CN106554736B - A kind of ceramic and elastomer bonded heat cure adhesive - Google Patents
A kind of ceramic and elastomer bonded heat cure adhesive Download PDFInfo
- Publication number
- CN106554736B CN106554736B CN201610998043.2A CN201610998043A CN106554736B CN 106554736 B CN106554736 B CN 106554736B CN 201610998043 A CN201610998043 A CN 201610998043A CN 106554736 B CN106554736 B CN 106554736B
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- ceramics
- heat cure
- silane
- cure adhesive
- elastomer bonded
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Classifications
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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
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09J161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- 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
-
- 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
- C09J115/00—Adhesives based on rubber derivatives
- C09J115/02—Rubber derivatives containing halogen
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of ceramics and elastomer bonded heat cure adhesives, this heat cure adhesive includes following components: phenolic resin 5-15%, film forming agent 5-15%, additional formaldehyde source 0.5-5%, acid absorbent 0.5-5%, adhesion promoters 5-10%, balance of solvent by weight percentage.Biggest feature of the invention is to contain silane-modified inorganic porous material support phenolic compounds as adhesion promoters, so that adhesive is formed a high-intensitive high reaction activity transition zone between elastomer and hard ceramic, effectively realizes adhesive to the bonding of high strength hard ceramics.
Description
Technical field
The present invention relates to a kind of heat cure adhesive containing silane-modified phenolic resin and super hard filler, the adhesive
It is used when for bonding ceramics and elastomer as primer.
Technical background
Many Adhesive compositions for providing and being bonded such as elastomer and metal base have been provided on the market.Usual steel
The Mohs' hardness of iron is in 4-5 or so, and the Mohs hard of normal silicate ceramics is just more than 8, pure alumina and zirconia ceramics
Hardness is more up to 9, and for the metal bases such as steel, the requirement of ceramic base material bonding is higher.
In bonding mechanism, substrate bonding two big effect nothing more than, first is that physical action, including infiltration, anchoring, absorption etc.
Deng；Second is that chemical action, the i.e. reaction with substrate surface active group.So for the bonding of hard ceramic substrate, adhesive
Physical property in terms of such as hardness must be close to ceramic base material；Then need in terms of chemical property can promptly with ceramic surface
Such as hydroxyl isoreactivity group reacts.Traditional heat cure adhesive is difficult to meet the two requirements simultaneously, leads to hard
The bonding of ceramic base material becomes industry problems.
The CN94194821.8 of Lord Corp. discloses a kind of priming paint and adhesive based on chlorinated polyolefins having high chlorine contents
Composition, the adhesive contain following component: a) chlorinated rubber；B) phenolic resin；C) curing agent；D) acid absorbent；E) pigments and fillers.
The invention has metal base extremely outstanding adhesive effect.
The CN201310443270 of Zhuzhou Time Inc. discloses a kind of heat cure adhesive and preparation method thereof, the gluing
Agent has following components: a) phenolic aldehyde/epoxy；B) promotor；C) halogenated polyolefin；D) co-vulcanization ingredient；E) metal oxide；F) attached
Adhesion promoter；G) wetting dispersing agent；H) inert filler.The invention has preferable effect for bonded metal substrate and natural rubber
Fruit.
The CN201110029305 of Anhui Zhong Ding company discloses a kind of phenolic-nitrile rubber hot vulcanized adhesive and its system
Preparation Method, the adhesive have following ingredient: a) nitrile rubber；B) phenolic resin；C) inorganic filler；D) vulcanizing agent；E) thickening tree
Rouge；F) coupling agent；G) anti-aging agent；H) solvent.The invention has preferable effect for bonded metal substrate and nitrile rubber.
And currently, certain fields are higher and higher to the hardness and strength requirement of ceramic base material.Such as ceramic lining plate industry,
Such product is to be integrated ceramics and rubber by heat cure adhesive bonding by Vulcanization to be made, and has the wear and shock-resistant of ceramics concurrently
The damping performance of performance and rubber is widely used in fields such as mining splicing dampings.In the whole work process of liner plate, constantly
By the impact of mud and slag, normal silicate ceramics lead to wearability and fatigue durability not since hardness and strength are inadequate
Good, service life is very limited, often needs to replace.In order to preferably adapt to the demand of these industries, each liner plate production firm
Start to transfer the more excellent ceramic material of service performance, design parameter is as follows:
As can be seen from the table, relative to conventional ceramic, aluminium oxide ceramics and zirconia ceramics have apparent hardness and
Advantage in terms of intensity, and these performances are most important in ceramic lining plate industry, can be obviously improved the service life of its product.
And currently, commercially available heat cure adhesive is difficult to realize good bonding to such hard high-strength ceramics, at this
Under kind of trend, it is necessary to which the adhesive of more preferable performance meets the bonding demand to hard ceramic.
Summary of the invention
In order to solve prior art problem, the present invention provides a kind of bottoms Nian Jie with elastomer dedicated for ceramic base material
Glue solution.Firstly, the characteristics of inorganic porous material that the present invention chooses all has hard high-strength, especially preferably
Zirconium oxide porous microsphere (design parameter is seen the above table), reinforcing effect is much better than common pigments and fillers (such as titanium white when as filler
Powder: HRC66；Calcium carbonate: HRC57)；Secondly, the present invention uses high activity (more reactive groups) silane treatment inorganic porous material,
Adhesion promoters are made in the phenolic compounds (preferably tri hydroxy methyl phenol) of strong reactivity in support, can be with the hydroxyl of ceramic surface
Isoreactivity group generates quickly reaction；Then, fine and close filler systems then by the way of the cooperation of big small particle are formed, greatly
Raising adhesive solidify after hardness and strength, so that its physicochemical property is more adapted to the bonding of ceramic base material.In summary a variety of
Scheme, the present invention perfectly solve the problems, such as the bonding of hard ceramic substrate.
The purpose of the present invention is to provide a kind of heat cure adhesive for bonding ceramic base material and elastomer, maximum spies
Sign is the adhesion promoters containing silane-modified porous inorganic filling materials support phenolic compounds.
The contents of the present invention include:
A kind of ceramic and elastomer bonded heat cure adhesive includes by weight percentage following components:
In some embodiments, by weight percentage, include following components:
In some embodiments, the film forming agent is selected from chlorinated natural rubber, high chlorination neoprene, chlorinated polyethylene
One of alkene, chlorinated polypropylene, chlorosulfonated polyethylene, chlorinated scoline.
In some embodiments, the additional formaldehyde source is selected from paraformaldehyde, acetal homopolymer, hexa-methylene four
One of amine, 2- polymethoxy dimethyl ether.
In some embodiments, the acid absorbent is zinc oxide or magnesia.
In some preferred embodiments, the acid absorbent is zinc oxide.
In some embodiments, the adhesion promoters are silane-modified porous inorganic filling materials support phenolic compounds.
In some embodiments, the silane in the silane-modified porous inorganic filling materials support phenolic compounds is selected from 3- ammonia
Propyl trimethoxy silicane, 1- aminopropyl triethoxysilane, 3- glycidyl ether oxypropyltrimethoxysilane, γ-first
Base acryloyloxypropyltrimethoxysilane, vinyltriethoxysilane, vinyltrimethoxysilane, N- (β-ammonia second
Base)-gamma-aminopropyl-triethoxy-silane, N- β-(aminoethyl)-γ aminopropyl trimethoxysilane, 3- aminopropyl trimethoxy
One of silane, methyltriethoxysilane.
In some embodiments, the porous inorganic filling materials in the silane-modified porous inorganic filling materials support phenolic compounds
Selected from one of zirconium silicate, alumina silicate, aluminium oxide, silica, zirconium oxide, silicon carbide, glass micro mist, Nano diamond.
In some preferred embodiments, the porous nothing in the silane-modified porous inorganic filling materials support phenolic compounds
Machine filler is zirconium oxide porous microsphere.
In some preferred embodiments, zirconium oxide porous microsphere is partial size 5nm and 2 μm of mixing.
In some embodiments, the phenolic compounds in the silane-modified porous inorganic filling materials support phenolic compounds is selected from
Phenol, p-tert-butylphenol, o-cresol, metacresol, resorcinol, tri hydroxy methyl phenol, m -bromoacetophenone, one in parachlorophenol
Kind.Further preferred tri hydroxy methyl phenol.
In some embodiments, the solvent is selected from one of aromatic hydrocarbons, ketones solvent or ether solvent.
The specific example of the aromatic hydrocarbons, including but not limited to: dimethylbenzene, toluene, ethylbenzene.
The specific example of the ketones solvent, including but not limited to: methyl ethyl ketone, methyl iso-butyl ketone (MIBK), cyclohexanone.
The specific example of the ether solvent, including but not limited to: ethylene glycol monomethyl ether, ethylene glycol ethyl ether.
In some preferred embodiments, the solvent is methyl iso-butyl ketone (MIBK).
In some embodiments, the preparation method of the adhesion promoters is comprised the steps of: porous inorganic filling materials
It is soaked in 70 DEG C of 30wt% silane coupling agent/acetone soln 4 hours, 50 DEG C of tri- hydroxyl of 20wt% is soaked in after filtering drying
2 hours in methylphenol/toluene solvant, up to adhesion promoters after drying.
Biggest feature of the invention is that contain silane-modified inorganic porous material support phenolic compounds promotees as bonding
Into agent, so that adhesive is formed a high-intensitive transition zone between elastomer and hard ceramic, promote adhesive to high-strength rigid
The bonding of matter ceramics.
Specific embodiment
Above explanation and the following examples is for disclosure and to illustrate the present invention, wherein each ingredient
Specific dosage and combination be not limited to by the scope of the present invention of claims defined.
(1) adhesion promoters
Silane-modified inorganic porous material support phenolic compounds of the invention is prepared according to the following steps:
Porous inorganic filling materials are soaked in 70 DEG C 30wt%N- β-(aminoethyl)-γ aminopropyl trimethoxysilane/the third
It 4 hours in ketone solution, is soaked in after filtering drying in 50 DEG C of 20wt% tri hydroxy methyl phenol/toluene solvant 2 hours, after dry
Up to adhesion promoters.
The corresponding formula serial number of adhesion promoters is as follows:
| Serial number | 1 | 2 | 3 |
| Adhesion promoters | Ad.1 | Ad.2 | Ad.3 |
It is ground in KD mill with silane-modified inorganic porous material support phenolic compounds obtained with following ingredient, until
Heat cure adhesive of the invention is obtained behind fineness < 10 μm.
(2) Adhesive composition
In order to make sample, degreasing need to be carried out to potsherd with methyl iso-butyl ketone (MIBK), uses three kinds of potsherd conducts here
The substrate of bonding: normal silicate ceramics, aluminium oxide ceramics and zirconia ceramics.Potsherd is according to according to GB/T7760-2003
Requirement preparation, with a thickness of 1.5mm ± 0.1mm, width 25mm ± 0.1mm of potsherd, length is 60mm ± 1mm.Applying
Before adhesive, the 17.5mm and 17.5mm for covering test specimen two ends are left with preventing the region to can be used for being bonded on rubber
The central area of 25mm long and 25mm ± 0.1mm wide is adhered on rubber with providing.Then the potsherd is coated about 5-10 μm
The heat cure adhesive of the example 1-26 of (drying layer thickness) thickness.
It is (normal on the market in film surface coated side glue Chemlok220 after drying at room temperature or at a certain temperature
Heat cure glue surface glue), bonding hot vulcanization test is carried out with natural rubber after drying again, while comparing Lord Corp. in parallel
Primer chemlok205, the Dow Chemical Company primer Thixon p-11 adhesive effect.
By unvulcanized natural rubber be placed in it is each apply in the test piece that installs, and vulcanize under 150 DEG C, the pressure of 5MPa
30min。
After vulcanization, the sample through being bonded is placed 24 hours at room temperature, carries out peel test later.
" coverage " is the remaining rubber percentage on the metal substrate of bonding after peel test.100% rubber
Destruction, which refers to when rubber destroys completely, does not have rubber part to peel off from metal surface.
Then by bonding potsherd --- natural rubber component is made 90 ° of angle removings according to GB/T 7760-2003 and is surveyed
Examination, " coverage " after record test.
Formula listed above, as a result as follows:
As can be seen that inorganic porous material support phenolic compounds silane-modified in the present invention from the above formula and result
Adhesive can be effectively promoted to the adhesive effect of hard ceramic, when selecting more excellent formula, the present invention is to aluminium oxide and oxygen
The adhesive effect for changing zircon ceramic is much better than commercially available product.
Claims (9)
1. a kind of ceramics and elastomer bonded heat cure adhesive, which is characterized in that by weight percentage, comprising with the following group
Point:
The adhesion promoters are silane-modified porous inorganic filling materials support phenolic compounds；
Porous inorganic filling materials in the silane-modified porous inorganic filling materials support phenolic compounds are zirconium oxide porous microsphere；
The zirconium oxide porous microsphere is partial size 200nm and 2 μm of mixing.
2. ceramics as described in claim 1 and elastomer bonded heat cure adhesive, which is characterized in that by weight percentage
Meter includes following components:
3. ceramics as claimed in claim 1 or 2 and elastomer bonded heat cure adhesive, which is characterized in that it is described at
Film is selected from chlorinated natural rubber, high chlorination neoprene, haloflex, chlorinated polypropylene, chlorosulfonated polyethylene, chlorination fourth
One of base rubber.
4. ceramics as claimed in claim 1 or 2 and elastomer bonded heat cure adhesive, which is characterized in that the volume
Outer formaldehyde source is selected from one of paraformaldehyde, acetal homopolymer, hexa, 2- polymethoxy dimethyl ether.
5. ceramics as claimed in claim 1 or 2 and elastomer bonded heat cure adhesive, which is characterized in that the suction
Sour agent is zinc oxide or magnesia.
6. ceramics as described in claim 1 and elastomer bonded heat cure adhesive, which is characterized in that described silane-modified
Silane in porous inorganic filling materials support phenolic compounds is selected from 3- aminopropyl trimethoxysilane, 3- aminopropyl-triethoxy silicon
Alkane, 3- glycidyl ether oxypropyltrimethoxysilane, γ-methacryloxypropyl trimethoxy silane, vinyl
Triethoxysilane, vinyltrimethoxysilane, N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane, N- β-(ammonia second
Base)-γ aminopropyl trimethoxysilane, one of methyltriethoxysilane.
7. ceramics as described in claim 1 and elastomer bonded heat cure adhesive, which is characterized in that described silane-modified
Phenolic compounds in porous inorganic filling materials support phenolic compounds is selected from phenol, p-tert-butylphenol, o-cresol, metacresol, isophthalic
One of diphenol, tri hydroxy methyl phenol, m -bromoacetophenone, parachlorophenol.
8. ceramics as claimed in claim 1 or 2 and elastomer bonded heat cure adhesive, which is characterized in that the solvent
Selected from one of aromatic hydrocarbons, ketones solvent or ether solvent.
9. ceramics as described in claim 1 and elastomer bonded heat cure adhesive, which is characterized in that the adhesion promoter
The preparation method of agent, which comprises the steps of:, is soaked in porous inorganic filling materials 70 DEG C of 30wt% silane coupling agent/acetone soln
In 4 hours, be soaked in after filtering drying in 50 DEG C of 20wt% tri hydroxy methyl phenol/toluene solvant 2 hours, it is dry after up to viscous
Connect promotor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610998043.2A CN106554736B (en) | 2016-11-14 | 2016-11-14 | A kind of ceramic and elastomer bonded heat cure adhesive |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610998043.2A CN106554736B (en) | 2016-11-14 | 2016-11-14 | A kind of ceramic and elastomer bonded heat cure adhesive |
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| CN106554736A CN106554736A (en) | 2017-04-05 |
| CN106554736B true CN106554736B (en) | 2019-09-06 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109161368B (en) * | 2018-09-07 | 2021-04-09 | 宁波普力通化学有限公司 | Hot vulcanization adhesive |
| CN115058221B (en) * | 2021-08-25 | 2024-06-07 | 安徽普力通新材料科技有限公司 | Special high-flexibility hot vulcanized adhesive for bonding easily-deformed base materials |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141643A (en) * | 1994-01-11 | 1997-01-29 | 劳德公司 | Primer and adhesive compositions based on chlorinated polyolefins having high chlorine contents |
| CN101368076A (en) * | 2008-10-01 | 2009-02-18 | 瑞阳汽车零部件（仙桃）有限公司 | High-efficiency adhesion agent for automobile brake flat and preparation method thereof |
| CN101497773A (en) * | 2009-01-24 | 2009-08-05 | 黑龙江省科学院石油化学研究院 | Undercoat adhesive for bonding hot vulcanization and preparation thereof |
| CN103074009A (en) * | 2013-01-24 | 2013-05-01 | 上海普力通新材料科技有限公司 | Adhesion promoter for bonding elastomers and metals and adhesive composition |
-
2016
- 2016-11-14 CN CN201610998043.2A patent/CN106554736B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141643A (en) * | 1994-01-11 | 1997-01-29 | 劳德公司 | Primer and adhesive compositions based on chlorinated polyolefins having high chlorine contents |
| CN101368076A (en) * | 2008-10-01 | 2009-02-18 | 瑞阳汽车零部件（仙桃）有限公司 | High-efficiency adhesion agent for automobile brake flat and preparation method thereof |
| CN101497773A (en) * | 2009-01-24 | 2009-08-05 | 黑龙江省科学院石油化学研究院 | Undercoat adhesive for bonding hot vulcanization and preparation thereof |
| CN103074009A (en) * | 2013-01-24 | 2013-05-01 | 上海普力通新材料科技有限公司 | Adhesion promoter for bonding elastomers and metals and adhesive composition |
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| CN106554736A (en) | 2017-04-05 |
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Denomination of invention: A hot vulcanized adhesive for bonding ceramics and elastomers Effective date of registration: 20230605 Granted publication date: 20190906 Pledgee: Industrial Bank Co.,Ltd. Shanghai Jinqiao Branch Pledgor: SHANGHAI POLYTON NEW MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2023310000227 |