CN106987094A - A kind of epoxy-resin systems and preparation method thereof - Google Patents
A kind of epoxy-resin systems and preparation method thereof Download PDFInfo
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- CN106987094A CN106987094A CN201710212890.6A CN201710212890A CN106987094A CN 106987094 A CN106987094 A CN 106987094A CN 201710212890 A CN201710212890 A CN 201710212890A CN 106987094 A CN106987094 A CN 106987094A
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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
-
- 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
-
- 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
- C08G59/5046—Amines heterocyclic
- C08G59/5053—Amines heterocyclic containing only nitrogen as a heteroatom
- C08G59/506—Amines heterocyclic containing only nitrogen as a heteroatom having one nitrogen atom in the ring
-
- 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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
Abstract
The present invention relates to epoxy resin production field, more particularly to a kind of epoxy-resin systems and preparation method thereof, the epoxy-resin systems are prepared from the following raw materials in parts by weight：85 95 parts of bisphenol f type epoxy resin, 0 10 parts of bisphenol A type epoxy resin, 05 parts of toughener, 57 parts of latent curing agent, 13 parts of accelerator.The preparation method of the present invention is simple, and operation is simple, scientific strong, it is adaptable to industrialized production.
Description
Technical field
The present invention relates to epoxy resin production field, more particularly to a kind of epoxy-resin systems and preparation method thereof.
Background technology
Pultrusion and it is Wrapping formed in, what is used mostly is unsaturated polyester resin, accounts for more than the 90% of resin demand,
But the pouring piece of unsaturated-resin can produce contraction after the setting, and some viscous hands are understood on surface, at this moment due to inside
Through solidification, it is therefore necessary to repairing type of polishing and polishing, in addition unsaturated-resin also has different degrees of stimulation nature and flavor
Road.And there is good physics, chemical property using epoxy resin cure product, it to metal and nonmetallic materials surface tool
There is excellent adhesive strength, dielectric properties are good, and shrinkage factor is small, and product size stability is good, and hardness is high, and pliability is preferably, right
Alkali and most of solvent-stable, and preferable surface smoothness is had using the object made by epoxy resin, it is solidifying in cast
Gu after, sanding and polishing can not obtain preferable effect yet.
The content of the invention
The problem of existing for prior art and the huge vacancy of in the market, it is an object of the invention to provide a kind of epoxy
Resin system and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of epoxy-resin systems, are prepared from the following raw materials in parts by weight：
85-95 parts of bisphenol f type epoxy resin, 0-10 parts of bisphenol A type epoxy resin, 0-5 parts of toughener, latent curing agent 5-7
Part, 1-3 parts of accelerator.
It is preferred that, the toughener is polysulfides, polyalcohols, polymer elastomer, polyurethane elastomer, thermoplastic resin
One or more in fat, heat property liquid crystal polymer processed, dissaving polymer, silsesquioxane, nano silicon.
It is preferred that, the latent curing agent is imidazoles, dicyandiamide, cyanoguanidine derivative, organic acid hydrazides, borontrifluoride
Boron-amine complex, diaminomaleonitrile, diaminomaleonitrile derivative, complex compound, the amine of many ammonium salts and aromatic amine and inorganic salts
Aminimide and super one kind being coordinated in the complex of silicate, molecular sieve blocked curing agent, microencapsulation curing agent
Or it is several.
It is preferred that, the accelerator is tertiary amine, tertiary ammonium salt, acetyl acetone salt, triphenylphosphine, triphenylphosphine salt, virtue
In the addition product of based isocyanate, organic carboxylate, organic carboxyl acid salt complex, thiocarbamide, thiourea derivative, titanate esters accelerator
One or more.
It is preferred that, the epoxide equivalent of the bisphenol f type epoxy resin is 50-1000g/mol, and viscosity is at 25 DEG C
200cps-10000cps；More preferred, the epoxide equivalent of bisphenol f type epoxy resin is 100-300g/mol, viscosity at 25 DEG C
For 500cps-5000cps.
It is preferred that, the epoxide equivalent of the bisphenol A type epoxy resin is 50-1000g/mol, and viscosity is at 25 DEG C
200cps-10000cps；More preferred, the epoxide equivalent of bisphenol A type epoxy resin is 100-300g/mol, viscosity at 25 DEG C
For 500cps-5000cps.
The preparation method of above-mentioned epoxy-resin systems, comprises the following steps：
（1）By bisphenol f type epoxy resin, bisphenol A type epoxy resin and toughener Hybrid Heating to 80 DEG C -90 DEG C, in heating
Stirring, until obtaining bright liquid, is then cooled to room temperature standby；
（2）Latent curing agent and accelerator are added to step（1）In gained liquid, then stirred with high speed dispersion dish, directly
Exist to no powder, and be not greater than 1mm particle and exist；
（3）Use grinder grinding steps（2）Gained liquid for several times, obtains final products, i.e. epoxy-resin systems.
Its preferred technical scheme is：
Step（3）In, grinder is three-roll grinder, and grinding number of times is no less than three times.
Step（3）In, the epoxy-resin systems finally given viscosity at 25 DEG C is less than 3000cps.
The preparation method of the epoxy-resin systems of the present invention adjusts composite epoxy resin from bisphenol A type epoxy resin
Viscosity, while the toughness of solidfied material can be increased；Increase the impact resistance of the toughness reinforcing material of solidfied material from toughener；
From latent curing agent and accelerator as the curing agent of whole resin system, the curing reaction temperature of resin system can be made
Reduction, realizes rapid curing, to meet pultrude process and winding process application.
The epoxy-resin systems solidification prepared by the inventive method is subjected to performance detection, method is：It is final by what is obtained
Product is incubated 4-5h at a temperature of 70 DEG C -80 DEG C, is then incubated 1h again at a temperature of 120 DEG C, finally at a temperature of 150 DEG C
30min is incubated, the epoxy resin solidified, epoxy resin its tensile strength after solidification reaches 60-80MPa, stretch modulus
For 3-4GPa, elongation at break 2-3%, bending strength is 100-120MPa, and bending modulus is 3-4GPa, heat distortion temperature ＞ 110
DEG C, curing degree ＞ 98%, density is（1.2-1.4）g/cm3, its performance can meet pultrude process and winding process to resin property
Requirement, Solidified enzyme can meet requirement of most of product to Properties of Epoxy Resin, be with a wide range of applications, and
The preparation method of the present invention is simple, and operation is simple, scientific strong, it is adaptable to industrialized production.
Embodiment
Specific embodiment of the invention given below is, it is necessary to which explanation is that the invention is not limited in implement in detail below
Example, all equivalents done on the basis of technical scheme each fall within protection scope of the present invention.
Embodiment 1：
The preparation methods of epoxy-resin systems is through the following steps that realize：
（1）85-95 parts of bisphenol f type epoxy resins, 0-10 parts of bisphenol A type epoxy resins and 0-5 parts of toughener are mixed by weight
Conjunction is heated to 80 DEG C -90 DEG C, heats while stirring, until obtaining bright liquid, is then cooled to room temperature standby；
（2）5-7 parts of latent curing agents and 1-2 parts of accelerator are added to step by weight（1）In gained liquid, Ran Houyong
High speed dispersion dish are stirred, until existing without powder, and are not greater than 1mm particle presence；
（3）Use three-roll grinder grinding steps（2）Gained liquid, at least grinds three times, obtains final products, i.e. epoxy resin body
System；
Wherein step（1）And step（2）Every part of standard of middle parts by weight is consistent.
The epoxide equivalent of the bisphenol f type epoxy resin of above-mentioned selection can be 50-1000g/mol, and viscosity is at 25 DEG C
200cps-10000cps, as the more preferred scheme of the present embodiment, the epoxide equivalent of the bisphenol f type epoxy resin of selection is
100-300g/mol, viscosity is 500cps-5000cps at 25 DEG C.
The epoxide equivalent of the bisphenol A type epoxy resin of above-mentioned selection can be 50-1000g/mol, and viscosity is at 25 DEG C
200cps-10000cps；As the more preferred scheme of the present embodiment, the epoxide equivalent of the bisphenol A type epoxy resin of selection is
100-300g/mol, viscosity is 500cps-5000cps at 25 DEG C.
Toughener is chosen as polysulfides, polyalcohols, polymer elastomer, polyurethane elastomer, thermoplastic resin, heat system
Property liquid crystal polymer, dissaving polymer, silsesquioxane, the one or more in nano silicon, the present embodiment choosing is poly-
Sulphur compound is used as toughener.
Latent curing agent is chosen as imidazoles, dicyandiamide, cyanoguanidine derivative, organic acid hydrazides, boron trifluoride-amine network
Compound, diaminomaleonitrile, diaminomaleonitrile derivative, the complex compound of many ammonium salts and aromatic amine and inorganic salts, amination acyl are sub-
Amine and the super one or more being coordinated in the complex of silicate, molecular sieve blocked curing agent, microencapsulation curing agent,
The present embodiment selects Imidazole Type Latent Curing Agent as latent curing agent.
Accelerator is chosen as tertiary amine, tertiary ammonium salt, acetyl acetone salt, triphenylphosphine, triphenylphosphine salt, aryl isocyanic acid
The addition product of ester, organic carboxylate, organic carboxyl acid salt complex, thiocarbamide, thiourea derivative, one kind in titanate esters accelerator or
Several, the present embodiment selects tertiary amine as accelerator.
The present embodiment step（3）In the obtained epoxy-resin systems viscosity at 25 DEG C be less than 3000cps.
By step（3）In obtained epoxy-resin systems solidification, curing is：By obtained epoxy-resin systems 70
4-5h is incubated at a temperature of DEG C -80 DEG C, 1h is then incubated again at a temperature of 120 DEG C, is finally incubated at a temperature of 150 DEG C
30min, the epoxy resin solidified, the tensile strength of the epoxy resin of solidification is 60-80MPa, and stretch modulus is 3-4GPa,
Elongation at break is 2-3%, and bending strength is 100-120MPa, and bending modulus is 3-4GPa, and heat distortion temperature is more than 110 DEG C, Gu
Change degree is more than 98%, and density is（1.2-1.4）g/cm3.The epoxy-resin systems prepared can meet pultrude process and winding process
Requirement to resin property, Solidified enzyme can meet requirement of most of product to Properties of Epoxy Resin, with extensive
Application value.
Embodiment 2：
Specific steps are same as Example 1, unlike：Step（1）In by weight by 88-92 parts of bisphenol f type epoxy resins,
3-8 parts of bisphenol A type epoxy resins and 1-3 parts of toughener Hybrid Heatings heat while stirring to 83 DEG C -87 DEG C, until obtaining
Bright liquid, is then cooled to room temperature standby；Toughness reinforcing is used as from polyalcohols, polymer elastomer and polyurethane elastomer mixture
Agent；Latent curing agent is used as from imidazoles and dicyandiamide mixture；Made from triphenylphosphine and triphenylphosphine salt mixture
For accelerator.
Embodiment 3：
Specific steps are same as Example 1, unlike：Step（1）In by weight by 90 parts of bisphenol f type epoxy resins, 5 parts
Bisphenol A type epoxy resin and 2 parts of toughener Hybrid Heatings heat while stirring to 85 DEG C, until obtaining bright liquid, then
It is cooled to room temperature standby；Toughener is used as from thermoplastic resin；Latent curing agent is used as from organic acid hydrazides；From having
Machine carboxylate is used as accelerator.
Embodiment 4：
Specific steps are same as Example 1, unlike：Step（2）In, 6 parts of latent curing agents and 1.5 parts of accelerator are added
Enter to step（1）In gained liquid；Toughener is used as from nano silicon；It is solid as latency from diaminomaleonitrile
Agent；Accelerator is used as from thiocarbamide.
Embodiment 5：
Specific steps are same as Example 3, unlike：Step（2）In, 6 parts of latent curing agents and 1.5 parts of accelerator are added
Enter to step（1）In gained liquid.
Embodiment 6：
Specific steps are same as Example 1, unlike：Step（2）In, 5 parts of latent curing agents and 2 parts of accelerator are added
To step（1）In gained liquid；Toughener is used as from dissaving polymer；From boron trifluoride-amine complex as latent
Property curing agent；Accelerator is used as from titanate esters accelerator.
One kind of embodiment described above, simply more preferably embodiment of the invention, those skilled in the art
The usual variations and alternatives that member is carried out in the range of technical solution of the present invention all should be comprising within the scope of the present invention.
Claims (10)
1. a kind of epoxy-resin systems, it is characterized in that：It is prepared from the following raw materials in parts by weight：Bisphenol f type epoxy resin 85-95
Part, 0-10 parts of bisphenol A type epoxy resin, 0-5 parts of toughener, 5-7 parts of latent curing agent, 1-3 parts of accelerator.
2. epoxy-resin systems according to claim 1, it is characterized in that：The toughener is polysulfides, polyalcohols, gathered
Compound elastomer, polyurethane elastomer, thermoplastic resin, heat property liquid crystal polymer processed, dissaving polymer, silsesquioxane,
One or more in nano silicon.
3. epoxy-resin systems according to claim 1, it is characterized in that：The latent curing agent is imidazoles, double cyanogen
Amine, cyanoguanidine derivative, organic acid hydrazides, boron trifluoride-amine complex, diaminomaleonitrile, diaminomaleonitrile derivative,
The complex compound of many ammonium salts and aromatic amine and inorganic salts, the complex of aminimide and super coordination silicate, molecular sieve envelope
One or more in closed form curing agent, microencapsulation curing agent.
4. epoxy-resin systems according to claim 1, it is characterized in that：The accelerator is tertiary amine, tertiary ammonium salt, levulinic
Ketone metal salt, triphenylphosphine, triphenylphosphine salt, the addition product of aromatic isocyanate, organic carboxylate, organic carboxylate complexing
One or more in thing, thiocarbamide, thiourea derivative, titanate esters accelerator.
5. epoxy-resin systems according to claim 1, it is characterized in that：The epoxide equivalent of the bisphenol f type epoxy resin
For 50-1000g/mol, viscosity is 200cps-10000cps at 25 DEG C.
6. epoxy-resin systems according to claim 1, it is characterized in that：The epoxide equivalent of the bisphenol A type epoxy resin
For 50-1000g/mol, viscosity is 200cps-10000cps at 25 DEG C.
7. the preparation method of the epoxy-resin systems according to claim any one of 1-6, it is characterized in that：Including following step
Suddenly：
（1）By bisphenol f type epoxy resin, bisphenol A type epoxy resin and toughener Hybrid Heating to 80 DEG C -90 DEG C, in heating
Stirring, until obtaining bright liquid, is then cooled to room temperature standby；
（2）Latent curing agent and accelerator are added to step（1）In gained liquid, then stirred with high speed dispersion dish, directly
Exist to no powder, and be not greater than 1mm particle and exist；
（3）Use grinder grinding steps（2）Gained liquid for several times, obtains final products.
8. the preparation method of epoxy-resin systems according to claim 7, it is characterized in that：The step（3）In, grinder
For three-roll grinder, grinding number of times is no less than three times.
9. the preparation method of epoxy-resin systems according to claim 7, it is characterized in that：The step（3）In obtain
Final products viscosity at 25 DEG C is less than 3000cps.
10. the preparation method of epoxy-resin systems according to claim 7, it is characterized in that：The step（3）In, finally
Tensile strength after product solidification is 60-80MPa, and stretch modulus is 3-4GPa, and elongation at break is 2-3%, and bending strength is
100-120MPa, bending modulus is 3-4GPa, and heat distortion temperature is more than 110 DEG C, and curing degree is more than 98%, and density is（1.2-1.4）
g/cm3。
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109135187A (en) * | 2018-07-14 | 2019-01-04 | 桂林理工大学 | A kind of preparation method of the epoxy resin toughened composite material of hybrid particle |
| CN110148509A (en) * | 2019-01-08 | 2019-08-20 | 天通控股股份有限公司 | A kind of high reliability FeSiCr integrated inductance particulate material and preparation method |
| CN111087760A (en) * | 2019-12-27 | 2020-05-01 | 北京光华纺织集团有限公司 | Epoxy resin system for wet winding and preparation method and application thereof |
| CN111116870A (en) * | 2019-12-31 | 2020-05-08 | 浙江华正新材料股份有限公司 | Latent resin composition, prepreg and epoxy composite material |
| WO2020125715A1 (en) * | 2018-12-20 | 2020-06-25 | 艾伦塔斯电气绝缘材料(珠海)有限公司 | Mono-component epoxy resin composition and preparation method therefor |
| CN111868844A (en) * | 2018-03-16 | 2020-10-30 | 亨斯迈先进材料许可(瑞士)有限公司 | Curable mixture for impregnating paper sleeves |
| CN111944271A (en) * | 2020-07-10 | 2020-11-17 | 中复碳芯电缆科技有限公司 | Low-heat-release and yellowing-resistant glass fiber reinforced plastic pultruded epoxy resin and preparation method thereof |
| CN112080108A (en) * | 2020-06-24 | 2020-12-15 | 南昌航空大学 | Preparation method of liquid polyurethane toughening modified epoxy resin system |
| CN114907548A (en) * | 2022-05-16 | 2022-08-16 | 南京海拓复合材料有限责任公司 | Epoxy resin batch for pultrusion of composite material and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111868844A (en) * | 2018-03-16 | 2020-10-30 | 亨斯迈先进材料许可(瑞士)有限公司 | Curable mixture for impregnating paper sleeves |
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| CN109135187B (en) * | 2018-07-14 | 2022-08-09 | 桂林理工大学 | Preparation method of hybrid particle toughened epoxy resin composite material |
| WO2020125715A1 (en) * | 2018-12-20 | 2020-06-25 | 艾伦塔斯电气绝缘材料(珠海)有限公司 | Mono-component epoxy resin composition and preparation method therefor |
| CN110148509A (en) * | 2019-01-08 | 2019-08-20 | 天通控股股份有限公司 | A kind of high reliability FeSiCr integrated inductance particulate material and preparation method |
| CN111087760A (en) * | 2019-12-27 | 2020-05-01 | 北京光华纺织集团有限公司 | Epoxy resin system for wet winding and preparation method and application thereof |
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| CN112080108A (en) * | 2020-06-24 | 2020-12-15 | 南昌航空大学 | Preparation method of liquid polyurethane toughening modified epoxy resin system |
| CN111944271A (en) * | 2020-07-10 | 2020-11-17 | 中复碳芯电缆科技有限公司 | Low-heat-release and yellowing-resistant glass fiber reinforced plastic pultruded epoxy resin and preparation method thereof |
| CN114907548A (en) * | 2022-05-16 | 2022-08-16 | 南京海拓复合材料有限责任公司 | Epoxy resin batch for pultrusion of composite material and preparation method thereof |
| WO2023221619A1 (en) * | 2022-05-16 | 2023-11-23 | 南京海拓复合材料有限责任公司 | Epoxy resin batch for composite material pultrusion and preparation method therefor |
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