-04 | 天津康普斯特科技发展有限公司 | A kind of method of the hybrid resin for being used to quickly manufacture injection mold and quick manufacture injection mold |
CN109514714A (en) * | 2018-12-14 | 2019-03-26 | 广西利升石业有限公司 | Jade stone mold |
CN109483705A (en) * | 2018-12-14 | 2019-03-19 | 广西利升石业有限公司 | Temperature-adjusting type jade stone mold |
CN111326298A (en) * | 2020-04-07 | 2020-06-23 | 华北电力大学(保定) | Inner-filling light extra-high voltage composite insulating cross arm |
WO2021217551A1 (en) * | 2020-04-30 | 2021-11-04 | 淮阴工学院 | Composite material for preparing dumbbell and method for manufacturing dumbbell using same |
CN112063118A (en) * | 2020-07-28 | 2020-12-11 | 艾达索高新材料芜湖有限公司 | Low-density flame-retardant epoxy SMC resin composition |
CN114561178A (en) * | 2022-02-25 | 2022-05-31 | 中国航空制造技术研究院 | Low-density flame-retardant filling adhesive and preparation method thereof |
CN114561178B (en) * | 2022-02-25 | 2024-01-26 | 中国航空制造技术研究院 | Low-density flame-retardant filling adhesive and preparation method thereof |
CN115449188A (en) * | 2022-10-25 | 2022-12-09 | 台州市黄岩区武汉理工高性能复合材料技术研究院 | Preparation method of high-strength epoxy mould pressing material |
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Application publication date: 20140514 |