CN116218147A - Modified epoxy resin composition with low heat release - Google Patents
Modified epoxy resin composition with low heat release Download PDFInfo
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- CN116218147A CN116218147A CN202211655247.8A CN202211655247A CN116218147A CN 116218147 A CN116218147 A CN 116218147A CN 202211655247 A CN202211655247 A CN 202211655247A CN 116218147 A CN116218147 A CN 116218147A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5026—Amines cycloaliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a modified epoxy resin composition with low heat release, which comprises a component A and a component B and is characterized in that: the component A comprises the following components in parts by weight: 75-85 parts of epoxy resin, 5-13 parts of modified epoxy resin, 8-12 parts of diluent and 1 part of coupling agent A187; the component B comprises: 30-50 parts of alicyclic amine curing agent and 50-70 parts of polyether amine curing agent. The invention provides a modified epoxy resin composition with low heat release, wherein isocyanate modified epoxy resin is added in the composition, so that the toughness of the epoxy resin composition is enhanced, the shrinkage rate is reduced, the heat release amount of the epoxy resin composition is reduced, the heat release temperature is reduced, and the problem of pain points in the process of accelerating blades is solved.
Description
Technical Field
The invention belongs to the technical field of vacuum infusion resins for wind power generation blades, and particularly relates to a modified epoxy resin composition with low heat release.
Background
With the increasing severity of environmental pollution, green energy is becoming the subject of pursuing energy development all over the world. Under the aim of double carbon, the consumption of renewable energy sources worldwide is increased at a high speed, and the 2021 year is increased by more than 15 percent in a same way. In the new energy era, china is a main contribution country of renewable energy. In 2021, the global renewable energy source total newly-installed 257GW, i have a ratio of nearly half in China, and 121GW is newly-installed. The global energy is irreversibly transformed to green low carbon, and new energy is already the main battlefield of a new industrial revolution.
The wind power blade is used as a key component of a wind power generation system, directly influences the performance of the whole system, and is composed of resin and fiber. Resin manufacturers continuously research the epoxy resin for wind power blades, for example, chinese patent CN 110564110A describes an epoxy resin composition suitable for a vacuum infusion process and a preparation method thereof, wherein the epoxy resin composition A consists of bisphenol A epoxy resin, a mixture of 1, 4-butanediol diglycidyl ether and bisphenol F epoxy resin, and the curing agent B consists of polyether amine, alicyclic amine and tertiary amine accelerators, and has the characteristics of low viscosity and good mechanical property; chinese patent CN112029237 describes an epoxy resin composition suitable for vacuum infusion process and a method for preparing the same, wherein the epoxy resin composition a is composed of bisphenol a epoxy resin, 1, 6-hexanediol diglycidyl ether and bisphenol F epoxy resin blend, and the curing agent B is composed of polyetheramine, dimethyl dipropyltriamine and coupling agent, and has the characteristics of good bonding force with fibers, excellent mechanical properties and long operation time; chinese patent CN101735564 describes a vacuum infusion resin for wind turbine blades and a method for preparing the same, wherein the epoxy composition a is composed of bisphenol a epoxy resin, an organosilicon modified epoxy resin, a diluent, a defoamer, a coupling agent blend, and the curing agent B is composed of alicyclic amine, aliphatic polyamine, an accelerator and a dye, and has the characteristics of stronger toughness, excellent water resistance, excellent temperature resistance, excellent wettability and longer operation time; chinese patent CN200910201435 describes a vacuum infusion resin for megawatt wind power blades and a method for preparing the same, wherein the epoxy composition a is composed of a bisphenol a epoxy resin, triglycidyl-para-aminophenol (AFG-90) trifunctional epoxy, 4, 5-epoxycyclohexyl-1, 2-dicarboxyiate diglycidyl ester (TDE-85) and a diluent polyol glycidyl ether blend, and the curing agent B is composed of alicyclic amine, aliphatic amine, having the characteristics of low viscosity and high toughness; chinese patent CN102702686a describes an epoxy resin system for producing megawatt wind turbine blades and a method for preparing the same, wherein the epoxy composition a is composed of a blend of bisphenol a epoxy resin, bisphenol F epoxy resin, low viscosity sea weed epoxy resin, diluent, thixotropic agent, functional auxiliary agent and the like, and the curing agent B is composed of alicyclic amine, aliphatic amine and aromatic amine, functional auxiliary agent, shaking agent and pigment, and has the characteristics of fast reaction speed and good wettability to fibers; chinese patent CN103694637 describes a high-toughness vacuum slow-speed epoxy resin for wind power blade and its preparation method, wherein the epoxy composition a is composed of epoxy resin, vinyl end-capped epoxy polyether, reactive diluent, coupling agent, defoamer blend, and the curing agent B is composed of one or two mixtures of aliphatic amine, alicyclic amine, aromatic amine, with better mechanical properties; with the arrival of wind power subsidy time ending and wind power flat-price Internet surfing time, continuous cost reduction and synergy become important issues in blade manufacture. In order to improve the utilization rate of the blade mold, increase the production efficiency and reduce the cost, a blade company improves the efficiency of manufacturing the blade by improving the curing temperature of the mold, but the blade company can cause a large amount of heat in the resin curing process, so that quality problems such as shell whitening, main beam swelling, local blackening of core materials and the like are caused. Therefore, in order to solve the problem of local defects caused by resin heat release in the process of wind power blade manufacturing acceleration, the patent intervenes from the aspect of a resin matrix, and a modified epoxy resin composition with low heat release is prepared.
Disclosure of Invention
The present invention aims to solve at least one of the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a modified epoxy resin composition having a low exotherm, comprising a component a and a component B, the component a comprising, in parts by weight: 75-85 parts of epoxy resin, 5-13 parts of modified epoxy resin, 8-12 parts of diluent and 1 part of coupling agent A187; the component B comprises: 30-50 parts of alicyclic amine curing agent and 50-70 parts of polyether amine curing agent.
Preferably, the modified epoxy resin is an isocyanate modified epoxy resin comprising one or more compounds having the following structure:
rn2 in the compound is selected from alkyl with 1-6 carbon atoms, and Rn1 in the compound is selected from one of toluene, isophorone, diphenylmethane, dicyclohexylmethane, hexamethylene and lysine.
Preferably, rn2 is an alkyl group of 4 carbon atoms and Rn1 is hexamethylene.
Preferably, the preparation method of the modified epoxy resin comprises the following specific steps: adding epoxy resin into a rotary stirrer, adding 0.1-0.3 part of triphenylphosphine catalyst, raising the temperature to 140 ℃, slowly dripping isocyanate into the stirrer by using a dripping device, maintaining the temperature at 135-145 ℃ after dripping, keeping the rotating speed at 800-1300r/min, and continuously stirring for 3-5h.
Preferably, the diluent is an epoxy reactive diluent selected from one or more of 1, 4-butanediol diglycidyl ether (XY 622), 1, 6-hexanediol diglycidyl ether, polyethylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether, p-tert-butyl glycidyl ether, n-butyl glycidyl ether, carbon dodecyl to tetradecyl glycidyl ether (XY 748), octyl glycidyl ether, butyl glycidyl ether.
Preferably, the diluent is carbon twelve to fourteen glycidyl ether (XY 748).
Preferably, the epoxy resin is a mixture of one or more of bisphenol a type epoxy resins (128 bisphenol a type epoxy resins, 6010 bisphenol a type epoxy resins, 127 bisphenol a type epoxy resins), 170 bisphenol F type epoxy resins.
Preferably, the epoxy resin is 127 bisphenol a epoxy resin.
Preferably, the polyether amine curing agent is selected from one or more of T403 polyether amine, D400 polyether amine, D230 polyether amine, D2000 polyether amine, T5000 polyether amine.
Preferably, the polyether amine curing agent is a combination of D230 polyether amine and D400 polyether amine.
Preferably, the alicyclic amine curing agent is selected from one or more of menthanediamine, 1, 2-cyclohexanediamine, 1, 3-cyclohexanediamine, methylcyclopentylenediamine, isophoronediamine.
Compared with the prior art, the invention at least comprises the following beneficial effects:
the invention provides a modified epoxy resin composition with low heat release, wherein isocyanate modified epoxy resin is added in the composition, so that the toughness of the epoxy resin composition is enhanced, the shrinkage rate is reduced, and the heat release amount of the epoxy resin composition is reduced, thereby reducing the heat release temperature and solving the problem of pain points caused by resin heat release in the process of manufacturing wind power blades.
Additional features and advantages of the disclosure will be set forth in the description which follows, or in part will be obvious from the description, or may be learned by practice of the techniques of the disclosure.
The specific embodiment is as follows:
the following describes in more detail the embodiments of the present invention in terms of several specific examples.
Example 1:
a preparation method for preparing isocyanate modified epoxy resin comprises the following specific steps:
100 parts of 127 bisphenol A epoxy resin is put into a rotary stirrer in parts by weight, 0.2 part of triphenylphosphine catalyst is added, the temperature is raised to 140 ℃, 50 parts of hexamethylene diisocyanate is slowly dripped into the stirrer by using a dripping device, the temperature is kept at 140 ℃ after the dripping is finished, the rotating speed is 1000r/min, and the stirring is carried out for 4 hours, wherein the reaction process is as follows:
wherein Rn2 is alkyl of 4 carbon atoms and Rn1 is hexamethylene.
A modified epoxy resin composition with low heat release and a preparation method thereof are specifically as follows:
s1, preparing a component A, namely weighing 9 parts by weight of isocyanate modified epoxy resin, 80 parts by weight of bisphenol A epoxy resin (127), 10 parts by weight of 1, 4-butanediol glycidyl ether and 1 part by weight of silane coupling agent (A187), putting the components into a reaction kettle, heating to 60-80 ℃, and stirring for 4 hours; then the mixture is put into a packaging barrel for sealing and preservation.
S3, preparing a component B, namely weighing 65 parts by weight of polyether amine with the molecular weight of 230 and 35 parts by weight of isophorone diamine, putting into a reaction kettle, heating to 40-60 ℃, stirring for 3 hours, and cooling; packaging into packaging barrel, and sealing for storage.
Example 2:
the preparation methods of the modified epoxy resin, the component A and the component B are the same as in the example 1, wherein the raw materials of the component A are as follows: 11 parts of isocyanate modified epoxy resin, 80 parts of bisphenol A epoxy resin, 8 parts of C12-C14 diglycidyl ether and 1 part of silane coupling agent (A187); the raw materials of the component B are as follows: the polyether amine with the molecular weight of 230 is 68 parts by weight and isophorone diamine is 32 parts by weight.
Example 3
The preparation methods of the modified epoxy resin, the component A and the component B are the same as in the example 1, wherein the raw materials of the component A are as follows: 13 parts of isocyanate modified epoxy resin, 76 parts of bisphenol A epoxy resin (127), 10 parts of C12-C14 diglycidyl ether and 1 part of silane coupling agent (A187); the raw materials of the component B are as follows: 62 parts of polyether amine with the molecular weight of 230 and 38 parts of isophorone diamine.
Example 4
The preparation methods of the modified epoxy resin, the component A and the component B are the same as in the example 1, wherein the raw materials of the component A are as follows: 7 parts of isocyanate modified epoxy resin, 80 parts of bisphenol A epoxy resin (127), 12 parts of C12-C14 diglycidyl ether and 1 part of silane coupling agent (A187); the raw materials of the component B are as follows: 60 parts of polyetheramine with the molecular weight of 230 and 40 parts of isophorone diamine.
Example 5
The preparation methods of the modified epoxy resin, the component A and the component B are the same as in the example 1, wherein the raw materials of the component A are as follows: the epoxy resin comprises, by weight, 5 parts of isocyanate modified epoxy, 83 parts of bisphenol A epoxy resin (127), 11 parts of C12-C14 diglycidyl ether and 1 part of silane coupling agent (A187). The raw materials of the component B are as follows: 70 parts of polyether amine with the molecular weight of 230 and 30 parts of isophorone diamine.
Example 6
The preparation methods of the modified epoxy resin, the component A and the component B are the same as in the example 1, wherein the raw materials of the component A are as follows: 9 parts of isocyanate modified epoxy, 80 parts of bisphenol F epoxy resin (127), 10 parts of 1, 6-hexanediol diglycidyl ether and 1 part of silane coupling agent (A187); the raw materials of the component B are as follows: the polyether amine with the molecular weight of 230 is 65 parts by weight and isophorone diamine is 35 parts by weight.
Example 7
The preparation methods of the modified epoxy resin, the component A and the component B are the same as in the example 1, wherein the raw materials of the component A are as follows: 11 parts of isocyanate modified epoxy, 78 parts of bisphenol A epoxy resin (127), 10 parts of C12-C14 diglycidyl ether and 1 part of silane coupling agent (A187); the raw material of the component B comprises, by weight, 65 parts of polyether amine with a molecular weight of 230 and 35 parts of isophorone diamine.
Example 8
The preparation methods of the modified epoxy resin, the component A and the component B are the same as in the example 1, wherein the raw materials of the component A are as follows: 11 parts of isocyanate modified epoxy, 78 parts of bisphenol A epoxy resin (127), 10 parts of C12-C14 diglycidyl ether and 1 part of silane coupling agent (A187); the preparation of the component B comprises the following raw materials in parts by weight: 68 parts of polyetheramine with a molecular weight of 230 and 32 parts of isophorone diamine.
Example 9
The preparation methods of the modified epoxy resin, the component A and the component B are the same as in the example 1, wherein the raw materials of the component A are as follows: 11 parts of isocyanate modified epoxy, 78 parts of bisphenol A epoxy resin (127), 10 parts of C12-C14 diglycidyl ether and 1 part of silane coupling agent (A187); the raw materials of the component B are as follows: 60 parts of polyetheramine with the molecular weight of 230 and 40 parts of isophorone diamine.
Example 10
The preparation methods of the modified epoxy resin, the component A and the component B are the same as in the example 1, wherein the raw materials of the component A are as follows: 11 parts of isocyanate modified epoxy, 78 parts of bisphenol A epoxy resin (127), 10 parts of C12-C14 diglycidyl ether and 1 part of silane coupling agent (A187). The raw materials of the component B are as follows: 70 parts of polyether amine with the molecular weight of 230 and 30 parts of isophorone diamine.
Comparative example 1
The preparation method of the component A and the component B is the same as in the example 1, wherein the raw materials of the component A are as follows: 88 parts of bisphenol A epoxy resin (127), 11 parts of C12-C14 diglycidyl ether and 1 part of silane coupling agent (A187). The raw materials of the component B are as follows: 60 parts of polyetheramine with the molecular weight of 230 and 40 parts of isophorone diamine.
Comparative example 2
The preparation method of the component A and the component B is the same as in the example 1, wherein the raw materials of the component A are as follows: 88 parts of bisphenol A epoxy resin (127), 11 parts of C12-C14 diglycidyl ether and 1 part of silane coupling agent (A187). The raw materials of the component B are as follows: 80 parts of polyetheramine with the molecular weight of 230 and 20 parts of isophorone diamine.
Performance test: resin samples were prepared and tested for relevant properties in the following steps for examples 1,2, 6, 8, 9 and comparative examples 1,2, the results being entered into table 1: 1) And (3) a component A: mixing the components B according to the weight ratio of 100:28, stirring for 4-6 minutes, observing whether stirring is uniform, if no filiform substances appear, namely, stirring uniformly, and if so, continuing stirring until stirring uniformly; 2) The stirred resin was subjected to a mixed viscosity test (according to standard GB/T22314), 100 parts were subjected to a 50 ℃ water bath exothermic comparative exothermic test (according to standard ASTM D2471), the remaining 400 parts were placed in a vacuum oven for bubble removal treatment, the bubble-removed resin was poured into a mold, post-cured according to a curing schedule of 25 ℃/24h to 70 ℃/8h, and then subjected to a cut-to-sample test mechanics (according to standard ISO 527-2), glass transition temperature (Tg) (according to GB/T19466.2), cure shrinkage (according to standard ISO-3521), and the like.
Table 1 list of properties for some of the examples and comparative examples
From the above experimental data, it can be seen that: the low-heat-release modified epoxy composition obtained by the invention has excellent performance, reduces the volume shrinkage rate of the cured resin while providing low heat release performance, and maintains good mechanical properties of the cured product.
The above process scale is intended to simplify the description of the present invention and applications, modifications and variations of the present invention will be apparent to those skilled in the art.
Although embodiments of the present invention have been disclosed above, it is not limited to the use of the description and embodiments, it is well suited to various fields of use for the invention, and further modifications may be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the particular details without departing from the general concepts defined in the claims and the equivalents thereof.
Claims (10)
1. A modified epoxy resin composition with low heat release, which is characterized by comprising a component A and a component B, and is characterized in that: the component A comprises the following components in parts by weight: 75-85 parts of epoxy resin, 5-13 parts of modified epoxy resin, 8-12 parts of diluent and 1 part of coupling agent A187; the component B comprises: 30-50 parts of alicyclic amine curing agent and 50-70 parts of polyether amine curing agent.
2. The low exotherm modified epoxy resin composition of claim 1, wherein the modified epoxy resin is an isocyanate modified epoxy resin comprising one or more compounds having the structure:
rn2 in the compound is selected from alkyl with 1-6 carbon atoms, and Rn1 in the compound is selected from one of tolyl, isophorone group, methyldiphenyl, methyldicyclohexyl, hexamethylene and lysine group.
3. The modified epoxy resin composition of claim 2, wherein Rn2 is an alkyl group of 4 carbon atoms and Rn1 is hexamethylene.
4. The modified epoxy resin composition of claim 1, wherein the diluent is an epoxy reactive diluent selected from one or more of 1, 4-butanediol diglycidyl ether (XY 622), 1, 6-hexanediol diglycidyl ether, polyethylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether, p-t-butyl glycidyl ether, n-butyl glycidyl ether, carbon twelve to tetradecyl glycidyl ether (XY 748), octyl glycidyl ether, butyl glycidyl ether.
5. The low exotherm modified epoxy resin composition of claim 4, wherein the diluent is a carbon twelve to tetradecyl glycidyl ether (XY 748).
6. The modified epoxy resin composition of claim 1, wherein the epoxy resin is a mixture of one or more of 128 bisphenol a type epoxy resin, 6010 bisphenol a type epoxy resin, 127 bisphenol a type epoxy resin, 170 bisphenol F type epoxy resin.
7. The modified epoxy resin composition of claim 6, wherein said epoxy resin is 127 bisphenol a type epoxy resin.
8. The modified epoxy resin composition of claim 1, wherein said polyether amine curing agent is selected from one or more of T403 polyether amine, D400 polyether amine, D230 polyether amine, D2000 polyether amine, T5000 polyether amine.
9. The modified epoxy resin composition of claim 1, wherein the cycloaliphatic amine curing agent is one or more of menthane diamine, 1, 2-cyclohexane diamine, 1, 3-cyclohexane diamine, methylcyclopentane diamine, isophorone diamine.
10. The modified epoxy resin composition with low heat release according to any one of claims 1 to 9, wherein the modified epoxy resin is prepared by the following steps: adding epoxy resin into a rotary stirrer, adding a certain amount of triphenylphosphine catalyst, raising the temperature to 135-145 ℃, slowly dripping isocyanate into the stirrer by using a dripping device, maintaining the temperature to 135-145 ℃ after dripping, and continuously stirring for 3-5h at the rotating speed of 800-1300 r/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117264176A (en) * | 2023-10-23 | 2023-12-22 | 四川东树新材料有限公司 | Hyperbranched modified amine hand paste epoxy resin composition and preparation method thereof |
| CN117362598A (en) * | 2023-11-09 | 2024-01-09 | 四川东树新材料有限公司 | Epoxy resin composition with low viscosity, high strength and difficult crystallization |
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2022
- 2022-12-22 CN CN202211655247.8A patent/CN116218147A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117264176A (en) * | 2023-10-23 | 2023-12-22 | 四川东树新材料有限公司 | Hyperbranched modified amine hand paste epoxy resin composition and preparation method thereof |
| CN117362598A (en) * | 2023-11-09 | 2024-01-09 | 四川东树新材料有限公司 | Epoxy resin composition with low viscosity, high strength and difficult crystallization |
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