CN106753121A - A kind of water boils easily separated crystal pro cessing modified epoxy and preparation method thereof - Google Patents
A kind of water boils easily separated crystal pro cessing modified epoxy and preparation method thereof Download PDFInfo
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- CN106753121A CN106753121A CN201611108457.XA CN201611108457A CN106753121A CN 106753121 A CN106753121 A CN 106753121A CN 201611108457 A CN201611108457 A CN 201611108457A CN 106753121 A CN106753121 A CN 106753121A
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- easily separated
- degumming
- modified epoxy
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
-
- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
Easily separated crystal pro cessing modified epoxy and preparation method thereof is boiled the invention discloses a kind of water, this modified epoxy is made up of first component, second component.Wherein first component contains epoxy resin, elastomer, degumming release agent, plasticizer, filler, thixotropic agent, and second component contains Polymercaptan curing agent, Tertiary amine accelerators, low molecular polyamides, silane coupler, degumming release agent, filler, thixotropic agent.When this glue is used for the processing of crystalline material positioning bonding, bonding force is strong, medium-resistance is good；When crystalline material completion heating degumming is separated, temperature is not high, cull is easy to cleaning.
Description
Technical field
Auxiliary material field is used the present invention relates to crystalline material processing, especially a kind of water boils easily separated crystal pro cessing with changing
Property epoxy glue and preparation method thereof.
Background technology
Material is the basis of human material's civilization, and since 21 century, crystalline material is used as microelectronics, photoelectron, logical
Critical material in the high-tech areas such as letter, space flight and modern military technology is paid attention to by countries in the world.It is brilliant with photoelectric functional
Body as development in Hi-Tech core material, with irreplaceable critical role.
Used with microelectronic industry and crystalline silicon used for solar batteries, LED (semiconductor) illuminations sapphire crystal, laser
Neodymium-doped yttrium-aluminum garnet crystal, the crystalline material that night vision device gallium arsenide is representative as optical glass, mostly fragility
Material, processing is positioned from the mechanical grip that machinery industry is commonly used, and easily causes workpiece to crush.Theoretically, vacuum suction
It is the best mode of disk on crystalline material, but vacuum absorption device gas circuit is complicated, and crystalline material is because of particular technique requirement difference
And face shape is changed greatly, it is impossible to customize special absorption seal for the different product of each face shape.Cemented in place adds
Work, though need degumming to separate after there is crystalline material completion, because of positioning bonding for face contacts, it is difficult to make crystal
Material is broken and deforms, it has also become the optimal selection of crystalline material positioning processing.Modified epoxy by epoxy resin, curing agent, change
Property the material composition such as agent, additive.When using, there is ring-opening polymerization in curing agent with epoxy resin, form network structure, from
And form bonding.Modified epoxy has that bonding force strong (shear strength is typically in more than 10MPa), shrinkage factor be small, user
Just, the advantages of resistant to chemical media, it has also become most commonly seen crystalline material positioning processing glue.
" bonding force is strong " is the necessary condition that modified epoxy is applied to crystalline material positioning processing.But modified epoxy compared with
Adhesive strength high is separated after govern crystalline material completion again from substrate.The system of " firmly viscous " with " easily separated " conflict
One, it is the maximum technological difficulties for restricting modified epoxy in crystalline material manufacture field application.High-temperature baking is that crystalline material is adopted
When with modified epoxy being positioning bonding glue, the most commonly used degumming separate mode.But not only energy resource consumption is big for high-temperature baking,
And baking is that the toxic and harmful for producing is big for environment pollution, what is more killed is if if gradient of temperature in baking process
Control is improper, easily causes hard and crisp crystalline material to rupture.Chinese patent ZL201110228621.1 and
The creative introducing surface-active in glue in ZL201210266587.1, by improving cured glue layer in aqueous
Dissolving, and reduce the difficulty of degumming separation, but when being processed under aqueous medium environment with glue-line, adhesive strength declines,
The reliable hidden danger for reducing of bonding.
The content of the invention
It is an object of the present invention to solve existing crystal pro cessing modified epoxy " it is viscous firm but separate it is difficult, separate easily but
Bonding is loosely " problem, there is provided one kind is easy to degumming separation, and bonding is reliable, and reliable, cull is bonded particularly in aqueous medium environment
Water easy to clean boils easily separated crystal pro cessing modified epoxy.
Easily separated crystal pro cessing modified epoxy is boiled the invention discloses a kind of water, it is characterised in that be by weight proportion
0.8~1.2:1 first component and second component composition；First component contains epoxy resin, elastomer, degumming release agent, plasticizer, fills out
Material, thixotropic agent, the ratio of weight and number of each component are as follows：60~100 parts of epoxy resin, 20~40 parts of elastomer, degumming release agent 0
~10 parts, 0~20 part of plasticizer, 0~20 part of filler, 0~10 part of thixotropic agent；Second component contains Polymercaptan curing agent, tertiary amine and promotees
Enter agent, low molecular polyamides, silane coupler, degumming release agent, filler, thixotropic agent, the ratio of weight and number of each component is as follows：
80~100 parts of Polymercaptan curing agent, 4~10 parts of Tertiary amine accelerators, 0~40 part of low molecular polyamides, silane coupler 1~5
Part, 5~20 parts of degumming release agent, 0~50 part of filler, 0~10 part of thixotropic agent.
The epoxy resin is one or more in bisphenol A epoxide resin, bisphenol F epoxy resin, novolac epoxy resin
Mixture;The elastomer is liquid polysulfide rubber, LNBR, hydroxy'terminated butadiene nitrile rubber, epoxy terminated butyronitrile rubber
The mixture of one or more in glue, liquid polyurethane rubber；The plasticizer be Phthalates, fatty acid ester,
The mixture of one or more in citric acid ester type, phosphoric acid ester, polyesters plasticizer.
The degumming release agent is the insoluble material that but swellable dissolves in the hot water of the cold water such as amylose, polyvinyl alcohol
In or several mixtures.
The mixing of one or more in calcium carbonate, silicon powder, titanium dioxide, metal powder, carbon black by granularity less than 300 mesh
Thing is added as filler, though part adhesive strength can be lost, can improve glue-line rigidity, and meeting the small use of processing displacement will
Ask.Added one or two the mixture in fumed silica, organobentonite as thixotropic agent, though can loss section
Point adhesive strength, but glue mobility can be reduced, meet gap it is larger when bonding requirements.
The Polymercaptan curing agent is the one kind or two in polyether-type Polymercaptan curing agent and polyester-type Polymercaptan curing agent
Kind mixture, Tertiary amine accelerators be one kind in adjacent (dimethylamino methyl) phenol, 2,4,6- tri- (dimethylamino) phenol or
Two kinds of mixture, the introducing of Tertiary amine accelerators can activate Polymercaptan curing agent and low molecular polyamides, accelerate epoxy systems
Curing rate；The silane coupler is the mixed of one or two in amino silicane coupling agent, epoxy silane coupling
Compound, the introducing of silane coupler can lift the water resistance of epoxy curing systems.
It is as follows that water of the present invention boils easily separated crystal pro cessing modified epoxy preparation method:
1st, the process that prepared by first component is as follows：Epoxy resin, elastomer, plasticizer are placed in reactor, in 40 DEG C~60 DEG C
Under be uniformly mixed, add filler, thixotropic agent and be well mixed；After being cooled to room temperature, add degumming release agent and mix
Uniformly;
2nd, the process that prepared by component B is as follows：Polymercaptan curing agent, low molecular polyamides, Tertiary amine accelerators are placed in reactor
In, it is uniformly mixed at 40 DEG C~60 DEG C, add filler, thixotropic agent and be well mixed；After being cooled to room temperature, silicon is added
Alkane coupling agent adds and degumming release agent and is well mixed.
Crystal pro cessing of the present invention modified epoxy quick solidifying, bonding are reliable, water-tolerant.Degumming is boiled by water to separate
When, degumming separates solvent swell and dissolves, and declines glue-line adhesive strength, and irreversible destruction glue-line, is separated beneficial to degumming
And cull cleaning.
Specific embodiment
Stop with reference to tool and implement example, the present invention is expanded on further.It will be appreciated that these embodiments are merely to illustrate this
Invention rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, this area skill
Various changes or modification that art personnel can make to the present invention, these equivalent form of values still fall within right appended by the present patent application will
Seek book limited range.
Embodiment 1（Weight ratio）
First component is formulated：
The liquid rubber 25 of 60 butyronitrile of E51 epoxy resin -40
The dibutyl phthalate (DBP) 15 of amylose 8
The organobentonite 8 of 500 mesh calcium carbonate 15
Component B is formulated：
3800 Polymercaptan curing agents of Capcure 60 2,4,6- tri- (dimethylamino) phenol 5
The amylose 10 of 651 daiamid epoxy curing agent 30
The A380 fume colloidal silicas 2 of R907 titanium dioxides 10
During preparation, E51 epoxy resin, the liquid rubber of butyronitrile -40, dibutyl phthalate (DBP) are placed in reactor by proportioning,
It is uniformly mixed at 40 DEG C~60 DEG C, adds 500 mesh calcium carbonate, organobentonite and be well mixed；It is cooled to room temperature
Afterwards, add amylose and be well mixed, it is standby as first component;By proportioning by the Polymercaptan curing agents of Capcure 3800,651
Daiamid epoxy curing agent, 2,4,6- tri- (dimethylamino) phenol are placed in reactor, are mixed in being stirred at 40 DEG C~60 DEG C
Uniformly, A380 fume colloidal silicas, R907 titanium dioxides are added and is well mixed；After being cooled to room temperature, amylose is added simultaneously
It is well mixed, it is standby as second component.When using, by first：Second=0.9:1（Weight ratio）It is well mixed to can be used for sapphire crystalline substance
The positioning bonding of body jacking, with quick solidifying, bonding is reliable the characteristics of.Boiled with hot water when tearing glue open, you can tear glue open and remove residual
Glue.
Embodiment 2（Weight ratio）
First component is formulated：
The F46 epoxy resin 30 of E51 epoxy resin 60
The mesh silicon powder 5 of JLY121 polysulfide rubber 35 500
A200 fume colloidal silicas 5
Component B is formulated：
Adjacent (dimethylamino methyl) phenol 8 of EH-316 Polymercaptan curing agents 60
The polyvinyl alcohol 15 of 650 daiamid epoxy curing agent 30
The A380 fume colloidal silicas 2 of R907 titanium dioxides 10
During preparation, E51 epoxy resin, F46 epoxy resin, JLY121 polysulfide rubber are placed in reactor by proportioning, in 40 DEG C
It is uniformly mixed at~60 DEG C, adds 500 mesh silicon powders, A200 fume colloidal silicas and be well mixed；It is cooled to room temperature
It is standby as first component.By proportioning by EH-316 Polymercaptan curing agents, 650 daiamid epoxy curing agents, neighbour's (dimethylamino first
Base) phenol is placed in reactor, is uniformly mixed at 40 DEG C~60 DEG C, adds A380 fume colloidal silicas, R907 titanium whites
Powder is simultaneously well mixed；After being cooled to room temperature, add polyvinyl alcohol and be well mixed, it is standby as second component.When using, by first：
Second=1:1（Weight ratio）Well mixed is positioning bonding when can be used for round as a ball sapphire crystal and polysilicon evolution, with solid
The advantage for change fast, bonding reliability, being heated to after 100 DEG C being easy to tear open glue.
Embodiment 3（Weight ratio）
First component is formulated：
The epoxy terminated nitrile rubbers 25 of the CHX100 of E51 epoxy resin 80
The tri-n-butyl citrate 15 of amylose 5
Component B is formulated：
3800 Polymercaptan curing agents of Capcure 100 2,4,6- tri- (dimethylamino) phenol 3
The adjacent polyvinyl alcohol 10 of (dimethylamino methyl) phenol 2
During preparation, E51 epoxy resin, the epoxy terminated nitrile rubbers of CHX100, the positive fourth fat of citric acid are placed in reactor by proportioning
In, it is uniformly mixed at 40 DEG C~60 DEG C；After being cooled to room temperature, add amylose and be well mixed, as first component
It is standby.The Polymercaptan curing agents of Capcure 3800,2,4,6- tri- (dimethylamino) phenol are placed in reactor by proportioning, in
It is uniformly mixed at 40 DEG C~60 DEG C；After being cooled to room temperature, add polyvinyl alcohol and be well mixed, it is standby as second component.
When using, by first：Second=1.1:1（Weight ratio）Well mixed is that positioning when can be used for sapphire crystal and polysilicon section is glued
Connect, have the advantages that quick solidifying, bonding is reliable, be heated to 90 DEG C after be easy to tear glue open.
Claims (8)
1. a kind of water boils easily separated crystal pro cessing modified epoxy, it is characterised in that:It is 0.8~1.2 by weight proportion:1
First component and second component are constituted；The first component contains epoxy resin, elastomer, degumming release agent, plasticizer, filler, thixotroping
Agent, the ratio of weight and number of each component is as follows：60~100 parts of epoxy resin, 20~40 parts of elastomer, 0~10 part of degumming release agent,
0~20 part of plasticizer, 0~20 part of filler, 0~10 part of thixotropic agent；The second component contains Polymercaptan curing agent, tertiary amine and promotes
Agent, low molecular polyamides, silane coupler, degumming release agent, filler, thixotropic agent, the ratio of weight and number of each component are as follows：It is poly-
80~100 parts of polythiol hardener, 4~10 parts of Tertiary amine accelerators, 0~40 part of low molecular polyamides, degumming release agent 5~20
Part, 0~50 part of filler, 0~10 part of thixotropic agent.
2. water according to claim 1 boils easily separated crystal pro cessing modified epoxy, it is characterised in that the asphalt mixtures modified by epoxy resin
Fat is the mixture of one or more in bisphenol A epoxide resin, bisphenol F epoxy resin, novolac epoxy resin.
3. water according to claim 1 boils easily separated crystal pro cessing modified epoxy, it is characterised in that the elastomer
For in liquid polysulfide rubber, LNBR, hydroxy'terminated butadiene nitrile rubber, epoxy terminated nitrile rubber, liquid polyurethane rubber
The mixture of one or more；The plasticizer be Phthalates, fatty acid ester, citric acid ester type, phosphoric acid ester,
The mixture of one or more in polyesters plasticizer.
4. water according to claim 1 boils easily separated crystal pro cessing modified epoxy, it is characterised in that the degumming point
It is the mixture of one or more in amylose, polyvinyl alcohol from agent.
5. water according to claim 1 boils easily separated crystal pro cessing modified epoxy, it is characterised in that described filler is
Granularity is less than the mixture of one or more in calcium carbonate, silicon powder, titanium dioxide, metal powder, the carbon black of 300 mesh；It is described to touch
Change agent is one or two the mixture in fumed silica, organobentonite.
6. water according to claim 1 boils easily separated crystal pro cessing modified epoxy, it is characterised in that the polymercaptan
Curing agent is one or two the mixture in polyether-type Polymercaptan curing agent and polyester-type Polymercaptan curing agent.
7. water according to claim 1 boils easily separated crystal pro cessing modified epoxy, it is characterised in that the tertiary amine promotees
It is one or two the mixture in adjacent (dimethylamino) phenol, 2,4,6- tri- (dimethylamino) phenol to enter agent；It is described
Silane coupler is one or two the mixture in amino silicane coupling agent, epoxy silane coupling.
8. a kind of water boils the preparation method of easily separated crystal pro cessing modified epoxy, it is characterised in that the preparation method is such as
Under:
（1）First component preparation process is as follows：Epoxy resin, elastomer, plasticizer are placed in reactor, at 40 DEG C~60 DEG C
It is uniformly mixed, adds filler, thixotropic agent and be well mixed；After being cooled to room temperature, add degumming release agent and mix equal
It is even;
（2）Component B preparation process is as follows：Polymercaptan curing agent, low molecular polyamides, Tertiary amine accelerators are placed in reactor
In, it is uniformly mixed at 40 DEG C~60 DEG C, add filler, thixotropic agent and be well mixed；After being cooled to room temperature, add de-
Glue release agent is simultaneously well mixed.
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| CN201611108457.XA CN106753121A (en) | 2016-12-06 | 2016-12-06 | A kind of water boils easily separated crystal pro cessing modified epoxy and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108624268A (en) * | 2018-04-16 | 2018-10-09 | 杭州电子科技大学 | A kind of solar silicon wafers manufacture composite material |
| CN109321185A (en) * | 2018-10-12 | 2019-02-12 | 南宁珀源能源材料有限公司 | Can boiling degumming bar glue and preparation method thereof |
| CN111873200A (en) * | 2020-07-15 | 2020-11-03 | 中锗科技有限公司 | Method for improving yield of rounding of germanium/silicon infrared crystal |
| CN112210331A (en) * | 2020-09-29 | 2021-01-12 | 晶科能源有限公司 | Solar crystal bar bottom plate glue, preparation method thereof and solar crystal bar cutting method |
| CN112940658A (en) * | 2021-02-01 | 2021-06-11 | 南宁珀源能源材料有限公司 | Stick glue and preparation method and application thereof |
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| CN112210331B (en) * | 2020-09-29 | 2022-02-25 | 晶科能源股份有限公司 | Solar crystal bar bottom plate glue, preparation method thereof and solar crystal bar cutting method |
| CN112940658A (en) * | 2021-02-01 | 2021-06-11 | 南宁珀源能源材料有限公司 | Stick glue and preparation method and application thereof |
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Application publication date: 20170531 |