CN101805533B - Heat-resistance energy-saving environment-protection epoxy solvent-free paint and production method thereof - Google Patents

Heat-resistance energy-saving environment-protection epoxy solvent-free paint and production method thereof Download PDF

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Publication number
CN101805533B
CN101805533B CN201010168553XA CN201010168553A CN101805533B CN 101805533 B CN101805533 B CN 101805533B CN 201010168553X A CN201010168553X A CN 201010168553XA CN 201010168553 A CN201010168553 A CN 201010168553A CN 101805533 B CN101805533 B CN 101805533B
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heat
epoxy
bismaleimides
percent
free paint
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CN201010168553XA
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CN101805533A (en
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俞翔霄
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SHAANXI HONGYE ELECTROMECHANICAL AND CHEMICAL ENGINEERING Co Ltd
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SHAANXI HONGYE ELECTROMECHANICAL AND CHEMICAL ENGINEERING Co Ltd
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Abstract

The invention discloses heat-resistance energy-saving environment-protection epoxy solvent-free paint. The prepared heat-resistance energy-saving environment-protection epoxy solvent-free paint consists of the following ingredients in percentage by weight: 40 to 50 percent of heat-resistance polyester, 8 to 10 percent of modified epoxy, 10 to 12 percent of tongma estolide, 30 to 40 percent of vinyltoluene, 1 to 1.5 percent of cumyl peroxide, 0.02 percent of hydroquinone and 0.02 percent of epoxide resin curing agents, wherein the percentage sum of the ingredients is 100 percent. The grade H heat-resistance grade can be reached, i.e. the work temperature is improved from 130 DEG C to 155 DG C to 180 DEG C, the energy is saved, materials are saved, the invention is favorable for size reduction, weight reduction and material saving of mechanical and electrical products, the volatile substances are reduced by 20 to 30 percent, and the invention has the advantages of heat resistance, energy saving, environment protection and the like.

Description

A kind of heat-resistance energy-saving environment-protection epoxy solvent-free paint and working method thereof
Technical field
The present invention relates to a kind of solvent-free paint and preparation thereof, particularly a kind of heat-resistance energy-saving environment-protection epoxy solvent-free paint and working method thereof.
Background technology
Contain a large amount of solvents in traditional lacquer,, cause environmental pollution, influence user's health in a large amount of volatilizations of producing, use exists the organic aromatic solvent of objectionable impurities.Along with domestic economy is built fast development,, reduce pollution to environment in order to reduce the volatile quantity of organic aromatic solvent; According to domestic different demands, the domestic existing many enterprise production of epoxy solvent-free paint, but according to national standard; Its temperature classification major part is B, F level; Can't satisfy the needs of some particular surroundingss, therefore, become the problem of each business research for the research of protecting the ring epoxy solvent-free paint.
Summary of the invention
Defective or deficiency to above-mentioned prior art exists the objective of the invention is to, and a kind of heat-resistance energy-saving environment-protection epoxy solvent-free paint and working method thereof are provided.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of heat-resistance energy-saving environment-protection epoxy solvent-free paint is characterized in that, this heat-resistance energy-saving environment-protection epoxy solvent-free paint that makes is made up of following raw materials by weight: heat-resistant polyester: 40~50%; Modified epoxy: 8~10%; Tong ma anhydride: 10~12%, Vinyl toluene: 30~40%, Di Cumyl Peroxide 99: 1~1.5%; Resorcinol: 0.02%, epoxy curing agent: 0.02%; The per-cent sum of above-mentioned raw materials is 100%.
Described modified epoxy is formulated by weight 9:1 or 10:1 by E-44 epoxy resin and bismaleimides.
Described tong ma anhydride is made up of tung oil acid anhydride, MALEIC ANHYDRIDE and bismaleimides, and its weight ratio prescription is: tung oil: 66.18%, and MALEIC ANHYDRIDE: 14.72%, bismaleimides: 19%.
The working method of above-mentioned heat-resistance energy-saving environment-protection epoxy solvent-free paint is characterized in that, comprises the following steps:
1) with bisphenol A epoxide resin with bi-maleimide modified one-tenth modified epoxy; This modified epoxy is formulated by weight 9:1 or 10:1 by E-44 epoxy resin and bismaleimides; The method of concrete modification is: E-44 epoxy resin is warmed up to 135 ℃~140 ℃ heating and melting, slowly adds bismaleimides then, insulation 2h; After treating that material is transparent, cooling promptly obtains modified epoxy;
2) become tong ma anhydride with bi-maleimide modified tung oil acid anhydride, this tong ma anhydride is made up of tung oil, MALEIC ANHYDRIDE and bismaleimides, and its weight ratio prescription is: tung oil: 66.18%, and MALEIC ANHYDRIDE: 14.72%, bismaleimides: 19%; The method of concrete modification is: tung oil is warming up to 90 ℃~110 ℃ dewaters, insulation 0.5~1h is cooled to 80 ℃ after dewatering, add MALEIC ANHYDRIDE; Be warming up to 140 ℃, insulation 0.5h slowly adds bismaleimides then, treat that bismaleimides adds after; Be warming up to 200 ± 2 ℃ with 5 ℃/min, insulation 1h, pocket knife method 2min~3min; The cooling cooling discharging is for use, and the cooling back keeps material transparent, reacts transparent to material again otherwise temperature is risen to 140 ℃;
3) get heat-resistant polyester by weight percentage: 40~50%, modified epoxy: 8~10%, tong ma anhydride: 10~12%; Vinyl toluene: 30~40%, Di Cumyl Peroxide 99: 1~1.5%, Resorcinol: 0.02%; Epoxy curing agent: 0.02%, put into reaction kettle, mix 1h~1.5h under the room temperature; The assurance mixing of materials is even, filters, and packing promptly gets heat-resistance energy-saving environment-protection epoxy solvent-free paint.
The present invention has introduced heat-stable bismaleimides and heat-resistant polyester collocation, and the heat-resistance energy-saving environment-protection epoxy solvent-free paint that obtains can reach H level temperature classification; Be that working temperature rises to 180 ℃, conserve energy, economical with materials by 130 ℃~155 ℃; Help the electronic product reduced volume; Weight reduction and economical with materials, volatile matter reduce 20~30%, have advantages such as heat-resisting, energy-saving and environmental protection.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed description.
1) modified epoxy preparation
By weight getting 1 part of 9 parts of raw material E-44 epoxy resin (or CYD-128 epoxy resin) and bismaleimides; E-44 epoxy resin is heated to 130 ℃~140 ℃, slowly adds bismaleimides, 2-3h is transparent to material in insulation; Stop heating, cool off subsequent use.
2) tong ma anhydride preparation
Get tung oil by weight percentage: 66.18%, MALEIC ANHYDRIDE: 14.72%, bismaleimides: 19%, tung oil is warming up to 90-110 ℃ dewaters; Insulation 0.5h-1h reduces to 80 ℃ and adds MALEIC ANHYDRIDE after dewatering, heat up 140 ℃; Insulation 0.5h slowly adds bismaleimides then, treat that bismaleimides adds after; Be warming up to 200 ± 2 ℃ with 5 ℃/min, insulation 1h, pocket knife method 2-3min; The cooling cooling discharging is for use, and the cooling back keeps material transparent, reacts transparent to material again otherwise temperature is risen to 140 ℃.
3) preparation of heat-resistance energy-saving environment-protection epoxy solvent-free paint
Get heat-resistant polyester by weight percentage: 40~50%, modified epoxy: 8~10%, tong ma anhydride: 10~12%; Vinyl toluene: 30~40%, Di Cumyl Peroxide 99: 1~1.5%, Resorcinol: 0.02%; Epoxy curing agent: 0.02%, put into reaction kettle, mix 1h~1.5h under the room temperature; The assurance mixing of materials is even, filters, and packing promptly gets heat-resistance energy-saving environment-protection epoxy solvent-free paint.
Preparation embodiment 1:
Get raw material E-44 epoxy resin 900kg, bismaleimides 100kg is heated to 135 ± 5 ℃ with raw material E-44 epoxy resin, slowly adds bismaleimides, insulation 2.5h, and material to be taken a sample is transparent, stops heating, cooling.
Get tung oil 661.8kg, MALEIC ANHYDRIDE 147.2kg, bismaleimides 190kg is warming up to 100 ± 5 ℃ with tung oil earlier and dewaters; Under this temperature, be incubated 1h, cool the temperature to 80 ℃ after dewatering, add MALEIC ANHYDRIDE, heat up 140 ℃ then; Insulation 0.5h slowly adds bismaleimides under this temperature, treat that bismaleimides adds after, with 5 ℃/min temperature rise rate to 200 ± 2 ℃; Insulation 1h, behind the pocket knife method 2-3min with routine, the cooling cooling discharging, cooling back material is transparent.
Get raw material heat-resistant polyester 400kg, modified epoxy 100kg, tong ma anhydride 100kg; Vinyl toluene 300kg, Di Cumyl Peroxide 99 15kg, Resorcinol 2kg; Epoxy curing agent 2kg; Put into reaction kettle, the method with routine under the room temperature is mixed 1h~1.5h, makes the material thorough mixing even; To material filtering, packing promptly gets product then.
Preparation embodiment 2:
Different is for present embodiment and embodiment 1; Change raw material E-44 epoxy resin into CYD-128 epoxy resin, and the weight ratio of CYD-128 epoxy resin and bismaleimides prepares according to 10:1, i.e. CYD-128 epoxy resin 1000kg; Bismaleimides 100kg, all the other are all with embodiment 1.
Preparation embodiment 3:
Different is for present embodiment and embodiment 1, and the add-on of heat-resistant polyester is 500kg, and the add-on of modified epoxy is 80kg, and all the other are with equal embodiment 1.
4) inspection after construction
Outward appearance: orange-yellow transparent liquid
Granularity: 20 ± 2 ℃ of big 4 flow cups, 20~40 seconds
Set time: 140 ℃ ± 2 ℃<60min
Electrical strength: normality>22kv/mm
180℃±2℃ >16kv/mm
Immersion 24h>20 kv/mm
Volume specific resistance: normality>1 * 10 12(Ω m)
Immersion 24h>1 * 10 10(Ω m)
180℃±2℃?>1×10 8(Ω·m)
Cohesive force: normality>100N,
TI>180.
The heat-resistance energy-saving environment-protection epoxy solvent-free paint that the present invention makes; Be H level temperature classification; Be that working temperature rises to 180 ℃ by 130 ℃~155 ℃, solidification value is low 10 ℃~20 ℃ of a H level solvent-free paint than general temperature classification, through U.S. UL authentication; The TI of product reaches 184 ℃, and enough nargin is arranged.

Claims (2)

1. the working method of a heat-resistance energy-saving environment-protection epoxy solvent-free paint is characterized in that, comprises the following steps:
1) with bisphenol A epoxide resin with bi-maleimide modified one-tenth modified epoxy; This modified epoxy is formulated by weight 9:1 or 10:1 by E-44 epoxy resin and bismaleimides; The method of concrete modification is: E-44 epoxy resin is warmed up to 135 ℃~140 ℃ heating and melting, slowly adds bismaleimides then, insulation 2h; After treating that material is transparent, cooling promptly obtains modified epoxy;
2) become tong ma anhydride with bi-maleimide modified tung oil acid anhydride, this tong ma anhydride is made by tung oil, MALEIC ANHYDRIDE and bismaleimides, and its weight ratio prescription is: tung oil: 66.18%, and MALEIC ANHYDRIDE: 14.72%, bismaleimides: 19%; The method of concrete modification is: tung oil is warming up to 90 ℃~110 ℃ dewaters, insulation 0.5~1h is cooled to 80 ℃ after dewatering, add MALEIC ANHYDRIDE; Be warming up to 140 ℃, insulation 0.5h slowly adds bismaleimides then, treat that bismaleimides adds after; Be warming up to 200 ± 2 ℃ with 5 ℃/min, insulation 1h, pocket knife method 2min~3min; The cooling cooling discharging is for use, and the cooling back keeps material transparent, reacts transparent to material again otherwise temperature is risen to 140 ℃;
3) get heat-resistant polyester by weight percentage: 40~50%, modified epoxy: 8~10%, tong ma anhydride: 10~12%, Vinyl toluene: 30~40%; Di Cumyl Peroxide 99: 1~1.5%, Resorcinol: 0.02%, epoxy curing agent: 0.02%; The per-cent sum of above-mentioned raw materials is 100%, puts into reaction kettle, mixes 1h~1.5h under the room temperature; The assurance mixing of materials is even, filters, and packing promptly gets heat-resistance energy-saving environment-protection epoxy solvent-free paint.
2. the heat-resistance energy-saving environment-protection epoxy solvent-free paint of the said method of claim 1 preparation.
CN201010168553XA 2010-05-11 2010-05-11 Heat-resistance energy-saving environment-protection epoxy solvent-free paint and production method thereof Expired - Fee Related CN101805533B (en)

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CN103122190B (en) * 2013-02-01 2015-01-07 陕西宏业电工电子新材料有限公司 Class-H insulation dry-type air-core reactor wire epoxy polyester low-solvent bonding paint and production method thereof
CN104112554B (en) * 2014-07-21 2016-06-29 固德电材系统(苏州)股份有限公司 The preparation method of the high-performance cloud master tape that a kind of belting machine uses

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CN101157817A (en) * 2007-10-22 2008-04-09 苏州巨峰绝缘材料有限公司 B. F-grade general epoxy less-solvent insulating impregnating varnish and preparation method thereof
CN100453578C (en) * 2006-05-12 2009-01-21 吴江市太湖绝缘材料厂 Solvent-free impregnating insulating paint

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CN1040383A (en) * 1989-08-16 1990-03-14 东方绝缘材料厂 Resins without solvent dipping
CN100453578C (en) * 2006-05-12 2009-01-21 吴江市太湖绝缘材料厂 Solvent-free impregnating insulating paint
CN101157817A (en) * 2007-10-22 2008-04-09 苏州巨峰绝缘材料有限公司 B. F-grade general epoxy less-solvent insulating impregnating varnish and preparation method thereof

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