CN105885356A - Vacuum infusion resin and preparation method and application thereof - Google Patents
Vacuum infusion resin and preparation method and application thereof Download PDFInfo
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- CN105885356A CN105885356A CN201610454389.6A CN201610454389A CN105885356A CN 105885356 A CN105885356 A CN 105885356A CN 201610454389 A CN201610454389 A CN 201610454389A CN 105885356 A CN105885356 A CN 105885356A
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- resin
- epoxy resin
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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
- C08G59/5006—Amines aliphatic
Abstract
The invention discloses vacuum infusion resin and a preparation method and application thereof. The vacuum infusion resin comprises toughening epoxy resin accounting for 50-70% of the total mass of the vacuum infusion resin and a curing agent accounting for 30-50% of the total mass of the vacuum infusion resin. The vacuum infusion resin has the advantages that the toughening epoxy resin enhances the toughness of the vacuum infusion resin and lowers the viscosity of the vacuum infusion resin, and later process operations are facilitated; tetramethyl guanidine is used as the curing agent of the toughening epoxy resin and is moderate in curing time and curing temperature, and the cured vacuum infusion resin is low in viscosity and excellent in performance; the vacuum infusion resin is low in viscosity, high in toughness, simple in preparation method and widely applicable to pouring field of medium- and high-voltage electric insulating parts and has a long working life under 40 DEG C.
Description
Technical field
The invention belongs to resin technology field, be specifically related to a kind of vacuum and import resin and preparation method thereof and answer
With.
Background technology
At present, middle pressure, insulating of electric measurement of high pressure part such as dry-type distribution transformer, support member, electric member etc. should
With extensively, these electrical insulations play the effect of electric insulation and load.Preparation at these electrical insulations
During, epoxy resin is one of important material, but, common epoxy resin viscosity is big, directly should
If middle high-pressure electrical insulations laminate makes, not only permeate difficulty, injection pressure height, mold filling
Time is long, and the bubble carried secretly in resin is difficult to eliminate.
Vacuum casting process is used to realize the epoxy resin bonding to insulating material at present.Vacuum pouring work
Skill is the Liquid molding techniques of a kind of low cost, and this technique utilizes negative pressure of vacuum effect and height on one-side mould
Permeating medium, makes resin import and is impregnated into material internal, and the molding composite element that is heating and curing, have
The advantages such as production efficiency is high, environmental pollution is little, quality of item is stable, excellent performance.
But, the vacuum in vacuum casting process of the prior art imports resin system and has working life
, therefore there is infiltration deficiency when medium-pressure or high pressure electrical insulations is poured into a mould, hold in the defect that short, toughness is not enough
Risk easy to crack.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is to provide a kind of vacuum to import resin, viscous
Spending low, toughness is high.
For reaching this purpose, the present invention by the following technical solutions:
A kind of vacuum imports resin, comprise following raw material: accounts for vacuum and imports the 50～70% of resin gross mass
Toughened epoxy resin, account for vacuum import resin gross mass 30～the firming agent of 50%；Such as, toughening type
Epoxy resin accounts for vacuum and imports the 50% of resin gross mass, 55%, 60%, 65%, 70%；Firming agent accounts for very
Empty importing the 30% of resin gross mass, 35%, 40%, 45%, 50%.
Preferably, a kind of vacuum imports resin, comprises following raw material: account for vacuum import resin gross mass 55～
The toughened epoxy resin of 65%, account for vacuum and import 35～the firming agent of 45% of resin gross mass；Such as,
Toughened epoxy resin account for vacuum import the 55% of resin gross mass, 56%, 57%, 58%, 59%, 60%,
61%, 62%, 63%, 64%, 65%；Firming agent account for vacuum import the 35% of resin gross mass, 36%,
37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%.
Wherein, described firming agent is tetramethyl guanidine, tetramethyl guanidine as the firming agent of toughened epoxy resin,
Hardening time and solidification temperature are moderate, cured after vacuum import resin viscosity low, function admirable,
A longer working life is had, it is to avoid the vacuum after solidification imports resin and loses too for a long time because depositing at a temperature of 40 DEG C
The waste that effect causes.During additionally the kind of firming agent is also selected from methyl tetrahydro phthalic anhydride and HHPA one
Kind or the mixed liquor of the two.
Wherein, described toughened epoxy resin, comprise following raw material: epoxy resin, nano-rubber particle are mixed
Closing liquid, reactive diluent, described epoxy resin is 90 with the mass ratio of described nano-rubber mix particles liquid:
(10～20), such as 90:10,90:12,90:15,90:16,90:18,90:20；Described asphalt mixtures modified by epoxy resin
The mass ratio of fat and described reactive diluent is 90:(5～15), such as 90:5,90:6,90:8,90:10,
90:12、90:15。
Described nano-rubber particle is full sulfuration carboxyl acrylonitrile-butadiene rubber powder end loose, without interleaving agent, averagely
Particle diameter is 50～150nm, such as 50nm, 60nm, 70nm, 80nm, 90nm, 100nm, 110nm,
120nm、130nm、140nm、150nm。
Wherein, described epoxy resin is in a liquid state under being room temperature bisphenol f type epoxy resin or bisphenol type epoxy
Resin.
Wherein, described nano-rubber mix particles liquid is for carry out scattered nanometer rubber with bisphenol A type epoxy resin
Glue particle solution.With bisphenol A type epoxy resin, nano-rubber particle is carried out dispersion and be prepared as nano-rubber grain
Sub-mixed liquor, makes nano-rubber particle more uniformly after being added in epoxy resin by nano-rubber mix particles liquid
Being scattered in epoxy resin, make the toughness of toughened epoxy resin prepared higher, performance is more longlasting.
Wherein, the preparation process of described nano-rubber mix particles liquid is: in parts by mass, take bisphenol-A ring
Epoxy resins 100 parts is in container, and the nano-rubber particle, the moistening of 0.8～1.2 part that add 20～35 parts divide
Powder, the coupling agent of 1.5～3 parts, such as 20 parts of nano-rubber particle, 22 parts, 25 parts, 28 parts, 30
Part, 32 parts, 34 parts, 35 parts, wetting dispersing agent 0.8 part, 0.9 part, 1 part, 1.1 parts, 1.2 parts,
Coupling agent 1.5 parts, 1.8 parts, 2 parts, 2.2 parts, 2.5 parts, 2.7 parts, 3 parts, at a temperature of 70～90 DEG C
Stir 1～1.5h with the mixing speed of 2000r/min, such as temperature is 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C,
90 DEG C, mixing time is 1h, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, is cooled to room temperature, prepares
Nano-rubber mix particles liquid.
Wherein, described reactive diluent is fats glycidyl ether.Nano-rubber particle and fats are shunk
The addition of glycerin ether makes the toughness of toughened epoxy resin increase, and viscosity reduces, it is simple to the technological operation in later stage.
Wherein, described fats glycidyl ether is 1,6-hexanediol diglycidyl ether, BDO
The mixture of at least two in diglycidyl ether, butyl glycidyl ether.
The two of the purpose of the present invention are the preparation method providing a kind of vacuum to import resin, comprise the following steps:
In toughened epoxy resin, add firming agent, under normal temperature and pressure, stir 0.5h, prepare vacuum and import tree
Fat；Wherein, described toughened epoxy resin accounts for vacuum and imports the 50～70% of resin gross mass, described solidification
Agent accounts for vacuum and imports the 30～50% of resin gross mass；
Preferably, described mixing speed is 1000～1500r/min, such as 1000r/min, 1100r/min,
1200r/min、1300r/min、1400r/min、1500r/min。
Wherein, the preparation process of described toughened epoxy resin is: add nano-rubber grain in the epoxy
Sub-mixed liquor, reactive diluent, with the speed stirring 0.5～1h of 2000r/min under room temperature, such as 0.5h,
0.8h, 1h, mix homogeneously, prepare toughened epoxy resin；
Preferably, the mass ratio of described epoxy resin and described nano-rubber mix particles liquid be 90:(10～
20), described epoxy resin is 90:(5～15 with the mass ratio of described reactive diluent).
The three of the purpose of the present invention are that providing a kind of vacuum to import resin pours into a mould at middle high-pressure electrical insulations
The application in field.
Compared with prior art, the invention have the benefit that the present invention vacuum import resin, comprise with
Lower raw material: account for vacuum and import 50～the toughened epoxy resin of 70% of resin gross mass, account for vacuum importing tree
The 30 of fat gross mass～the firming agent of 50%；The toughness that toughened epoxy resin makes vacuum import resin strengthens,
And reduce vacuum and import the viscosity of resin, it is simple to the technological operation in later stage；Tetramethyl guanidine is as toughening type
The firming agent of epoxy resin, hardening time and solidification temperature are moderate, cured after vacuum import the viscous of resin
Spend low, function admirable, at a temperature of 40 DEG C, there is a longer working life, it is to avoid the vacuum after solidification imports
Resin lost efficacy because depositing too for a long time the waste caused.
Detailed description of the invention
Technical scheme is further illustrated below by detailed description of the invention.
As no specific instructions, the various raw materials of the present invention are the most commercially available to be buied, or the routine side according to this area
Method prepares.
Embodiment 1
1) preparation of nano-rubber mix particles liquid: in parts by mass, takes bisphenol A epoxide resin 100 parts
To container, add the nano-rubber particle of 20 parts, the wetting dispersing agent of 0.8 part, the coupling agent of 1.5 parts,
At a temperature of 70 DEG C, the mixing speed with 2000r/min stirs 1h, is cooled to room temperature, prepares nanometer rubber
The sub-mixed liquor of micelle.
2) preparation of toughened epoxy resin: in parts by mass, adds in the bisphenol F epoxy resin of 90 parts
The most scattered nano-rubber mix particles liquid of 15 parts and the 1,6 hexanediol diglycidylether of 10 parts, 1,4-
The fats glycidyl ethers reactive diluents that butanediol diglycidyl ether mixes according to 1:1, at room temperature
Use 2000r/min to carry out high-speed stirred 0.5～1h, make mixed liquor uniform.
3) in parts by mass, above-mentioned mixed liquor adds the firming agent tetramethyl guanidine of 115 parts, long at room temperature
Pressure mixing speed is 1000～1500r/min, and mixing time is 0.5h, vacuum processed can import resin.
Embodiment 2
1) preparation of nano-rubber mix particles liquid: in parts by mass, takes bisphenol A epoxide resin 100 parts
To container, add the nano-rubber particle of 30 parts, the wetting dispersing agent of 1 part, the coupling agent of 2 parts,
At a temperature of 80 DEG C, the mixing speed with 2000r/min stirs 1.2h, is cooled to room temperature, prepares nano-rubber
Mix particles liquid.
2) preparation of toughened epoxy resin: in parts by mass, adds in the bisphenol F epoxy resin of 90 parts
The most scattered nano-rubber mix particles liquid of 10 parts and the 1,6 hexanediol diglycidylether of 5 parts, 1,4-
The fats glycidyl ethers reactive diluents that butanediol diglycidyl ether mixes according to 1:1, at room temperature
Use 2000r/min to carry out high-speed stirred 0.5～1h, make mixed liquor uniform.
3) in parts by mass, above-mentioned mixed liquor adds the firming agent tetramethyl guanidine of 105 parts, long at room temperature
Pressure mixing speed is 1000～1500r/min, and mixing time is 0.5h, can prepare vacuum and import resin.
Embodiment 3
1) preparation of nano-rubber mix particles liquid: in parts by mass, takes bisphenol A epoxide resin 100 parts
To container, add the nano-rubber particle of 35 parts, the wetting dispersing agent of 1.2 parts, the coupling agent of 2.5 parts,
At a temperature of 90 DEG C, the mixing speed with 2000r/min stirs 1.5h, is cooled to room temperature, prepares nanometer
Rubber particles mixed liquor.
2) preparation of toughened epoxy resin: in parts by mass, adds in the bisphenol F epoxy resin of 90 parts
The most scattered nano-rubber mix particles liquid of 20 parts and the butyl glycidyl ether of 15 parts, 1,4-butanediol two
The fats glycidyl ethers reactive diluents that glycidyl ether mixes according to 1:1, at room temperature uses 200
0r/min carries out high-speed stirred 0.5～1h, makes mixed liquor uniform.
3) in parts by mass, above-mentioned mixed liquor adds the firming agent tetramethyl guanidine of 125 parts, long at room temperature
Pressure mixing speed is 1000～1500r/min, and mixing time is 0.5h, can prepare vacuum and import resin.
Embodiment 4
1) preparation of nano-rubber mix particles liquid: in parts by mass, takes bisphenol A epoxide resin 100 parts
To container, add the nano-rubber particle of 25 parts, the wetting dispersing agent of 1.2 parts, the coupling agent of 2 parts,
At a temperature of 75 DEG C, the mixing speed with 2000r/min stirs 1.5h, is cooled to room temperature, prepares nanometer
Rubber particles mixed liquor.
2) preparation of toughened epoxy resin: in parts by mass, adds in the bisphenol F epoxy resin of 90 parts
The most scattered nano-rubber mix particles liquid of 15 parts and the butyl glycidyl ether of 10 parts, 1,4-butanediol two
The fats glycidyl ethers reactive diluents that glycidyl ether mixes according to 1:1, at room temperature uses 200
0r/min carries out high-speed stirred 0.5～1h, makes mixed liquor uniform.
3) in parts by mass, above-mentioned mixed liquor adds the firming agent tetramethyl guanidine of 49.28 parts, at room temperature
Long pressure mixing speed is 1000～1500r/min, and mixing time is 0.5h, can prepare vacuum and import resin.
Embodiment 5
1) preparation of nano-rubber mix particles liquid: in parts by mass, takes bisphenol A epoxide resin 100 parts
To container, add the nano-rubber particle of 24 parts, the wetting dispersing agent of 0.9 part, the coupling agent of 2.3 parts,
At a temperature of 85 DEG C, the mixing speed with 2000r/min stirs 1.3h, is cooled to room temperature, prepares nanometer
Rubber particles mixed liquor.
2) preparation of toughened epoxy resin: in parts by mass, adds in the bisphenol F epoxy resin of 90 parts
The most scattered nano-rubber mix particles liquid of 18 parts and the butyl glycidyl ether of 12 parts, 1,4-butanediol two
The fats glycidyl ethers reactive diluents that glycidyl ether mixes according to 1:1, at room temperature uses 200
0r/min carries out high-speed stirred 0.5～1h, makes mixed liquor uniform.
3) in parts by mass, above-mentioned mixed liquor adds the firming agent tetramethyl guanidine of 80 parts, in room temperature length pressure
Lower mixing speed is 1000～1500r/min, and mixing time is 0.5h, can prepare vacuum and import resin.
The commercially available liquid-state epoxy resin that model is EPIKOTETM RESIN 1800 is used to be used as middle high-pressure
The cast of electrical insulations transformator, as the comparative example of the present invention, leads vacuum prepared by embodiment 1～5
Enter resin and be used as the cast of middle high-pressure electrical insulations transformator, the transformator after cast is carried out performance survey
Examination, experimental result is as shown in table 1.
Table 1
Limit stress density factor KICOne of mechanical performance index for material, describes material opposing crackle
The ability of unstable propagation, close with the material of material, internal organizational structure, as-rolled condition and condition of heat treatment etc.
Cut is closed；GICEnergy is compared in fracture for material.By the data of table 1 it can be seen that vacuum prepared by the present invention is led
Enter resin and be used as the cast of middle high-pressure electrical insulations, the medium-high voltage power compared with comparative example, after cast
Toughness and the break resistance of gas insulating part all improve a lot, and viscosity is low, it is ensured that vacuum imports resin-cast
Sufficiently permeate after middle high-pressure electrical insulations, effectively reduce middle high-pressure electrical insulations after cast
The risk of cracking.
The vacuum of the present invention imports resin, and viscosity is low, and toughness is high, has longer being suitable at a temperature of 40 DEG C
Phase, and the preparation method of the vacuum importing resin of the present invention is simple, can be widely applied to medium-high voltage power
Gas insulating part cast field.
Applicant states, the present invention illustrates detailed process equipment and the technique of the present invention by above-described embodiment
Flow process, but the invention is not limited in above-mentioned detailed process equipment and technological process, i.e. do not mean that the present invention
Have to rely on above-mentioned detailed process equipment and technological process could be implemented.Person of ordinary skill in the field should
This understands, any improvement in the present invention, and the equivalence of raw material each to product of the present invention is replaced and auxiliary element
Interpolation, concrete way choice etc., within the scope of all falling within protection scope of the present invention and disclosure.
Claims (10)
1. a vacuum imports resin, it is characterised in that comprise following raw material: account for vacuum and import the total matter of resin
50～the toughened epoxy resin of 70% measured, 30～the firming agent of 50% accounting for vacuum importing resin gross mass.
Vacuum the most according to claim 1 imports resin, it is characterised in that described firming agent is tetramethyl
Base guanidine.
Vacuum the most according to claim 1 imports resin, it is characterised in that described toughening type asphalt mixtures modified by epoxy resin
Fat comprises following raw material: epoxy resin, nano-rubber mix particles liquid, reactive diluent, described asphalt mixtures modified by epoxy resin
Fat is 90:(10～20 with the mass ratio of described nano-rubber mix particles liquid), described epoxy resin is with described
The mass ratio of reactive diluent is 90:(5～15).
Vacuum the most according to claim 3 imports resin, it is characterised in that described epoxy resin is normal
The bisphenol f type epoxy resin being in a liquid state under temperature or bisphenol A type epoxy resin.
Vacuum the most according to claim 3 imports resin, it is characterised in that described nano-rubber particle
Mixed liquor is for carry out scattered nano-rubber particle solution with bisphenol A type epoxy resin；
Preferably, the preparation process of described nano-rubber mix particles liquid is: in parts by mass, take bisphenol-A
Epoxy resin 100 parts, in container, adds the nano-rubber particle of 20～35 parts, the moistening of 0.8～1.2 part
Dispersant, the coupling agent of 1.5～3 parts, at a temperature of 70～90 DEG C with the mixing speed of 2000r/min stir 1～
1.5h, is cooled to room temperature, prepares nano-rubber mix particles liquid.
Vacuum the most according to claim 3 imports resin, it is characterised in that described reactive diluent is
Fats glycidyl ether；
Preferably, described fats glycidyl ether is 1,6-hexanediol diglycidyl ether, Isosorbide-5-Nitrae-fourth two
The mixture of at least two in alcohol diglycidyl ether, butyl glycidyl ether.
7. the preparation method of a vacuum as claimed in claim 1 importing resin, it is characterised in that increasing
Tough type epoxy resin adds firming agent, prepares vacuum after stirring and import resin；Wherein, described
Toughened epoxy resin accounts for vacuum and imports the 50～70% of resin gross mass, and described firming agent accounts for vacuum and imports tree
The 30～50% of fat gross mass.
Preparation method the most according to claim 7, it is characterised in that the condition of described stirring is: stir
Mixing speed is 1000～1500r/min, and whipping temp is room temperature, and stirring pressure is normal pressure, and mixing time is 0.5h.
Preparation method the most according to claim 7, it is characterised in that described toughened epoxy resin
Preparation process be: in the epoxy add nano-rubber mix particles liquid, reactive diluent, under room temperature
With the speed stirring 0.5～1h of 2000r/min, mix homogeneously, prepare toughened epoxy resin；
Preferably, the mass ratio of described epoxy resin and described nano-rubber mix particles liquid be 90:(10～
20), described epoxy resin is 90:(5～15 with the mass ratio of described reactive diluent).
10. a vacuum as claimed in claim 1 imports resin at middle high-pressure electrical insulations cast neck
The application in territory.
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| CN110091459A (en) * | 2019-04-28 | 2019-08-06 | 维龙(镇江)机电科学研究院有限公司 | A kind of epoxy resin casting workpiece process for making and using epoxy resin casting workpiece made of this method |
| US11071998B2 (en) | 2017-09-05 | 2021-07-27 | George Irvin Fisher | Thick polymer coating of a substrate apparatus and method |
| US11167456B2 (en) | 2018-08-30 | 2021-11-09 | George Irvin Fisher | Thick polymer coating of a substrate apparatus and method |
| CN114702787A (en) * | 2022-04-25 | 2022-07-05 | 叶金蕊 | Super-high voltage resistant insulating resin suitable for vacuum suction injection molding and preparation method thereof |
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| CN114702787A (en) * | 2022-04-25 | 2022-07-05 | 叶金蕊 | Super-high voltage resistant insulating resin suitable for vacuum suction injection molding and preparation method thereof |
| WO2023206651A1 (en) * | 2022-04-25 | 2023-11-02 | 叶金蕊 | Ultrahigh-voltage-resistant insulating resin suitable for vacuum resin absorbable molding, and preparation method therefor |
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| CN105885356B (en) | 2019-01-04 |
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