CN107686717A - A kind of preparation method of high-temperature resistant silicone adhesive - Google Patents
A kind of preparation method of high-temperature resistant silicone adhesive Download PDFInfo
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- CN107686717A CN107686717A CN201710790408.7A CN201710790408A CN107686717A CN 107686717 A CN107686717 A CN 107686717A CN 201710790408 A CN201710790408 A CN 201710790408A CN 107686717 A CN107686717 A CN 107686717A
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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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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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
- C09J11/08—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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2205/02—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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- 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
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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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- 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
- C08L2205/06—Polymer mixtures characterised by other features having improved processability or containing aids for moulding methods
Abstract
The invention discloses a kind of preparation method of high-temperature resistant silicone adhesive, including the step of prepare component A, prepare component B and component A and component B are mixed into solidify afterwards.In the step of preparing component A and component B, add raw materials into the mixing of the first material cylinder and be stirred, directly can be carried out in the system of opening wide, it is not necessary to which specific inert gas shielding is stirred under conditions of vacuum；In addition, by the mixture being stirred from the first material cylinder by the filter screen natural filtration of 300~400 mesh to the second material cylinder, it is not necessary to high pressure is extruded.Compared with traditional organic silicon adhesive preparation technology, the preparation method of high-temperature resistant silicone adhesive provided by the present invention both simplifies working condition, the production time is also saved simultaneously, and there is the performances such as very high refractive index, light transmittance and high temperature resistant according to the organosilicon adhesive obtained by the method for the present invention.
Description
Technical field
The present invention relates to technical field of polymer materials, more particularly to a kind of preparation side of high-temperature resistant silicone adhesive
Method.
Background technology
So far, most of traditional processing technology of adhesive is by scattered, high pressure at a high speed in de-airing mixer
Extrusion, vacuum defoam and extruded several stages such as filling to complete.In these production technologies, some technologies of generally existing
Defect, such as：Working condition is harsh, production process is complicated, the production time is long, production efficiency is low etc..
As organic silicon adhesive in the extensive use of each industrial technical field, its preparation technology also receives attention
And research.How a kind of organic silicon adhesive preparation technology convenient, efficient, that be suitable for large-scale industrialized production is developed
It is urgent problem to be solved.
The content of the invention
In order to solve the above-mentioned technical problem, it is an object of the invention to provide a kind of preparation of high-temperature resistant silicone adhesive
Method.
The preparation method for the high-temperature resistant silicone adhesive that embodiments of the present invention are provided, is comprised the following steps：System
Standby component A：Weigh in parts by weight：20~50 parts of aminated compounds, 10~18 parts of epoxy resin compound, curing agent 5~
10 parts；Aminated compounds and epoxy resin compound are sequentially added in the first material cylinder of mixer and stirred, is then added solid
Agent, continue to stir；By obtained mixture from the first material cylinder through filter screen natural filtration to the second material cylinder；To the second material cylinder
In mixture it is filling, obtain component A；Prepare component B：Weigh in parts by weight：25~40 parts of the hydrogeneous silicones of phenyl, increase
Tough dose 3~6 parts, 5~10 parts of curing agent, 0.009~0.1 part of platinum catalyst；By the hydrogeneous silicones of phenyl, toughener, platinum catalysis
Agent sequentially adds stirs in the first material cylinder of mixer, then adds curing agent, continues to stir；By obtained mixture from
Through filter screen natural filtration to the second material cylinder in one material cylinder；It is filling to the mixture in the second material cylinder, obtain component B；By described in
Component A and component B mixing solidify afterwards, that is, be made high-temperature resistant silicone adhesive.
Relative to prior art, the preparation method for the high-temperature resistant silicone adhesive that embodiments of the present invention are provided,
Process conditions are simple, and production process is convenient, and preparation time is shorter, and production efficiency is high, and the organosilicon adhesive being prepared
Translucency and light transmittance are good, and have very high resistance to elevated temperatures, can be widely used in electronics, machinery, aviation, building,
The industry such as medical treatment and communication.
Preferably, in the preparation method for the high-temperature resistant silicone adhesive that embodiments of the present invention are provided, preparation group
Part A is identical with the speed in the step of preparing component B, being stirred in the first material cylinder with continuing stirring, is 40 specifically
~60rpm/min.
Preferably, in the preparation method for the high-temperature resistant silicone adhesive that embodiments of the present invention are provided, preparation group
For part A with the step of preparing component B, the time stirred in the first material cylinder and continue stirring is respectively 20~40 minutes.
Preferably, in the preparation method for the high-temperature resistant silicone adhesive that embodiments of the present invention are provided, preparation group
For part A with the step of preparing component B, the natural filtration uses 300~400 mesh filter screens.
Preferably, in the preparation method for the high-temperature resistant silicone adhesive that embodiments of the present invention are provided, preparation group
In the step of part A, the aminated compounds is N ' N-4, the double maleic amides of 4 '-diphenyl-methane type.
Preferably, in the preparation method for the high-temperature resistant silicone adhesive that embodiments of the present invention are provided, preparation group
In the step of part A, described epoxy resin compound is：Glycidyl ether type epoxy resin, glycidol esters asphalt mixtures modified by epoxy resin
Fat, glycidyl amine epoxy resin, linear aliphatic epoxy resin or alicyclic based epoxy resin.
Preferably, in the preparation method for the high-temperature resistant silicone adhesive that embodiments of the present invention are provided, preparation group
In the step of part B, the hydrogeneous silicones of described phenyl contains comprising one or several kinds of hydrogen contents in 0.01~0.5% phenyl
Hydrogen polysiloxanes.
Preferably, in the preparation method for the high-temperature resistant silicone adhesive that embodiments of the present invention are provided, preparation group
In the step of part B, described toughener is carboxyl LNBR, polysulfide rubber, liquid silastic, polyethers, polysulfones, received
One or more in rice calcium carbonate and nano titanium oxide.
Preferably, in the preparation method for the high-temperature resistant silicone adhesive that embodiments of the present invention are provided, preparation group
Part A is with the step of preparing component B, and described curing agent is 4,4 '-MDA.
Preferably, in the preparation method for the high-temperature resistant silicone adhesive that embodiments of the present invention are provided, preparation group
In the step of part B, described platinum catalyst is chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound.
To sum up, the production technology of a kind of high-temperature resistant silicone adhesive of the present invention, is preparing component A and component B
The step of in, the raw material weighed sequentially added into the first material cylinder mixed and be stirred, produced with traditional organosilicon adhesive
Compared to being, the operating procedure can be carried out directly technique in the system of opening wide, it is not necessary to specific inert gas shielding or
It is stirred under conditions of vacuum；In addition, in preparation process, by the mixture being stirred from the first material cylinder by 300~
The filter screen natural filtration of 400 mesh is compared with the production technology of traditional organosilicon adhesive, is somebody's turn to do to the second material cylinder
Operating procedure natural filtration is flowed out, it is not necessary to which high pressure is extruded.It follows that embodiments of the present invention provided it is resistance to
The preparation method of high temperature silicone adhesive both simplifies working condition, while also saves the production time, and in the production
Obtained organosilicon adhesive has the performances such as very high refractive index, light transmittance and high temperature resistant under technological operation.
Embodiment
The present invention is described in further detail below, to facilitate those skilled in the art with reference to specification word energy
Enough it is practiced (in following embodiment, various raw materials are 1 gram per mass parts).
Embodiment 1
Prepare component A：Weigh aminated compounds N ' N-4 in parts by weight, double 25 parts of the maleic amides of 4 '-diphenyl-methane type,
16 parts of epoxy resin compound bisphenol F types epoxy resin, curing agent 4,8 parts of 4 '-MDA；By what is weighed
Above-mentioned aminated compounds and epoxy resin compound, in the first material cylinder for sequentially adding mixer, start stirring (50rpm/
Min stirring 30 minutes) is maintained, adds curing agent afterwards, continues stirring 30 minutes under same rotational speed；By what is obtained by stirring
Mixture flows out from the first material cylinder by the filter screen natural filtration of 300~400 mesh, enters the second material cylinder；By natural filtration
The mixture progress gone out is filling, obtains component A.
Prepare component B：30 parts of the hydrogeneous silicones of phenyl that hydrogen content is 0.15%, toughener carboxylic are weighed in parts by weight
4 parts of base LNBR, curing agent 4,6 parts of 4 '-MDA, platinum catalyst chloroplatinic acid tetramethyl tetravinyl
0.08 part of cyclotetrasiloxane complex compound；The hydrogeneous silicones of the phenyl weighed, toughener, platinum catalyst are sequentially added into stirring
In first material cylinder of machine, start stirring (40rpm/min) and maintain stirring 30 minutes, add curing agent afterwards, under same rotational speed after
Continuous stirring 30 minutes；The mixture obtained by stirring is passed through to the filter screen natural filtration stream of 300-400 mesh from the first material cylinder
Go out, enter the second material cylinder；The mixture progress that natural filtration is gone out is filling, obtains component B.
Mix, stir 15 minutes, reduced pressure lower pumping in use, component A and B component are added among reaction bulb
10 minutes, the bubble in reaction system is removed, 60 DEG C is then heated to, is taken out after 30 minutes, be cooled to room temperature, you can obtained
Organosilicon adhesive with high-temperature stability.
Embodiment 2
Prepare component A：Weigh aminated compounds N ' N-4 in parts by weight, double 35 parts of the maleic amides of 4 '-diphenyl-methane type,
16 parts of epoxy resin compound polybutadiene, curing agent 4,5 parts of 4 '-MDA；The amine that will have been weighed
Compound, epoxy resin compound, it is added sequentially in the first material cylinder of mixer, starts stirring (60rpm/min) maintenance
Stirring 30 minutes, adds curing agent afterwards, continues stirring 20 minutes under same rotational speed；By the mixture obtained by stirring from
Flowed out in first material cylinder by the filter screen natural filtration of 300~400 mesh, enter the second material cylinder；The mixing that natural filtration is gone out
Thing progress is filling, obtains component A.
Prepare component B：Hydrogen content is weighed as 28 parts of the hydrogeneous silicones of 0.15% phenyl, toughener polysulfide using parts by weight
4 parts of rubber, curing agent 4,8 parts of 4 '-MDA, platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane
0.05 part of complex compound；By the hydrogeneous silicones of the phenyl weighed, toughener, platinum catalyst sequentially adds the first material of mixer
In cylinder, start stirring (50rpm/min) and maintain stirring 30 minutes, add curing agent afterwards, continue 40 points of stirring under same rotational speed
Clock；The mixture obtained by stirring is flowed out from the first material cylinder by the filter screen natural filtration of 300-400 mesh, entered
Second material cylinder；The mixture progress that natural filtration is gone out is filling, obtains component B.
In use, component A and B component are added sequentially to mix among reaction bulb, stir 15 minutes, under reduced pressure
Pumping 10 minutes, the bubble in reaction system is removed, 60 DEG C is then heated to, is taken out after 30 minutes, be cooled to room temperature, you can
Obtain the organosilicon adhesive with high-temperature stability.
Embodiment 3
Prepare component A：Weigh aminated compounds N ' N-4 in parts by weight, double 30 parts of the maleic amides of 4 '-diphenyl-methane type,
15 parts of epoxy resin compound bisphenol F types epoxy resin, curing agent 4,8 parts of 4 '-MDA；By what is weighed
Aminated compounds, epoxy resin compound, it is added sequentially in the first material cylinder of mixer, starts stirring (40rpm/min)
Stirring 30 minutes is maintained, adds curing agent afterwards, continues stirring 30 minutes under same rotational speed；The mixing that will be obtained by stirring
Thing flows out from the first material cylinder by the filter screen natural filtration of 300-400 mesh, enters the second material cylinder；Natural filtration is gone out
Mixture progress is filling, obtains component A.
Prepare component B：It is referred to as 0.15% 30 parts of the hydrogeneous silicones of phenyl using parts by weight hydrogen content, toughener nano-sized carbon
Sour 5 parts of calcium, curing agent 4,6 parts of 4 '-MDA, platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane
0.06 part of complex compound；By the hydrogeneous silicones of the phenyl weighed, toughener, platinum catalyst sequentially adds the first material of mixer
In cylinder, start stirring (50rpm/min) and maintain stirring 30 minutes, add curing agent afterwards, continue 30 points of stirring under same rotational speed
Clock；The mixture obtained by stirring is flowed out from the first material cylinder by the filter screen natural filtration of 300-400 mesh, entered
Second material cylinder；The mixture progress that natural filtration is gone out is filling, obtains component B.
In use, component A and B component are added sequentially to mix among reaction bulb, stir 15 minutes, under reduced pressure
Pumping 10 minutes, the bubble in reaction system is removed, 60 DEG C is then heated to, is taken out after 30 minutes, be cooled to room temperature, you can
Obtain the organosilicon adhesive with high-temperature stability.
Embodiment 4
Prepare component A：Weigh aminated compounds N ' N-4 in parts by weight, double 35 parts of the maleic amides of 4 '-diphenyl-methane type,
16 parts of epoxy resin compound polybutadiene, curing agent 4,6 parts of 4 '-MDA；The amine that will have been weighed
Compound, epoxy resin compound, it is added sequentially in the first material cylinder of mixer, starts stirring (60rpm/min) maintenance
Stirring 30 minutes, adds curing agent afterwards, continues stirring 20 minutes under same rotational speed；By the mixture obtained by stirring from
Flowed out in first material cylinder by the filter screen natural filtration of 300-400 mesh, enter the second material cylinder；The mixing that natural filtration is gone out
Thing progress is filling, obtains component A.
Prepare component B：30 parts of the hydrogeneous silicones of phenyl that hydrogen content is 0.15% is weighed in parts by weight, and toughener is received
5 parts of titanium dioxide of rice, curing agent 4,6 parts of 4 '-MDA, platinum catalyst chloroplatinic acid tetramethyl tetravinyl ring four
0.05 part of silicone complex；The hydrogeneous silicones of the phenyl weighed, toughener, platinum catalyst are sequentially added into mixer
In first material cylinder, start stirring (50rpm/min) and maintain stirring 30 minutes, add curing agent afterwards, continue to stir under same rotational speed
Mix 20 minutes；The mixture obtained by stirring is flowed out from the first material cylinder by the filter screen natural filtration of 300-400 mesh,
Enter the second material cylinder；The mixture progress that natural filtration is gone out is filling, obtains component B.
In use, component A and B component are added sequentially to mix among reaction bulb, stir 15 minutes, under reduced pressure
Pumping 10 minutes, the bubble in reaction system is removed, 60 DEG C is then heated to, is taken out after 30 minutes, be cooled to room temperature, you can
Obtain the organosilicon adhesive with high-temperature stability.
Embodiment 5
Prepare component A：Aminated compounds N ' N-4, double 40 parts of the maleic amides of 4 '-diphenyl-methane type, ring are weighed with parts by weight
15 parts of the phenolic group ethane type epoxy resin of oxygen tree lipoid substance four, curing agent 4,7 parts of 4 '-MDA；It will weigh
Aminated compounds, epoxy resin compound, be added sequentially in the first material cylinder of mixer, start stirring (50rpm/
Min stirring 40 minutes) is maintained, adds curing agent afterwards, continues stirring 30 minutes under same rotational speed；By what is obtained by stirring
Mixture flows out from the first material cylinder by the filter screen natural filtration of 300-400 mesh, enters the second material cylinder；By natural filtration
The mixture progress gone out is filling, obtains component A.
Prepare component B：Hydrogen content is weighed as 30 parts of the hydrogeneous silicones of 0.15% phenyl, toughener carboxyl using parts by weight
5 parts of LNBR and polysulfide rubber mixture, curing agent 4,8 parts of 4 '-MDA, platinum catalyst chloroplatinic acid
0.05 part of t etram-ethyltetravinylcyclotetrasiloxane complex compound；By the hydrogeneous silicones of the phenyl weighed, toughener, platinum catalysis
Agent is sequentially added in the first material cylinder of mixer, is started stirring (60 rpm/min) and is maintained stirring 30 minutes, adds solidification afterwards
Agent, continue stirring 30 minutes under same rotational speed；The mixture obtained by stirring is passed through into 300-400 mesh from the first material cylinder
Filter screen natural filtration outflow, enter the second material cylinder；The mixture progress that natural filtration is gone out is filling, obtains component B.
In use, component A and B component are added sequentially to mix among reaction bulb, stir 15 minutes, under reduced pressure
Pumping 10 minutes, the bubble in reaction system is removed, 60 DEG C is then heated to, is taken out after 30 minutes, be cooled to room temperature, you can
Obtain the organosilicon adhesive with high-temperature stability.
Embodiment 6
Prepare component A：Aminated compounds N ' N-4, double 35 parts of the maleic amides of 4 '-diphenyl-methane type, ring are weighed with parts by weight
16 parts of oxygen tree lipoid substance polybutadiene, curing agent 4,8 parts of 4 '-MDA；The amine that will have been weighed
Compound, epoxy resin compound, it is added sequentially in the first material cylinder of mixer, starts stirring (40rpm/min) and maintain to stir
Mix 40 minutes, add curing agent afterwards, continue stirring 30 minutes under same rotational speed；By the mixture obtained by stirring from the
Flowed out in one material cylinder by the filter screen natural filtration of 300~400 mesh, enter the second material cylinder；The mixture that natural filtration is gone out
Carry out filling, obtain component A.
Prepare component B：Hydrogen content is weighed as 30 parts of the hydrogeneous silicones of 0.15% phenyl, toughener liquid using parts by weight
5 parts of silicon rubber, curing agent 4,7 parts of 4 '-MDA, the silica of platinum catalyst chloroplatinic acid tetramethyl tetravinyl ring four
0.07 part of alkane complex compound；The hydrogeneous silicones of the phenyl weighed, toughener, platinum catalyst are sequentially added into the first of mixer
In material cylinder, start stirring (60rpm/min) and maintain stirring 30 minutes, add curing agent afterwards, continue stirring 20 under same rotational speed
Minute；The mixture obtained by stirring is flowed out from the first material cylinder by the filter screen natural filtration of 300-400 mesh, entered
To the second material cylinder；The mixture progress that natural filtration is gone out is filling, obtains component B.
In use, component A and B component are added sequentially to mix among reaction bulb, stir 15 minutes, under reduced pressure
Pumping 10 minutes, the bubble in reaction system is removed, 60 DEG C is then heated to, is taken out after 30 minutes, be cooled to room temperature, you can
Obtain the organosilicon adhesive with high-temperature stability.
Embodiment 7
Prepare component A：Aminated compounds N ' N-4, double 40 parts of the maleic amides of 4 '-diphenyl-methane type, ring are weighed with parts by weight
16 parts of oxygen tree lipoid substance bisphenol f type epoxy resin, curing agent 4,6 parts of 4 '-MDA；The amine that will have been weighed
Class compound, epoxy resin compound, it is added sequentially in the first material cylinder of mixer, starts stirring (50rpm/min) dimension
Stirring 30 minutes is held, adds curing agent afterwards, continues stirring 30 minutes under same rotational speed；The mixture that will be obtained by stirring
Flowed out from the first material cylinder by the filter screen natural filtration of 300-400 mesh, enter the second material cylinder；Natural filtration is gone out mixed
Compound progress is filling, obtains component A.
Prepare component B：Hydrogen content is weighed as 30 parts of the hydrogeneous silicones of 0.15% phenyl, toughener nanometer using parts by weight
4 parts of calcium carbonate and nano titanium dioxide mixture, curing agent 4,8 parts of 4 '-MDA, platinum catalyst chloroplatinic acid four
0.08 part of methyl tetravinyl cyclotetrasiloxane complex compound；By the hydrogeneous silicones of the phenyl weighed, toughener, platinum catalyst
In the first material cylinder for sequentially adding mixer, start stirring (50 rpm/min) and maintain stirring 20 minutes, add curing agent afterwards,
Continue stirring 30 minutes under same rotational speed；The mixture obtained by stirring is passed through to the filter of 300-400 mesh from the first material cylinder
Net natural filtration flows out, and enters the second material cylinder；The mixture progress that natural filtration is gone out is filling, obtains component B.
In use, component A and B component are added sequentially to mix among reaction bulb, stir 15 minutes, under reduced pressure
Pumping 10 minutes, the bubble in reaction system is removed, 60 DEG C is then heated to, is taken out after 30 minutes, be cooled to room temperature, you can
Obtain the organosilicon adhesive with high-temperature stability.
Embodiment 8
Prepare component A：Aminated compounds N ' N-4, double 35 parts of the maleic amides of 4 '-diphenyl-methane type, ring are weighed with parts by weight
14 parts of the phenolic group ethane type epoxy resin of oxygen tree lipoid substance four, curing agent 4,6 parts of 4 '-MDA；It will weigh
Aminated compounds, epoxy resin compound, be added sequentially in the first material cylinder of mixer, start stirring (40rpm/
Min stirring 30 minutes) is maintained, adds curing agent afterwards, continues stirring 30 minutes under same rotational speed；By what is obtained by stirring
Mixture flows out from the first material cylinder by the filter screen natural filtration of 300~400 mesh, enters the second material cylinder；By natural filtration
The mixture progress gone out is filling, obtains component A.
Prepare component B：Hydrogen content is weighed as 30 parts of the hydrogeneous silicones of 0.15% phenyl, toughener polysulfide using parts by weight
5 parts of rubber, curing agent 4,6 parts of 4 '-MDA, platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane
0.08 part of complex compound；By the hydrogeneous silicones of the phenyl weighed, toughener, platinum catalyst sequentially adds the first material of mixer
In cylinder, start stirring (50rpm/min) and maintain stirring 30 minutes, add curing agent afterwards, continue 20 points of stirring under same rotational speed
Clock；The mixture obtained by stirring is flowed out from the first material cylinder by the filter screen natural filtration of 300-400 mesh, entered
Second material cylinder；The mixture progress that natural filtration is gone out is filling, obtains component B.
In use, by component A and B component according to 1：1 ratio is added sequentially among reaction bulb, is stirred 15 minutes, is subtracted
Press strip part lower pumping 10 minutes, the bubble in reaction system is removed, 60 DEG C is then heated to, is taken out after 30 minutes, be cooled to room
Temperature, you can obtain the organosilicon adhesive with high-temperature stability.
Organosilicon adhesive performance test after solidification：
Light transmittance, index determination
By the colourless transparent liquid that resulting component A and component B are mixed to get in above-mentioned implementation example, removed under reduced pressure gas
Bubble, then takes and is added separately on a small quantity in silica dish, be then heated to 60 DEG C, taken out after 20 minutes, be cooled to cold curing,
The test of light transmittance is carried out, uses instrument as the split type light transmittance tester devices of DRTG-81；By institute in above-mentioned implementation example
Obtain component A and component B and be mixed to get colourless transparent liquid, pressure-off bubble removing, then take it is a small amount of be respectively coated in long 10cm,
Wide 5cm, thick 2mm glass plate on, the thickness of the organosilicon adhesive of coating is 0.5mm, is then heated to 60 DEG C, 20 minutes
After take out, be cooled to cold curing, carry out the test of index of refraction, used instrument is DR-M4 multi-wavelength Abbe refractometers
(wavelength 589nm).Test result is as shown in table 1 below：
Organosilicon adhesive light transmittance, index determination after the solidification of table 1.
| Sample | There is bubble-free | Color | Light transmittance (%) | Index of refraction |
| Embodiment 1 | Nothing | Water white transparency | >99.0 | 1.4741 |
| Embodiment 2 | Nothing | Water white transparency | >99.0 | 1.4738 |
| Embodiment 3 | Nothing | Water white transparency | >99.0 | 1.4737 |
| Embodiment 4 | Nothing | Water white transparency | >99.0 | 1.4739 |
| Embodiment 5 | Nothing | Water white transparency | >99.0 | 1.4741 |
| Embodiment 6 | Nothing | Water white transparency | >99.0 | 1.4740 |
| Embodiment 7 | Nothing | Water white transparency | >99.0 | 1.4745 |
| Embodiment 8 | Nothing | Water white transparency | >99.0 | 1.4739 |
Resistance to elevated temperatures determines：
Colourless transparent liquid obtained by component A in above-mentioned implementation example and component B is mixed, removed under reduced pressure bubble, so
After be heated to 60 DEG C, taken out after 20 minutes, be cooled to cold curing, the organosilicon is then carried out in the range of 100~600 DEG C
The high temperature resistant measure of adhesive.As a result it is as shown in table 2 below：
Organosilicon adhesive resistance to elevated temperatures after table 2. solidifies is tested
In the above-mentioned preparation method that embodiments of the present invention are provided, the production production time of organosilicon adhesive is very
It is short, the raw material components weighed are sequentially added into the mixing of the first material cylinder and are stirred, work is produced with traditional organosilicon adhesive
Compared to being, the operating procedure can be carried out directly skill in the system of opening wide, it is not necessary to specific inert gas shielding or true
It is stirred under conditions of sky；In addition, the blending ingredients being stirred are passed through to the filter screen normal pressure of 300~400 mesh from the first material cylinder
The second material cylinder is filled into, is compared with the production technology of traditional organosilicon adhesive, the operating procedure natural filtration
Outflow, it is not necessary to extruding outflow.Thus, the preparation method of this kind of organic silicon adhesive had both simplified production stage, simultaneously
The whole production time is also saved, substantially increases production efficiency, and obtained organosilicon under production technology operation
Adhesive products have the performances such as very high refractive index, light transmittance and high temperature resistant.
Claims (10)
1. a kind of preparation method of high-temperature resistant silicone adhesive, it is characterised in that comprise the following steps：
Prepare component A：Weigh in parts by weight：20~50 parts of aminated compounds, 10~18 parts of epoxy resin compound and solid
5~10 parts of agent；Aminated compounds and epoxy resin compound are sequentially added in the first material cylinder of mixer and stirred, then
Curing agent is added, continues to stir；By obtained mixture from the first material cylinder through filter screen natural filtration to the second material cylinder；To second
Mixture in material cylinder is filling, obtains component A；
Prepare component B：Weigh in parts by weight：25~40 parts of the hydrogeneous silicones of phenyl, 3~6 parts of toughener, curing agent 5~10
0.009~0.1 part of part and platinum catalyst；The hydrogeneous silicones of phenyl, toughener, platinum catalyst are sequentially added the first of mixer
Stirred in material cylinder, then add curing agent, continue to stir；By obtained mixture from the first material cylinder through filter screen natural filtration to
Second material cylinder；It is filling to the mixture in the second material cylinder, obtain component B；
The component A and component B is mixed into solidify afterwards, that is, high-temperature resistant silicone adhesive is made.
2. the preparation method of high-temperature resistant silicone adhesive according to claim 1, it is characterised in that prepare component A and
In the step of preparing component B, it is described stirred in the first material cylinder with continue stirring speed it is identical, be 40~60rpm/min.
3. the preparation method of high-temperature resistant silicone adhesive according to claim 1, it is characterised in that prepare component A and
In the step of preparing component B, the time stirred in the first material cylinder and continue stirring is respectively 20~40 minutes.
4. the preparation method of high-temperature resistant silicone adhesive according to claim 1, it is characterised in that prepare component A and
In the step of preparing component B, the natural filtration uses 300~400 mesh filter screens.
5. the preparation method of high-temperature resistant silicone adhesive according to any one of claim 1 to 4, it is characterised in that
In the step of preparing component A, the aminated compounds is N ' N-4, the double maleic amides of 4 '-diphenyl-methane type.
6. the preparation method of the high-temperature resistant silicone adhesive according to any one of claims 1 to 4, its feature exist
In in the step of preparing component A, the epoxy resin compound is：Glycidyl ether type epoxy resin, glycidol esters
Epoxy resin, glycidyl amine epoxy resin, linear aliphatic epoxy resin or alicyclic based epoxy resin.
7. the preparation method of the high-temperature resistant silicone adhesive according to any one of claims 1 to 4, its feature exist
In in the step of preparing component B, the hydrogeneous silicones of phenyl includes one or several kinds of hydrogen contents 0.01~0.5%
Phenyl hydrogen containing siloxane.
8. the preparation method of the high-temperature resistant silicone adhesive according to any one of claims 1 to 4, its feature exist
In in the step of preparing component B, the toughener is carboxyl LNBR, polysulfide rubber, liquid silastic, polyethers, poly-
One or more in sulfone, nano-calcium carbonate and nano titanium oxide.
9. the preparation method of the high-temperature resistant silicone adhesive according to any one of claims 1 to 4, its feature exist
In, prepare component A and the step of prepare component B in, the curing agent is 4,4 '-MDA.
10. the preparation method of the high-temperature resistant silicone adhesive according to any one of claims 1 to 4, its feature exist
In in the step of preparing component B, the platinum catalyst is chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439212A (en) * | 2018-11-07 | 2019-03-08 | 合肥凯大新型材料科技有限公司 | A kind of carbon/carbon compound material low bulk adhesive |
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| CN103044918A (en) * | 2011-10-11 | 2013-04-17 | 中国科学院化学研究所 | Organosilicone resin/epoxy resin hybrid materials for packaging light emitting diodes |
| CN104804705A (en) * | 2015-05-06 | 2015-07-29 | 成都拓利化工实业有限公司 | Low release quantity additive halogen-free flame-retardant heat-conduction organic silicon pouring sealant and preparation method thereof |
| CN107022336A (en) * | 2017-04-10 | 2017-08-08 | 复旦大学 | A kind of organosilicon adhesive of modification and preparation method thereof |
| CN107118738A (en) * | 2017-05-11 | 2017-09-01 | 复旦大学 | A kind of ultraviolet aging resistance organosilicon adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103044918A (en) * | 2011-10-11 | 2013-04-17 | 中国科学院化学研究所 | Organosilicone resin/epoxy resin hybrid materials for packaging light emitting diodes |
| CN104804705A (en) * | 2015-05-06 | 2015-07-29 | 成都拓利化工实业有限公司 | Low release quantity additive halogen-free flame-retardant heat-conduction organic silicon pouring sealant and preparation method thereof |
| CN107022336A (en) * | 2017-04-10 | 2017-08-08 | 复旦大学 | A kind of organosilicon adhesive of modification and preparation method thereof |
| CN107118738A (en) * | 2017-05-11 | 2017-09-01 | 复旦大学 | A kind of ultraviolet aging resistance organosilicon adhesive and preparation method thereof |
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| CN109439212A (en) * | 2018-11-07 | 2019-03-08 | 合肥凯大新型材料科技有限公司 | A kind of carbon/carbon compound material low bulk adhesive |
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