CN108865047A - Anti-radiation adhesive of high temperature resistant and preparation method thereof - Google Patents
Anti-radiation adhesive of high temperature resistant and preparation method thereof Download PDFInfo
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- CN108865047A CN108865047A CN201810602119.4A CN201810602119A CN108865047A CN 108865047 A CN108865047 A CN 108865047A CN 201810602119 A CN201810602119 A CN 201810602119A CN 108865047 A CN108865047 A CN 108865047A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J179/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09J161/00 - C09J177/00
- C09J179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09J179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/03—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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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention discloses anti-radiation adhesives of a kind of high temperature resistant and preparation method thereof, using polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, isopropyl palmitate, naphtha, filler, antiradiation agent, coupling agent, surfactant, curing agent and diluent as the anti-radiation adhesive of high temperature resistant made from raw material, with high adhesion strength, high temperature resistance and impact strength, and the anti-radiation adhesive of high temperature resistant has high uvioresistant ability effect, radiation resistance is good, is 10.43w/m in irradiation intensity2, wave-length coverage is under the uv light irradiation of 280~315nm, and strength retention is high.It is obtained and bubble in the anti-radiation adhesive of high temperature resistant can be eliminated it is not necessary that defoaming agent is added in addition, method provided by the invention is simple, keep deaeration effect more convenient, thorough.
Description
Technical field
The present invention relates to adhesive field, especially a kind of anti-radiation adhesive of high temperature resistant and preparation method thereof.
Background technique
Adhesive refers to the technology that homogeneous or heterogeneous surface is linked together with adhesive, and there is stress distribution to connect
The features such as continuous, light-weight, technological temperature is low.It is glued especially suitable for different materials, different thicknesses, ultra-thin specification and complex component
Connection.Splicing RECENT DEVELOPMENTS is most fast, and application industry is extremely wide.There are many classification method of adhesive, can be divided into heat by application method
Curable type, heat molten type, room temperature curing type, pressure sensitive etc.；It is divided into structural, non-configuration or special glue by application；Connecing form can
It is divided into water-soluble, emulsion type, solvent type and various solid-state versions etc..But existing adhesive high temperature resistance and radiation resistance
Can be poor, it is impossible to meet requirements.
Summary of the invention
In view of this, the object of the present invention is to provide anti-radiation adhesive of a kind of high temperature resistant and preparation method thereof, high temperature resistant
Performance is good, and radiation resistance is high.
To achieve the goals above, the present invention provides the following technical solutions：
A kind of anti-radiation adhesive of high temperature resistant, the raw material including following parts by weight：.
Preferably, the filler is spodumene, pearl cotton, expanded perlite, silicon powder, Sodium Polyacrylate, magnesia, virtue
Synthetic fibre pulp fibers and sericite.
Preferably, the antiradiation agent include isomeric alcohol polyethenoxy ether, succinate, ricinoleic acid polyoxypropylene ester,
Septichen phenyl ester, methyl-silicone oil and dipentaerythritol.
Preferably, the coupling agent is 3- aminopropyl triethoxysilane, 3- mercaptopropyl trimethoxysilane, ethylenediamine third
Ethyl triethoxy silicane alkane or ethylenediamine hydroxypropyl methyl dimethoxysilane.
Preferably, the surfactant is Tween 80, neopelex or sorbester p18.
Preferably, the curing agent is diethylenetriamine, maleic anhydride, hexahydrophthalic acid anhydride or triethanolamine.
Preferably, the diluent is ethyl acetate, acetone, propyl alcohol, ethylene glycol ethyl ether, N, N- dimethylethanolamine or N,
N- dimethyl methyl hydramine.
The present invention also provides a kind of above-mentioned preparation methods of the anti-radiation adhesive of high temperature resistant, include the following steps：
A) by polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, palmitinic acid
Isopropyl ester, naphtha and diluent are 60~100r/min in revolving speed, stir evenly, obtain the first homomixture；
B) at 60~100r/min into the first homomixture that step a) is obtained be added filler, antiradiation agent, coupling agent,
Surfactant, diluent, after addition revolving speed be 40~60r/min, stir evenly, obtain the second homomixture；
C) curing agent is added into the second homomixture that step b) is obtained at 40~60r/min, stir evenly to get.
The present invention provides anti-radiation adhesives of a kind of high temperature resistant and preparation method thereof, with polyimides, phthalonitrile
Resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, isopropyl palmitate, naphtha, filler, antiradiation agent, coupling
Agent, surfactant, curing agent and diluent be raw material made from the anti-radiation adhesive of high temperature resistant, have high adhesion strength,
High temperature resistance and impact strength, and the anti-radiation adhesive of high temperature resistant has high uvioresistant ability effect, radiation resistance
It is good, it is 10.43w/m in irradiation intensity2, wave-length coverage is under the uv light irradiation of 280~315nm, and strength retention is high.Separately
Outside, method provided by the invention is simple, obtained and can eliminate in the anti-radiation adhesive of high temperature resistant it is not necessary that defoaming agent is added
Bubble keeps deaeration effect more convenient, thorough.
Specific embodiment
The anti-radiation adhesive of a kind of high temperature resistant provided by the invention, the raw material including following parts by weight：.
Above-mentioned technical proposal, with polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base first
Sulfonic acid, isopropyl palmitate, naphtha, filler, antiradiation agent, coupling agent, surfactant, curing agent and diluent are raw material
The anti-radiation adhesive of high temperature resistant obtained has high adhesion strength, high temperature resistance and impact strength, and the anti-spoke of high temperature resistant
Adhesive is penetrated with high uvioresistant ability effect, radiation resistance is good, is 10.43w/m in irradiation intensity2, wave-length coverage is
Under the uv light irradiation of 280~315nm, strength retention is high.
Polyimides can be improved the high temperature resistance of the anti-radiation adhesive of high temperature resistant.In the present invention, polyimides
Parts by weight are 50~80 parts；In an embodiment of the present invention, the parts by weight of polyimides are 55~75 parts；In other implementations
In example, the parts by weight of polyimides are 60~70 parts.
O-phthalonitrile resin is used to improve the antiseptic property and oxidation resistent susceptibility of the anti-radiation adhesive of high temperature resistant.In this hair
In bright, the parts by weight of o-phthalonitrile resin are 20~30 parts；In an embodiment of the present invention, the weight of o-phthalonitrile resin
Measuring number is 22~28 parts；In other embodiments, the parts by weight of o-phthalonitrile resin are 24~26 parts.
Glyptal is used to improve the impact strength of the anti-radiation adhesive of high temperature resistant.In the present invention, glyceryl alcohol
The parts by weight of acid resin are 10~20 parts；In an embodiment of the present invention, the parts by weight of glyptal are 12~17
Part；In other embodiments, the parts by weight of glyptal are 13~15 parts.
Acryloyl isopropylamine base methanesulfonic acid is used to improve the dimensional stability of the anti-radiation adhesive of high temperature resistant.In the present invention
In, the parts by weight of acryloyl isopropylamine base methanesulfonic acid are 7~10 parts；In an embodiment of the present invention, acryloyl isopropylamine base
The parts by weight of methanesulfonic acid are 7.5~9.5 parts；In other embodiments, the parts by weight of acryloyl isopropylamine base methanesulfonic acid are 8
~9 parts.
Isopropyl palmitate and naphtha are used to improve the adhesion strength of the anti-radiation adhesive of high temperature resistant.In the present invention
In, the parts by weight of isopropyl palmitate are 5~8 parts；In an embodiment of the present invention, the parts by weight of isopropyl palmitate are
5.5~7.5 parts；In other embodiments, the parts by weight of isopropyl palmitate are 6~7 parts.
In the present invention, the parts by weight of naphtha are 2~4 parts；In an embodiment of the present invention, the parts by weight of naphtha
Number is 2.4~3.5 parts；In other embodiments, the parts by weight of naphtha are 2.8~3.2 parts.
Filler is used to improve the high temperature resistance and dimensional stability of the anti-radiation adhesive of high temperature resistant.In implementation of the invention
Example in, filler include spodumene, pearl cotton, expanded perlite, silicon powder, Sodium Polyacrylate, magnesia, ppta-pulp fibre and
Sericite；In other embodiments, spodumene, pearl cotton, expanded perlite, silicon powder, Sodium Polyacrylate, magnesia, aramid fiber
The mass ratio of pulp fibers and sericite is (0.4~0.6)：(1~2)：(0.3~0.5)：(0.1~0.2)：(2~3)：(0.2
~0.4)：(1~2)：(0.3~0.4).
In the present invention, the parts by weight of filler are 30~50 parts；In an embodiment of the present invention, the parts by weight of filler
It is 35~46 parts；In other embodiments, the parts by weight of filler are 37~41 parts.
Antiradiation agent is while improving the radiation resistance of the anti-radiation adhesive of high temperature resistant, additionally it is possible to improve the stripping of resin
From intensity and mechanical property.In an embodiment of the present invention, antiradiation agent includes isomeric alcohol polyethenoxy ether, succinate, castor
Sesame oil acid polyoxypropylene ester, septichen phenyl ester, methyl-silicone oil and dipentaerythritol；In other embodiments, isomery alcohol
Polyoxyethylene ether, succinate, ricinoleic acid polyoxypropylene ester, septichen phenyl ester, methyl-silicone oil and dipentaerythritol
Mass ratio be (0.2~0.4)：(1~2)：(0.3~0.5)：(0.2~0.3)：(0.7~1)：(1~2).
In the present invention, the parts by weight of antiradiation agent are 0.5~1 part；In an embodiment of the present invention, antiradiation agent
Parts by weight are 0.6~0.9 part；In other embodiments, the parts by weight of antiradiation agent are 0.7~0.8 part.
In an embodiment of the present invention, coupling agent be 3- aminopropyl triethoxysilane, 3- mercaptopropyl trimethoxysilane,
Ethylenediaminepropyltriethoxysilane or ethylenediamine hydroxypropyl methyl dimethoxysilane.
In the present invention, the parts by weight of coupling agent are 1~2 part；In an embodiment of the present invention, the parts by weight of coupling agent
Number is 1.2~1.8 parts；In other embodiments, the parts by weight of coupling agent are 1.4~1.6 parts.
In an embodiment of the present invention, surfactant is Tween 80, neopelex or sorbester p18.
In the present invention, the parts by weight of surfactant are 5~8 parts；In an embodiment of the present invention, surfactant
Parts by weight be 5.5~7.5 parts；It can only blame in other embodiments, the parts by weight of surfactant are 6~7 parts.
In an embodiment of the present invention, curing agent is diethylenetriamine, maleic anhydride, hexahydrophthalic acid anhydride or three
Ethanol amine.
In the present invention, the parts by weight of curing agent are 10~20 parts；In an embodiment of the present invention, the weight of curing agent
Number is 12~18 parts；In other embodiments, the parts by weight of curing agent are 14~16 parts.
In an embodiment of the present invention, diluent is ethyl acetate, acetone, propyl alcohol, ethylene glycol ethyl ether, N, N- dimethyl second
Hydramine or N, N- dimethyl methyl hydramine.
In the present invention, the parts by weight of diluent are 10~20 parts；In an embodiment of the present invention, the weight of diluent
Number is 12~18 parts；In other embodiments, the parts by weight of diluent are 14~16 parts.
The present invention also provides a kind of above-mentioned preparation methods of the anti-radiation adhesive of high temperature resistant, include the following steps：
A) by polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, palmitinic acid
Isopropyl ester, naphtha and diluent are 60~100r/min in revolving speed, stir evenly, obtain the first homomixture；
B) at 60~100r/min into the first homomixture that step a) is obtained be added filler, antiradiation agent, coupling agent,
Surfactant, diluent, after addition revolving speed be 40~60r/min, stir evenly, obtain the second homomixture；
C) curing agent is added into the second homomixture that step b) is obtained at 40~60r/min, stir evenly to get.
Here, polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, palmitinic acid
Isopropyl ester, naphtha, filler, antiradiation agent, coupling agent, surfactant, curing agent and diluent are same as above, herein not
It repeats again.
In the present invention, by limiting the revolving speed of each step, so as to allow for high temperature resistant anti-it is not necessary that defoaming agent is added
Radiate bubble-free in adhesive.
In above-mentioned technical proposal, preparation method is simple, obtained and can to eliminate high temperature resistant anti-it is not necessary that defoaming agent is added
Bubble in adhesive is radiated, keeps deaeration effect more convenient, thorough, the anti-radiation adhesive of high temperature resistant obtained is glued with high
Knotting strength, high temperature resistance and impact strength, and the anti-radiation adhesive of high temperature resistant has high uvioresistant ability effect, anti-spoke
It is good to penetrate performance, is 10.43w/m in irradiation intensity2, wave-length coverage is strength retention under the uv light irradiation of 280~315nm
It is high.
In order to further illustrate the present invention, below with reference to embodiment to a kind of anti-radiation gluing of high temperature resistant provided by the invention
Agent and preparation method thereof is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
The anti-radiation adhesive of high temperature resistant, the raw material including following parts by weight：
55 parts of polyimides, 24 parts of o-phthalonitrile resins, 13 parts of glyptals, 7.5 parts of acryloyl isopropylamine bases
Methanesulfonic acid, 5.5 parts of isopropyl palmitates, 2.8 parts of naphthas, 37 parts of fillers, 0.5 part of antiradiation agent, 1.4 parts of three second of 3- aminopropyl
Oxysilane, 5.5 parts of sorbester p18s, 12 parts of maleic anhydrides and 12 parts of ethyl acetate；
Filler includes that mass ratio is 0.6:1.8:0.45:0.1:2:0.4:1.6:0.4 spodumene, expands treasure at pearl cotton
Zhu Yan, silicon powder, Sodium Polyacrylate, magnesia, ppta-pulp fibre and sericite；
Antiradiation agent includes that mass ratio is 0.28:1.2:0.48:0.28:0.7:1 isomeric alcohol polyethenoxy ether, succinic acid
Ester, ricinoleic acid polyoxypropylene ester, septichen phenyl ester, methyl-silicone oil and dipentaerythritol.
The preparation method of the anti-radiation adhesive of high temperature resistant, includes the following steps：
A) by polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, palmitinic acid
Isopropyl ester, naphtha and diluent are 800r/min in revolving speed, stir evenly, obtain the first homomixture；
B) filler, antiradiation agent, three second of 3- aminopropyl is added into the first homomixture that step a) is obtained at 80r/min
Oxysilane, sorbester p18, ethyl acetate, after addition revolving speed be 40r/min, stir evenly, obtain the second homomixture；
C) maleic anhydride is added into the second homomixture that step b) is obtained at 60r/min, stirs evenly, i.e.,
?.
Embodiment 2
The anti-radiation adhesive of high temperature resistant, the raw material including following parts by weight：
80 parts of polyimides, 26 parts of o-phthalonitrile resins, 10 parts of glyptals, 8 parts of acryloyl isopropylamine base first
Sulfonic acid, 8 parts of isopropyl palmitates, 2.4 parts of naphthas, 30 parts of fillers, 0.6 part of antiradiation agent, 1.6 parts of mercapto propyl trimethoxies
Silicon, 8 parts of neopelexes, 14 parts of hexahydrophthalic acid anhydrides and 20 parts of acetone；
Filler includes that mass ratio is 0.52:1:0.3:0.16:2.4:0.35:1:0.36 spodumene, expands treasure at pearl cotton
Zhu Yan, silicon powder, Sodium Polyacrylate, magnesia, ppta-pulp fibre and sericite；
Antiradiation agent includes that mass ratio is 0.2:1:0.36:0.3：0.75:2 isomeric alcohol polyethenoxy ether, succinate,
Ricinoleic acid polyoxypropylene ester, septichen phenyl ester, methyl-silicone oil and dipentaerythritol.
The preparation method of the anti-radiation adhesive of high temperature resistant, includes the following steps：
A) by polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, palmitinic acid
Isopropyl ester, naphtha and diluent are 60r/min in revolving speed, stir evenly, obtain the first homomixture；
B) filler, antiradiation agent, mercapto propyl trimethoxy is added into the first homomixture that step a) is obtained at 80r/min
Base silicon, neopelex, acetone, after addition revolving speed be 40r/min, stir evenly, obtain the second homomixture；
C) hexahydrophthalic acid anhydride is added into the second homomixture that step b) is obtained at 50r/min, stirs evenly, i.e.,
?.
Embodiment 3
The anti-radiation adhesive of high temperature resistant, the raw material including following parts by weight：
60 parts of polyimides, 30 parts of o-phthalonitrile resins, 12 parts of glyptals, 10 parts of acryloyl isopropylamine base first
Sulfonic acid, 6 parts of isopropyl palmitates, 3.5 parts of naphthas, 46 parts of fillers, 0.7 part of antiradiation agent, 1 part of ethylenediamine propyl triethoxy
Silane, 5 parts of Tween 80s, 20 parts of triethanolamines and 14 parts of propyl alcohol；
Filler includes that mass ratio is 0.4:1.2:0.32:0.2:3:0.25:1.2:0.3 spodumene, expands treasure at pearl cotton
Zhu Yan, silicon powder, Sodium Polyacrylate, magnesia, ppta-pulp fibre and sericite；
Antiradiation agent includes that mass ratio is 0.25:1.6:0.3:0.22:0.85:1.2 isomeric alcohol polyethenoxy ether, amber
Acid esters, ricinoleic acid polyoxypropylene ester, septichen phenyl ester, methyl-silicone oil and dipentaerythritol.
The preparation method of the anti-radiation adhesive of high temperature resistant, includes the following steps：
A) by polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, palmitinic acid
Isopropyl ester, naphtha and diluent are 80r/min in revolving speed, stir evenly, obtain the first homomixture；
B) filler, antiradiation agent, ethylenediamine propyl is added into the first homomixture that step a) is obtained at 100r/min
Triethoxysilane, Tween 80, propyl alcohol, after addition revolving speed be 50r/min, stir evenly, obtain the second homomixture；
C) triethanolamine is added into the second homomixture that step b) is obtained at 40r/min, stir evenly to get.
Embodiment 4
The anti-radiation adhesive of high temperature resistant, the raw material including following parts by weight：
75 parts of polyimides, 20 parts of o-phthalonitrile resins, 17 parts of glyptals, 9.5 parts of acryloyl isopropylamine bases
Methanesulfonic acid, 7 parts of isopropyl palmitates, 3.2 parts of naphthas, 42 parts of fillers, 0.8 part of antiradiation agent, 2 parts of ethylenediamine hydroxypropyl methyls two
Methoxy silane, 6 parts of sorbester p18s, 16 parts of maleic anhydrides and 16 parts of ethylene glycol ethyl ethers；
Filler includes that mass ratio is 0.48:1.4:0.42:0.12:2.6:0.27:2:It is 0.37 spodumene, pearl cotton, swollen
Swollen perlite, silicon powder, Sodium Polyacrylate, magnesia, ppta-pulp fibre and sericite；
Antiradiation agent includes that mass ratio is 0.4:1.8:0.35:0.2:0.8:1.4 isomeric alcohol polyethenoxy ether, succinic acid
Ester, ricinoleic acid polyoxypropylene ester, septichen phenyl ester, methyl-silicone oil and dipentaerythritol.
The preparation method of the anti-radiation adhesive of high temperature resistant, includes the following steps：
A) by polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, palmitinic acid
Isopropyl ester, naphtha and diluent are 600r/min in revolving speed, stir evenly, obtain the first homomixture；
B) filler, antiradiation agent, ethylenediamine propyl first is added into the first homomixture that step a) is obtained at 60r/min
Base dimethoxysilane, sorbester p18, ethylene glycol ethyl ether, after addition revolving speed be 60r/min, stir evenly, obtain second
Homomixture；
C) maleic anhydride is added into the second homomixture that step b) is obtained at 60r/min, stirs evenly, i.e.,
?.
Embodiment 5
The anti-radiation adhesive of high temperature resistant, the raw material including following parts by weight：
70 parts of polyimides, 22 parts of o-phthalonitrile resins, 15 parts of glyptals, 9 parts of acryloyl isopropylamine base first
Sulfonic acid, 7.5 parts of isopropyl palmitates, 4 parts of naphthas, 50 parts of fillers, 0.9 part of antiradiation agent, 1.2 parts of 3- aminopropyl-triethoxies
Silane, 7 parts of Tween 80s, 18 parts of diethylenetriamines and 18 parts of N, N- dimethylethanolamine；
Filler includes that mass ratio is 0.45:2:0.5:0.14:2.2:0.2:1.4:0.33 spodumene, pearl cotton, expansion
Perlite, silicon powder, Sodium Polyacrylate, magnesia, ppta-pulp fibre and sericite；
Antiradiation agent includes that mass ratio is 0.36:2:0.5:0.24:1:1.6 isomeric alcohol polyethenoxy ether, succinate,
Ricinoleic acid polyoxypropylene ester, septichen phenyl ester, methyl-silicone oil and dipentaerythritol.
The preparation method of the anti-radiation adhesive of high temperature resistant, includes the following steps：
A) by polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, palmitinic acid
Isopropyl ester, naphtha and diluent are 100r/min in revolving speed, stir evenly, obtain the first homomixture；
B) filler, antiradiation agent, three second of 3- aminopropyl is added into the first homomixture that step a) is obtained at 60r/min
Oxysilane, Tween 80, N, N- dimethylethanolamine, after addition revolving speed be 60r/min, stir evenly, obtain second
Homomixture；
C) diethylenetriamine is added into the second homomixture that step b) is obtained at 40r/min, stir evenly to get.
Embodiment 6
The anti-radiation adhesive of high temperature resistant, the raw material including following parts by weight：
50 parts of polyimides, 28 parts of o-phthalonitrile resins, 20 parts of glyptals, 7 parts of acryloyl isopropylamine base first
Sulfonic acid, 5 parts of isopropyl palmitates, 2 parts of naphthas, 35 parts of fillers, 1 part of antiradiation agent, 1.8 parts of 3- mercapto propyl trimethoxy silicon
Alkane, 7.5 parts of neopelexes, 10 parts of hexahydrophthalic acid anhydrides and 10 parts of N, N- dimethyl methyl hydramine；
Filler includes that mass ratio is 0.55:1.6:0.35:0.18:2.8:0.36:1.8:0.39 spodumene, pearl cotton,
Expanded perlite, silicon powder, Sodium Polyacrylate, magnesia, ppta-pulp fibre and sericite；
Antiradiation agent includes that mass ratio is 0.35:1.4:0.45:0.26:0.9:1.8 isomeric alcohol polyethenoxy ether, amber
Acid esters, ricinoleic acid polyoxypropylene ester, septichen phenyl ester, methyl-silicone oil and dipentaerythritol.
The preparation method of the anti-radiation adhesive of high temperature resistant, includes the following steps：
A) by polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, palmitinic acid
Isopropyl ester, naphtha and diluent are 60r/min in revolving speed, stir evenly, obtain the first homomixture；
B) filler, antiradiation agent, 3- mercapto propyl front three is added into the first homomixture that step a) is obtained at 80r/min
Oxysilane, neopelex, N, N- dimethyl methyl hydramine in revolving speed are 50r/min after addition, and stirring is equal
It is even, obtain the second homomixture；
C) hexahydrophthalic acid anhydride is added into the second homomixture that step b) is obtained at 60r/min, stirs evenly, i.e.,
?.
Embodiment 7
The anti-radiation adhesive of high temperature resistant, the raw material including following parts by weight：
65 parts of polyimides, 25 parts of o-phthalonitrile resins, 14 parts of glyptals, 8.5 parts of acryloyl isopropylamine bases
Methanesulfonic acid, 6.5 parts of isopropyl palmitates, 3 parts of naphthas, 40 parts of fillers, 0.75 part of antiradiation agent, 1.5 parts of ethylenediamine propyl three
Ethoxysilane, 6.5 parts of Tween 80s, 15 parts of diethylenetriamines and 15 parts of N, N- dimethylethanolamine；
Filler includes that mass ratio is 0.5：1.5:0.4:0.15:2.5:0.3:1.5:0.35 spodumene, pearl cotton, expansion
Perlite, silicon powder, Sodium Polyacrylate, magnesia, ppta-pulp fibre and sericite；
Antiradiation agent includes that mass ratio is 0.3:1.5:0.4:0.25:0.85:1.5 isomeric alcohol polyethenoxy ether, amber
Acid esters, ricinoleic acid polyoxypropylene ester, septichen phenyl ester, methyl-silicone oil and dipentaerythritol.
The preparation method of the anti-radiation adhesive of high temperature resistant, includes the following steps：
A) by polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, palmitinic acid
Isopropyl ester, naphtha and diluent are 80r/min in revolving speed, stir evenly, obtain the first homomixture；
B) filler, antiradiation agent, ethylenediamine propyl three is added into the first homomixture that step a) is obtained at 80r/min
Ethoxysilane, Tween 80, N, N- dimethylethanolamine in revolving speed are 50r/min after addition, stir evenly, obtain the
Two homomixtures；
C) diethylenetriamine is added into the second homomixture that step b) is obtained at 50r/min, stir evenly to get.
The anti-radiation adhesive of high temperature resistant made from Examples 1 to 7 is subjected to adhesion strength, high temperature resistance, radiation resistance
It can test, the results are shown in Table 1.
Radiation resistance measurement：The anti-radiation adhesive of high temperature resistant of specially above-mentioned preparation measures after uv light irradiation
Its intensity keeps data, irradiation intensity 10.43w/m2, wave-length coverage is 280~315nm.
The measurement result of 1 Examples 1 to 7 of table
Above description can be realized professional and technical personnel in the field or using this to stating in the disclosed embodiments
It is bright, it enables those skilled in the art to implement or use the present invention.Various modifications to these embodiments are to this field
It will be apparent for professional technician, the general principles defined herein can not depart from spirit of the invention
Or in the case where range, realize in other embodiments.Therefore, the present invention is not intended to be limited to these implementations shown in this article
Example, and it is to fit to the widest scope consistent with principles disclosed herein and novel features.
Claims (8)
1. a kind of anti-radiation adhesive of high temperature resistant, which is characterized in that the raw material including following parts by weight：
2. the anti-radiation adhesive of high temperature resistant as described in claim 1, which is characterized in that the filler includes spodumene, pearl
Cotton, expanded perlite, silicon powder, Sodium Polyacrylate, magnesia, ppta-pulp fibre and sericite.
3. the anti-radiation adhesive of high temperature resistant as described in claim 1, which is characterized in that the antiradiation agent includes that isomery alcohol is poly-
Ethylene oxide ether, succinate, ricinoleic acid polyoxypropylene ester, septichen phenyl ester, methyl-silicone oil and dipentaerythritol.
4. the anti-radiation adhesive of high temperature resistant as described in claim 1, which is characterized in that the coupling agent is three second of 3- aminopropyl
Oxysilane, 3- mercaptopropyl trimethoxysilane, ethylenediaminepropyltriethoxysilane or ethylenediamine hydroxypropyl methyl dimethoxy
Silane.
5. the anti-radiation adhesive of high temperature resistant as described in claim 1, which is characterized in that the surfactant be Tween 80,
Neopelex or sorbester p18.
6. the anti-radiation adhesive of high temperature resistant as described in claim 1, which is characterized in that the curing agent be diethylenetriamine,
Maleic anhydride, hexahydrophthalic acid anhydride or triethanolamine.
7. the anti-radiation adhesive of high temperature resistant as described in claim 1, which is characterized in that the diluent is ethyl acetate, third
Ketone, propyl alcohol, ethylene glycol ethyl ether, N, N- dimethylethanolamine or N, N- dimethyl methyl hydramine.
8. a kind of preparation method of the anti-radiation adhesive of high temperature resistant as described in any one of claims 1 to 7, which is characterized in that
Include the following steps：
A) by polyimides, o-phthalonitrile resin, glyptal, acryloyl isopropylamine base methanesulfonic acid, palmitinic acid isopropyl
Ester, naphtha and diluent are 60~100r/min in revolving speed, stir evenly, obtain the first homomixture；
B) filler, antiradiation agent, coupling agent, surface is added into the first homomixture that step a) is obtained at 60~100r/min
Activating agent, diluent, after addition revolving speed be 40~60r/min, stir evenly, obtain the second homomixture；
C) curing agent is added into the second homomixture that step b) is obtained at 40~60r/min, stir evenly to get.
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Cited By (1)
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