CN108314977B - A kind of aqueous fluorubber lotion adhesive and preparation method thereof - Google Patents
A kind of aqueous fluorubber lotion adhesive and preparation method thereof Download PDFInfo
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- CN108314977B CN108314977B CN201810240817.4A CN201810240817A CN108314977B CN 108314977 B CN108314977 B CN 108314977B CN 201810240817 A CN201810240817 A CN 201810240817A CN 108314977 B CN108314977 B CN 108314977B
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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
- C09J127/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Adhesives based on derivatives of such polymers
- C09J127/02—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J127/12—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Adhesives based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5006—Amines aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5046—Amines heterocyclic
- C08G59/5053—Amines heterocyclic containing only nitrogen as a heteroatom
- C08G59/506—Amines heterocyclic containing only nitrogen as a heteroatom having one nitrogen atom in the ring
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- 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
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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
- C09J11/06—Non-macromolecular additives organic
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- 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
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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- 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
- 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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
- C08L2312/00—Crosslinking
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Abstract
A kind of aqueous fluorubber lotion adhesive and preparation method thereof, it belongs to adhesive preparation technical field.The present invention is mainly by 95~105 parts of non-volatile part parts by weight of aqueous fluorubber lotion, 10~30 parts of aqueous epoxy resins, 3~9 parts of amine hardener, 1~3 part of acid absorbent, 0~5 part of emulsion film forming auxiliary agent is made, the amine hardener is water-soluble or water-dispersible amine hardener, acid absorbent is light magnesium oxide, zinc oxide, calcium oxide, the mixture of one of calcium hydroxide or its corresponding aqueous dispersions or in which several compositions, emulsion film forming auxiliary agent is ethylene glycol, butyl glycol ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, propandiol butyl ether, dipropylene glycol monopropyl ether, Dipropylene glycol mono-n-butyl Ether, N, N- dimethyl acetamide, the mixture of one of N-Methyl pyrrolidone or in which several compositions.The present invention is suitable with solvent type fluorubber adhesive strength, VOC content 1%~4%.
Description
Technical field
The invention belongs to adhesive preparation technical fields；More particularly to a kind of aqueous fluorubber lotion adhesive and its preparation
Method.
Background technique
In recent years, as people are to the increasingly strong of environmental protection requirement, without volatile organic compounds (VOC) or low
VOC system has become the research direction of new material.Conventional fluoroelastomeric adhesive is that fluororubber compounded rubber is dissolved in ester, ketone etc.
In solvent, the modifying agent such as tackifier resins, curing agent are added, can prepare with the excellent properties such as high temperature resistant, oil resistant, ageing-resistant
Adhesive and coating products, these products are widely used in fluorine adhesive plaster, fluorine adhesive plaster and Anodising aluminium alloy, fluorine adhesive plaster and chromium plating
Steel, glass cloth with it is bonding between Anodising aluminium alloy, high silicon oxygen cloth and Anodising aluminium alloy.But such product, which contains, largely to be had
Solvent, there are danger inflammable, explosive, toxic to human body.Therefore, to the research of high performance fluorine rubber adhesive Water-borne modification
It is of great significance.
About aqueous fluorubber lotion existing research.For example Japan Patent has studied one kind and contains fluorubber, fluororesin, sulphur
The aqueous fluorubber vulcanisable compound of agent, wherein poly- ammonia system vulcanizing agent or polyalcohol system vulcanizing agent can be selected in vulcanizing agent,
In addition to this also contain surfactant and organic solvent.When forming film with this water composition, fluororesin is largely exuded to painting
The durability or non-adhesive of film can be improved in the surface of film.United States Patent (USP) reports a kind of aqueous fluorine rubber coating, by
Two groups are grouped as, and component A is a kind of fluorubber lotion, and B component is a kind of amino silane compounds, and amino-compound is at least
One end amino group directly with fatty chain link, formula in be additionally added a kind of reinforced filling and a kind of acid absorbent.The U.S. Ling You
A kind of curable fluorubber lotion of patent report includes fluorubber in material of main part fluorubber lotion, surfactant, inhales acid
Agent and a kind of salt.The curing agent of fluorubber aqueous dispersions mainly selects ammonia type curing agent, bisphenol type curing agent, peroxide type solid
Agent.Saint-Gobain's modeling industry in the U.S. and Lao Lun Internaional, Inc have developed jointly a kind of novel aqueous fluorine rubber coating production
Product, it is a kind of VOC free material, according to the difference of curing system form, can be divided into heat cured system, Storage period is at least 3
A month one-component；System Curing At Room Temperature, the two-component that Storage period is 12 days.This coating has as fluorubber material
Temperature tolerance, resistant to chemical media, corrosion-resistant, abrasion resistance properties.It can be coated in the surface of many materials, including rubber, fiber, modeling
Material, metal etc., and do not need priming agent.A kind of fluorubber lotion of Shandong Eastern Mountain new material exploitation, mainly by vinylidene and
Hexafluoropropene combined polymerization is made.This fluorubber lotion can be used in coated cloth, and coated cloth may make to have brilliant resistance toization
The performances such as product, oil resistant, heatproof.
It can be seen that the emulsion modified research of aqueous fluorubber is mainly coatings art, the related modified aqueous cream of fluorubber
The research of liquid adhesive has not been reported.
Summary of the invention
It is an object of the present invention to provide a kind of aqueous fluorubber lotion adhesives and preparation method thereof.
The invention is realized by the following technical scheme:
A kind of aqueous fluorubber lotion adhesive, the aqueous fluorubber lotion adhesive is mainly by aqueous fluorubber
Lotion, aqueous epoxy resins, amine hardener, acid absorbent, emulsion film forming auxiliary agent are made, and non-volatile part parts by weight are respectively 95
~105 parts of aqueous fluorubber lotion, 10~30 parts of aqueous epoxy resins, 3~9 parts of amine hardener, 1~3 part of suction acid
Agent, 0~5 part of emulsion film forming auxiliary agent, the amine hardener are water-soluble or water-dispersible amine hardener, the suction acid
Agent is one of light magnesium oxide, zinc oxide, calcium oxide, calcium hydroxide or its corresponding aqueous dispersions or in which several compositions
Mixture, the emulsion film forming auxiliary agent be ethylene glycol, butyl glycol ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, propylene glycol fourth
One of ether, dipropylene glycol monopropyl ether, Dipropylene glycol mono-n-butyl Ether, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone or its
In several compositions mixture.
A kind of aqueous fluorubber lotion adhesive of the present invention, it is aqueous in the aqueous fluorubber lotion adhesive
Non-volatile part parts by weight of fluorubber lotion are 95 parts, and non-volatile part parts by weight of aqueous epoxy resins are 10 parts, and amine is solid
Non-volatile part parts by weight of agent are 3 parts, and non-volatile part parts by weight of acid absorbent are 1 part, the weight of emulsion film forming auxiliary agent
Number is 1 part.
A kind of aqueous fluorubber lotion adhesive of the present invention, it is aqueous in the aqueous fluorubber lotion adhesive
Non-volatile part parts by weight of fluorubber lotion are 105 parts, and non-volatile part parts by weight of aqueous epoxy resins are 30 parts, and amine is solid
Non-volatile part parts by weight of agent are 9 parts, and non-volatile part parts by weight of acid absorbent are 3 parts, the weight of emulsion film forming auxiliary agent
Number is 5 parts.
A kind of aqueous fluorubber lotion adhesive of the present invention, it is aqueous in the aqueous fluorubber lotion adhesive
Non-volatile part parts by weight of fluorubber lotion are 100 parts, and non-volatile part parts by weight of aqueous epoxy resins are 20 parts, and amine is solid
Non-volatile part parts by weight of agent are 5 parts, and non-volatile part parts by weight of acid absorbent are 2 parts, the weight of emulsion film forming auxiliary agent
Number is 3 parts.
The group of a kind of aqueous fluorubber lotion adhesive of the present invention, the fluorubber lotion becomes mass fraction
15~30% fluorubber, 0.5~2.0% emulsifier, surplus are distilled water, and the fluorubber is vinylidene and hexafluoro
Fluorubber made from copolymerization of propylene, the emulsifier are condensation compound of alkyl phenol and epoxy ethane OP-10 emulsifier.
A kind of aqueous fluorubber lotion adhesive of the present invention, the aqueous epoxy resins include soluble epoxide
Resin, nonionic external emulsion epoxy resin emulsion, the preparation of modified nonionic emulsifier one of epoxy resin latex or its
In several compositions mixture, including aqueous epoxy resins MHR-36, epoxy resin of aqueous phenolic aldehyde BH652 lotion, water-base epoxy
Resin H220A, aqueous epoxy resins E-20 lotion.
A kind of aqueous fluorubber lotion adhesive of the present invention, the amine hardener are m-phenylene diamine (MPD), diamino
Diphenyl-methane, N, the bis- cortex cinnamomi fork -1,6- hexamethylene diamines of N-, trimethylhexamethylenediamine, 3,9- bis- (3- aminopropyl) -2,4,8,
Tetra- oxaspiro of 10- (5,5) hendecane, Hanzhong chemical industry aliphatic polyamine H220B, rise waffle work water-soluble aliphatic cyclic amine EA50B,
The mixture of one of aromatic amine BH560 of unexpected rival's chemical industry or in which several compositions.
A kind of preparation method of aqueous fluorubber lotion adhesive of the present invention, includes the following steps:
Step 1, aqueous fluorubber lotion, the water-base epoxy tree for weighing certain mass respectively according to non-volatile part parts by weight
Rouge, amine hardener, acid absorbent, emulsion film forming auxiliary agent, for use；
Step 2 pours into the load weighted aqueous fluorubber lotion of step 1, aqueous epoxy resins in reaction vessel, in room temperature
After lower mechanical stirring is uniform, for use；
Step 3, the reaction vessel that the load weighted amine hardener of step 1, acid absorbent, emulsion film forming auxiliary agent are added to step 2
In, after mechanical stirring is uniform, a kind of aqueous fluorubber lotion adhesive is made.
A kind of preparation method of aqueous fluorubber lotion adhesive of the present invention, mechanical agitator revolving speed in step 2
Being set as 200~500rpm mechanical stirring time is 10~30min.
A kind of preparation method of aqueous fluorubber lotion adhesive of the present invention, mechanical agitator revolving speed in step 3
Being set as 200~10000rpm mechanical stirring time is 10~30min.
A kind of aqueous fluorubber lotion adhesive of the present invention, aqueous epoxy resins include water-soluble epoxy resin,
Nonionic external emulsion epoxy resin emulsion, one of epoxy resin latex of modified nonionic emulsifier preparation or in which several
The mixture of composition, such as H220A of commercially available Hanzhong chemical industry, the Shanghai love MU601 of Expo, Guangzhou unexpected rival's chemical industry BH651,
MHR-36, MHR-70, the epoxy resin E-20 product emulsion of the magnificent chemical industry of BH652, U.S..
A kind of aqueous fluorubber lotion adhesive of the present invention, aqueous amine curing agent include commercially available Hanzhong chemical industry
Aliphatic polyamine H220B, the water-soluble aliphatic cyclic amine EA50B for rising waffle work, unexpected rival's chemical industry one of aromatic amine BH560 etc. or
The wherein mixture of several compositions.
A kind of aqueous fluorubber lotion adhesive of the present invention is bonded between B501 fluorine adhesive plaster, contacts pressure chamber Wen Gu
Change 7d, room temperature T-type peel strength is up to 1.29KN/m, and room temperature T-type peel strength is up to 1.63KN/ after 200 DEG C of agings for 24 hours
m。
A kind of aqueous fluorubber lotion adhesive of the present invention is bonded B501 fluorine adhesive plaster and anodized aluminum, contact pressure
After room temperature curing for 24 hours, then 60 DEG C of solidification 3h, 180 ° of peel strengths of room temperature are up to 1.07KN/m, and fluorine adhesive plaster destroys, and 200
180 ° of peel strengths of room temperature are up to 0.97KN/m after DEG C aging for 24 hours, and fluorine adhesive plaster destroys.
A kind of aqueous fluorubber lotion adhesive of the present invention, VOC suitable with solvent type fluorubber adhesive strength
Content 1%~4%, the VOC content 70%~78% of common solvent type fluorubber adhesive.
A kind of aqueous fluorubber lotion adhesive of the present invention, compared with solvent type fluorubber adhesive, the present invention
The aqueous fluorubber adhesive of preparation not only has lower VOC content, reduces asking for solvent type adhesive environmental pollution
Topic, at the same have with the comparable adhesive strength of solvent type fluorubber adhesive, have a good application prospect.
A kind of aqueous fluorubber lotion adhesive of the present invention, is not limited to adhesive area, in water paint, aqueous
The fields such as resin also have wide application prospects.
A kind of preparation method of aqueous fluorubber lotion adhesive of the present invention, first by aqueous fluorubber lotion and
Aqueous epoxy resins are blended uniformly according to a certain ratio；Again according to a certain ratio by amine hardener, acid absorbent, emulsion film forming auxiliary agent
It is added in above-mentioned mixed emulsion, according to aqueous epoxy resins and the discrete form of amine hardener in water, selects mechanical blending
Method prepare uniform aqueous fluorubber lotion adhesive.Modified water-soluble fluorubber lotion adhesive is in amine curing agent condition
Under, hybridization network is blended with crosslinked fluororubber formation in aqueous epoxy resins, significantly improves viscous after aqueous fluorubber lotion solidifies
Connect performance；Amine curing agent is both the curing agent of epoxy resin, at the same also can vulcanised fluororubbers, promotion is played to cross-linking system
Effect.This adhesive have with the comparable adhesive strength of solvent type fluorubber adhesive, while greatly reducing organic solvent
Usage amount.
Specific embodiment
Specific embodiment 1:
A kind of aqueous fluorubber lotion adhesive, the aqueous fluorubber lotion adhesive is mainly by aqueous fluorubber
Lotion, aqueous epoxy resins, amine hardener, acid absorbent, emulsion film forming auxiliary agent are made, and non-volatile part parts by weight are respectively water
100 parts of fluorubber of property, 20 parts of aqueous epoxy resins E-20 lotion, aqueous 8 parts of alicyclic ring amine hardener EA50B, acid absorbent magnesia
1.5 parts of aqueous dispersions, 4 parts of emulsion film forming auxiliary agent n,N-dimethylacetamide.
A kind of preparation method of aqueous fluorubber lotion adhesive, includes the following steps: described in present embodiment
Step 1, aqueous fluorubber lotion, the water-base epoxy tree for weighing certain mass respectively according to non-volatile part parts by weight
Rouge, amine hardener, acid absorbent, emulsion film forming auxiliary agent, for use；
Step 2 pours into the load weighted aqueous fluorubber lotion of step 1, aqueous epoxy resins in reaction vessel, in room temperature
After lower mechanical stirring is uniform, for use；
Step 3, the reaction vessel that the load weighted amine hardener of step 1, acid absorbent, emulsion film forming auxiliary agent are added to step 2
In, after mechanical stirring is uniform, a kind of aqueous fluorubber lotion adhesive is made.
A kind of preparation method of aqueous fluorubber lotion adhesive described in present embodiment, mechanical agitator in step 2
Revolving speed is set as the 300rpm mechanical stirring time for 20min.
A kind of preparation method of aqueous fluorubber lotion adhesive described in present embodiment, mechanical agitator in step 3
Revolving speed is set as the 1000rpm mechanical stirring time for 20min.
A kind of aqueous fluorubber lotion adhesive described in present embodiment, T-type peel strength are marked by GB/T2791-1995
Standard is tested, as follows by viscous material T-type peel test method: B501 fluorine adhesive plaster sample dimensions are long * wide=200*25mm, In
Material surface to be glued applies 3 times glue, every to hang 10~15min all over room temperature, then closes up, contact pressure room temperature curing 5-7d, Huo Zhejie
After pressing room temperature curing for 24 hours, then 60 DEG C of solidification 3h.
A kind of aqueous fluorubber lotion adhesive described in present embodiment is bonded between B501 fluorine adhesive plaster, contacts pressure chamber
Temperature solidification 7d, room temperature T-type peel strength are 1.29KN/m, and room temperature T-type peel strength is 1.01KN/m after 200 DEG C of agings for 24 hours.
A kind of aqueous fluorubber lotion adhesive described in present embodiment, 180 ° of peel strengths press GB/T2790-1995
Standard is tested, as follows by 180 ° of peel test methods of viscous material: B501 fluorine adhesive plaster sample dimensions are long * wide=400*
25mm；Aluminium alloy sample dimensions are long * wide * thickness=200*25*3mm, and according to HB/Z197-91 standard to aluminium alloy batten
Carry out phosphoric acid anodised surfaces processing.3 times glue are applied in material surface to be glued, it is every to hang 10~15min all over room temperature, then close up,
After contact pressure room temperature curing 7d, or contact pressure room temperature curing for 24 hours, then 60 DEG C of solidification 3h.
A kind of aqueous fluorubber lotion adhesive described in present embodiment is bonded B501 fluorine adhesive plaster and anodized aluminum, connects
After pressing room temperature curing for 24 hours, then 60 DEG C of solidification 3h, 180 ° of peel strengths of room temperature are 1.07KN/m, and fluorine adhesive plaster destroys, 200
180 ° of peel strengths of room temperature are 0.86KN/m after DEG C aging for 24 hours, and fluorine adhesive plaster destroys.
A kind of aqueous fluorubber lotion adhesive and solvent type fluorubber adhesive, unmodified water described in present embodiment
Property the comparison of fluorubber lotion test result it is as shown in table 1:
1 peel strength test contrast table (KN/m) of table
From table 1, it can be seen that a kind of peel strength of aqueous fluorubber lotion adhesive described in present embodiment >=
0.7KN/m meets application.
A kind of aqueous fluorubber lotion adhesive, VOC content 3% described in present embodiment.
Specific embodiment 2:
A kind of aqueous fluorubber lotion adhesive, the aqueous fluorubber lotion adhesive is mainly by aqueous fluorubber
Lotion, aqueous epoxy resins, amine hardener, acid absorbent, emulsion film forming auxiliary agent are made, and non-volatile part parts by weight are respectively water
Property 100 parts of fluorubber, 15 parts of aqueous epoxy resins H220A, 8 parts of aliphatic polyamine H220B, acid absorbent Zinc oxide water dispersion
1 part of liquid, 2 parts of emulsion film forming auxiliary agent butyl glycol ether.
A kind of preparation method of aqueous fluorubber lotion adhesive, includes the following steps: described in present embodiment
Step 1, aqueous fluorubber lotion, the water-base epoxy tree for weighing certain mass respectively according to non-volatile part parts by weight
Rouge, amine hardener, acid absorbent, emulsion film forming auxiliary agent, for use；
Step 2 pours into the load weighted aqueous fluorubber lotion of step 1, aqueous epoxy resins in reaction vessel, in room temperature
After lower mechanical stirring is uniform, for use；
Step 3, the reaction vessel that the load weighted amine hardener of step 1, acid absorbent, emulsion film forming auxiliary agent are added to step 2
In, after mechanical stirring is uniform, a kind of aqueous fluorubber lotion adhesive is made.
A kind of preparation method of aqueous fluorubber lotion adhesive described in present embodiment, mechanical agitator in step 2
Revolving speed is set as the 300rpm mechanical stirring time for 20min.
A kind of preparation method of aqueous fluorubber lotion adhesive described in present embodiment, mechanical agitator in step 3
Revolving speed is set as the 9000rpm mechanical stirring time for 10min.
A kind of aqueous fluorubber lotion adhesive described in present embodiment, T-type peel strength are marked by GB/T2791-1995
Standard is tested, as follows by viscous material T-type peel test method: B501 fluorine adhesive plaster sample dimensions are long * wide=200*25mm, In
Material surface to be glued applies 3 times glue, every to hang 10~15min all over room temperature, then closes up, contact pressure room temperature curing 5-7d, Huo Zhejie
After pressing room temperature curing for 24 hours, then 60 DEG C of solidification 3h.
A kind of aqueous fluorubber lotion adhesive described in present embodiment is bonded between B501 fluorine adhesive plaster, contacts pressure chamber
Temperature solidification 7d, room temperature T-type peel strength are 1.22KN/m, and room temperature T-type peel strength is 0.98KN/m after 200 DEG C of agings for 24 hours.
A kind of aqueous fluorubber lotion adhesive described in present embodiment, 180 ° of peel strengths press GB/T2790-1995
Standard is tested, as follows by 180 ° of peel test methods of viscous material: B501 fluorine adhesive plaster sample dimensions are long * wide=400*
25mm；Aluminium alloy sample dimensions are long * wide * thickness=200*25*3mm, and according to HB/Z197-91 standard to aluminium alloy batten
Carry out phosphoric acid anodised surfaces processing.3 times glue are applied in material surface to be glued, it is every to hang 10~15min all over room temperature, then close up,
After contact pressure room temperature curing 7d, or contact pressure room temperature curing for 24 hours, then 60 DEG C of solidification 3h.
A kind of aqueous fluorubber lotion adhesive described in present embodiment is bonded B501 fluorine adhesive plaster and anodized aluminum, connects
After pressing room temperature curing for 24 hours, then 60 DEG C of solidification 3h, 180 ° of peel strengths of room temperature are 0.63KN/m, and fluorine adhesive plaster destroys, 200
180 ° of peel strengths of room temperature are 0.83KN/m after DEG C aging for 24 hours, and fluorine adhesive plaster destroys.
A kind of aqueous fluorubber lotion adhesive and solvent type fluorubber adhesive, unmodified water described in present embodiment
Property the comparison of fluorubber lotion test result it is as shown in table 2:
2 peel strength test contrast table (KN/m) of table
, it can be seen that a kind of T-type peel strength of aqueous fluorubber lotion adhesive described in present embodiment from table 2
>=0.7KN/m meets application.
A kind of aqueous fluorubber lotion adhesive, VOC content 1.6% described in present embodiment.
Specific embodiment 3:
A kind of aqueous fluorubber lotion adhesive, the aqueous fluorubber lotion adhesive is mainly by aqueous fluorubber
Lotion, aqueous epoxy resins, amine hardener, acid absorbent are made, and non-volatile part parts by weight are respectively aqueous fluorubber 100
Part, 18 parts of epoxy resin of aqueous phenolic aldehyde BH652 lotion, 9 parts of aqueous epoxy curing agent BH560, acid absorbent magnesia aqueous dispersions
1.5 part.
A kind of preparation method of aqueous fluorubber lotion adhesive, includes the following steps: described in present embodiment
Step 1, aqueous fluorubber lotion, the water-base epoxy tree for weighing certain mass respectively according to non-volatile part parts by weight
Rouge, amine hardener, acid absorbent, for use；
Step 2 pours into the load weighted aqueous fluorubber lotion of step 1, aqueous epoxy resins in reaction vessel, in room temperature
After lower mechanical stirring is uniform, for use；
The load weighted amine hardener of step 1, acid absorbent are added in the reaction vessel of step 2 step 3, and mechanical stirring is equal
After even, a kind of aqueous fluorubber lotion adhesive is made.
A kind of preparation method of aqueous fluorubber lotion adhesive described in present embodiment, mechanical agitator in step 2
Revolving speed is set as the 300rpm mechanical stirring time for 20min.
A kind of preparation method of aqueous fluorubber lotion adhesive described in present embodiment, mechanical agitator in step 3
Revolving speed is set as the 1000rpm mechanical stirring time for 10min.
A kind of aqueous fluorubber lotion adhesive described in present embodiment, T-type peel strength are marked by GB/T2791-1995
Standard is tested, as follows by viscous material T-type peel test method: B501 fluorine adhesive plaster sample dimensions are long * wide=200*25mm, In
Material surface to be glued applies 3 times glue, every to hang 10~15min all over room temperature, then closes up, contact pressure room temperature curing 5-7d, Huo Zhejie
After pressing room temperature curing for 24 hours, then 60 DEG C of solidification 3h.
A kind of aqueous fluorubber lotion adhesive described in present embodiment is bonded between B501 fluorine adhesive plaster, contacts pressure chamber
Temperature solidification 7d, room temperature T-type peel strength are 1.15KN/m, and room temperature T-type peel strength is 1.26KN/m after 200 DEG C of agings for 24 hours.
A kind of aqueous fluorubber lotion adhesive described in present embodiment, 180 ° of peel strengths press GB/T2790-1995
Standard is tested, as follows by 180 ° of peel test methods of viscous material: B501 fluorine adhesive plaster sample dimensions are long * wide=400*
25mm；Aluminium alloy sample dimensions are long * wide * thickness=200*25*3mm, and according to HB/Z197-91 standard to aluminium alloy batten
Carry out phosphoric acid anodised surfaces processing.3 times glue are applied in material surface to be glued, it is every to hang 10~15min all over room temperature, then close up,
After contact pressure room temperature curing 7d, or contact pressure room temperature curing for 24 hours, then 60 DEG C of solidification 3h.
A kind of aqueous fluorubber lotion adhesive described in present embodiment is bonded B501 fluorine adhesive plaster and anodized aluminum, connects
After pressing room temperature curing for 24 hours, then 60 DEG C of solidification 3h, 180 ° of peel strengths of room temperature are 0.55KN/m, and fluorine adhesive plaster destroys, 200
180 ° of peel strengths of room temperature are 0.97KN/m after DEG C aging for 24 hours, and fluorine adhesive plaster destroys.
A kind of aqueous fluorubber lotion adhesive and solvent type fluorubber adhesive, unmodified water described in present embodiment
Property the comparison of fluorubber lotion test result it is as shown in table 3:
3 peel strength test contrast table (KN/m) of table
, it can be seen that a kind of T-type peel strength of aqueous fluorubber lotion adhesive described in present embodiment from table 3
>=0.7KN/m meets application.
A kind of aqueous fluorubber lotion adhesive, VOC content 1.0% described in present embodiment.
Specific embodiment 4:
A kind of aqueous fluorubber lotion adhesive, the aqueous fluorubber lotion adhesive is mainly by aqueous fluorubber
Lotion, aqueous epoxy resins, amine hardener, acid absorbent, emulsion film forming auxiliary agent are made, and non-volatile part parts by weight are respectively water
100 parts of fluorubber of property, 16 parts of aqueous epoxy resins MHR-36, water-soluble 7 parts of alicyclic ring amine hardener EA50B, acid absorbent hydrogen-oxygen
Change 1 part of calcium aqueous dispersions, 3 parts of emulsion film forming auxiliary agent n,N-dimethylacetamide.
A kind of preparation method of aqueous fluorubber lotion adhesive, includes the following steps: described in present embodiment
Step 1, aqueous fluorubber lotion, the water-base epoxy tree for weighing certain mass respectively according to non-volatile part parts by weight
Rouge, amine hardener, acid absorbent, emulsion film forming auxiliary agent, for use；
Step 2 pours into the load weighted aqueous fluorubber lotion of step 1, aqueous epoxy resins in reaction vessel, in room temperature
After lower mechanical stirring is uniform, for use；
Step 3, the reaction vessel that the load weighted amine hardener of step 1, acid absorbent, emulsion film forming auxiliary agent are added to step 2
In, after mechanical stirring is uniform, a kind of aqueous fluorubber lotion adhesive is made.
A kind of preparation method of aqueous fluorubber lotion adhesive described in present embodiment, mechanical agitator in step 2
Revolving speed is set as the 400rpm mechanical stirring time for 20min.
A kind of preparation method of aqueous fluorubber lotion adhesive described in present embodiment, mechanical agitator in step 3
Revolving speed is set as the 1000rpm mechanical stirring time for 20min.
A kind of aqueous fluorubber lotion adhesive described in present embodiment, T-type peel strength are marked by GB/T2791-1995
Standard is tested, as follows by viscous material T-type peel test method: B501 fluorine adhesive plaster sample dimensions are long * wide=200*25mm, In
Material surface to be glued applies 3 times glue, every to hang 10~15min all over room temperature, then closes up, contact pressure room temperature curing 5-7d, Huo Zhejie
After pressing room temperature curing for 24 hours, then 60 DEG C of solidification 3h.
A kind of aqueous fluorubber lotion adhesive described in present embodiment is bonded between B501 fluorine adhesive plaster, contacts pressure chamber
Temperature solidification 7d, room temperature T-type peel strength are 1.21KN/m, and room temperature T-type peel strength is 1.63KN/m after 200 DEG C of agings for 24 hours.
A kind of aqueous fluorubber lotion adhesive described in present embodiment, 180 ° of peel strengths press GB/T2790-1995
Standard is tested, as follows by 180 ° of peel test methods of viscous material: B501 fluorine adhesive plaster sample dimensions are long * wide=400*
25mm；Aluminium alloy sample dimensions are long * wide * thickness=200*25*3mm, and according to HB/Z197-91 standard to aluminium alloy batten
Carry out phosphoric acid anodised surfaces processing.3 times glue are applied in material surface to be glued, it is every to hang 10~15min all over room temperature, then close up,
After contact pressure room temperature curing 7d, or contact pressure room temperature curing for 24 hours, then 60 DEG C of solidification 3h.
A kind of aqueous fluorubber lotion adhesive described in present embodiment is bonded B501 fluorine adhesive plaster and anodized aluminum, connects
After pressing room temperature curing for 24 hours, then 60 DEG C of solidification 3h, 180 ° of peel strengths of room temperature are 1.02KN/m, and fluorine adhesive plaster destroys, 200
180 ° of peel strengths of room temperature are 0.81KN/m after DEG C aging for 24 hours, and fluorine adhesive plaster destroys.
A kind of aqueous fluorubber lotion adhesive and solvent type fluorubber adhesive, unmodified water described in present embodiment
Property the comparison of fluorubber lotion test result it is as shown in table 4:
4 peel strength test contrast table (KN/m) of table
From table 4, it can be seen that a kind of peel strength of aqueous fluorubber lotion adhesive described in present embodiment >=
0.7KN/m meets application.
A kind of aqueous fluorubber lotion adhesive, VOC content 2.9% described in present embodiment.
Specific embodiment 5:
A kind of aqueous fluorubber lotion adhesive, the aqueous fluorubber lotion adhesive is mainly by aqueous fluorubber
Lotion, aqueous epoxy resins, amine hardener, acid absorbent, emulsion film forming auxiliary agent are made, and non-volatile part parts by weight are respectively 95
~105 parts of aqueous fluorubber lotion, 10~30 parts of aqueous epoxy resins, 3~9 parts of amine hardener, 1~3 part of suction acid
Agent, 0~5 part of emulsion film forming auxiliary agent, the amine hardener are water-soluble or water-dispersible amine hardener, the suction acid
Agent is one of light magnesium oxide, zinc oxide, calcium oxide, calcium hydroxide or its corresponding aqueous dispersions or in which several compositions
Mixture, the emulsion film forming auxiliary agent be ethylene glycol, butyl glycol ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, propylene glycol fourth
One of ether, dipropylene glycol monopropyl ether, Dipropylene glycol mono-n-butyl Ether, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone or its
In several compositions mixture.
A kind of aqueous fluorubber lotion adhesive described in present embodiment is bonded between B501 fluorine adhesive plaster, contacts pressure chamber
Temperature solidification 7d, room temperature T-type peel strength are up to 1.29KN/m, and room temperature T-type peel strength is up to after 200 DEG C of agings for 24 hours
1.63KN/m。
A kind of aqueous fluorubber lotion adhesive described in present embodiment is bonded B501 fluorine adhesive plaster and anodized aluminum, connects
After pressing room temperature curing for 24 hours, then 60 DEG C of solidification 3h, 180 ° of peel strengths of room temperature are up to 1.07KN/m, and fluorine adhesive plaster destroys,
180 ° of peel strengths of room temperature are up to 0.97KN/m after 200 DEG C of agings for 24 hours, and fluorine adhesive plaster destroys.
A kind of aqueous fluorubber lotion adhesive of the present invention, VOC suitable with solvent type fluorubber adhesive strength
Content 1%~4%, the VOC content 70%~78% of common solvent type fluorubber adhesive.
A kind of aqueous fluorubber lotion adhesive described in present embodiment, compared with solvent type fluorubber adhesive, this
The aqueous fluorubber adhesive of invention preparation not only has lower VOC content, reduces solvent type adhesive environmental pollution
The problem of, at the same have with the comparable adhesive strength of solvent type fluorubber adhesive, have a good application prospect.
Specific embodiment 6:
A kind of aqueous fluorubber lotion adhesive according to specific embodiment five, the aqueous fluorubber lotion
Non-volatile part parts by weight of aqueous fluorubber lotion are 95 parts in adhesive, non-volatile part parts by weight of aqueous epoxy resins
It is 10 parts, non-volatile part parts by weight of amine hardener are 3 parts, and non-volatile part parts by weight of acid absorbent are 1 part, emulsion film forming
The parts by weight of auxiliary agent are 1 part.
Specific embodiment 7:
A kind of aqueous fluorubber lotion adhesive according to specific embodiment five, the aqueous fluorubber lotion
Non-volatile part parts by weight of aqueous fluorubber lotion are 105 parts in adhesive, non-volatile part parts by weight of aqueous epoxy resins
Number is 30 parts, and non-volatile part parts by weight of amine hardener are 9 parts, and non-volatile part parts by weight of acid absorbent are 3 parts, lotion at
The parts by weight of film auxiliary agent are 5 parts.
Specific embodiment 8:
A kind of aqueous fluorubber lotion adhesive according to specific embodiment five, the aqueous fluorubber lotion
Non-volatile part parts by weight of aqueous fluorubber lotion are 100 parts in adhesive, non-volatile part parts by weight of aqueous epoxy resins
Number is 20 parts, and non-volatile part parts by weight of amine hardener are 5 parts, and non-volatile part parts by weight of acid absorbent are 2 parts, lotion at
The parts by weight of film auxiliary agent are 3 parts.
Specific embodiment 9:
A kind of aqueous fluorubber lotion adhesive, the group of the fluorubber lotion according to specific embodiment five
It is distilled water as the fluorubber of mass fraction 15~30%, 0.5~2.0% emulsifier, surplus, the fluorubber is inclined
Fluorubber made from vinyl fluoride and hexafluoropropene combined polymerization, the emulsifier are condensation compound of alkyl phenol and epoxy ethane OP-10
Emulsifier.
Specific embodiment 10:
A kind of aqueous fluorubber lotion adhesive, the aqueous epoxy resins packet according to specific embodiment five
Include epoxy resin latex prepared by water-soluble epoxy resin, nonionic external emulsion epoxy resin emulsion, modified nonionic emulsifier
One of or in which several compositions mixture, including aqueous epoxy resins MHR-36, epoxy resin of aqueous phenolic aldehyde BH652 cream
Liquid, aqueous epoxy resins H220A, aqueous epoxy resins E-20 lotion.
Specific embodiment 11:
A kind of aqueous fluorubber lotion adhesive according to specific embodiment five, the amine hardener are isophthalic
Diamines, diaminodiphenylmethane, N, the bis- cortex cinnamomi fork -1,6- hexamethylene diamines of N-, trimethylhexamethylenediamine, (the 3- amino of 3,9- bis-
Propyl) -2,4,8,10- four oxaspiro (5,5) hendecane, aliphatic polyamine H220B, water-soluble aliphatic cyclic amine EA50B, aromatic amine
The mixture of one of BH560 or in which several compositions.
Specific embodiment 12:
A kind of preparation method of aqueous fluorubber lotion adhesive according to specific embodiment five, including walk as follows
It is rapid:
Step 1, aqueous fluorubber lotion, the water-base epoxy tree for weighing certain mass respectively according to non-volatile part parts by weight
Rouge, amine hardener, acid absorbent, emulsion film forming auxiliary agent, for use；
Step 2 pours into the load weighted aqueous fluorubber lotion of step 1, aqueous epoxy resins in reaction vessel, in room temperature
After lower mechanical stirring is uniform, for use；
Step 3, the reaction vessel that the load weighted amine hardener of step 1, acid absorbent, emulsion film forming auxiliary agent are added to step 2
In, after mechanical stirring is uniform, a kind of aqueous fluorubber lotion adhesive is made.
A kind of preparation method of aqueous fluorubber lotion adhesive described in present embodiment, mechanical agitator in step 2
Revolving speed is set as 200~500rpm mechanical stirring time for 10~30min.
A kind of preparation method of aqueous fluorubber lotion adhesive described in present embodiment, mechanical agitator in step 3
Revolving speed is set as 200~10000rpm mechanical stirring time for 10~30min.
Claims (9)
1. a kind of aqueous fluorubber lotion adhesive, it is characterised in that: the aqueous fluorubber lotion adhesive mainly by
Aqueous fluorubber lotion, aqueous epoxy resins, amine hardener, acid absorbent, emulsion film forming auxiliary agent are made, non-volatile part parts by weight
Number be respectively 95~105 parts aqueous fluorubber lotions, 10~30 parts of aqueous epoxy resins, 3~9 parts of amine hardener, 1~
3 parts of acid absorbent, 0~5 part of emulsion film forming auxiliary agent, the amine hardener are water-soluble or water-dispersible amine hardener,
The acid absorbent be one of light magnesium oxide, zinc oxide, calcium oxide, calcium hydroxide or its corresponding aqueous dispersions or its
In several compositions mixture, the emulsion film forming auxiliary agent be ethylene glycol, butyl glycol ether, propylene glycol monomethyl ether, propylene glycol second
Ether, propandiol butyl ether, dipropylene glycol monopropyl ether, Dipropylene glycol mono-n-butyl Ether, DMAC N,N' dimethyl acetamide, in N-Methyl pyrrolidone
One kind or in which several compositions mixture；The group of the fluorubber lotion becomes the fluorine rubber of mass fraction 15~30%
Glue, 0.5~2.0% emulsifier, surplus are distilled water, and the fluorubber is that vinylidene and hexafluoropropene combined polymerization are made
Fluorubber, the emulsifier be condensation compound of alkyl phenol and epoxy ethane OP-10 emulsifier.
2. a kind of aqueous fluorubber lotion adhesive according to claim 1, it is characterised in that: the aqueous fluorubber
Non-volatile part parts by weight of aqueous fluorubber lotion are 95 parts in lotion adhesive, non-volatile part weight of aqueous epoxy resins
Number is 10 parts, and non-volatile part parts by weight of amine hardener are 3 parts, and non-volatile part parts by weight of acid absorbent are 1 part, lotion
The parts by weight of coalescing agent are 1 part.
3. a kind of aqueous fluorubber lotion adhesive according to claim 1, it is characterised in that: the aqueous fluorubber
Non-volatile part parts by weight of aqueous fluorubber lotion are 105 parts in lotion adhesive, non-volatile part weight of aqueous epoxy resins
Measuring number is 30 parts, and non-volatile part parts by weight of amine hardener are 9 parts, and non-volatile part parts by weight of acid absorbent are 3 parts, cream
The parts by weight of liquid coalescing agent are 5 parts.
4. a kind of aqueous fluorubber lotion adhesive according to claim 1, it is characterised in that: the aqueous fluorubber
Non-volatile part parts by weight of aqueous fluorubber lotion are 100 parts in lotion adhesive, non-volatile part weight of aqueous epoxy resins
Measuring number is 20 parts, and non-volatile part parts by weight of amine hardener are 5 parts, and non-volatile part parts by weight of acid absorbent are 2 parts, cream
The parts by weight of liquid coalescing agent are 3 parts.
5. a kind of aqueous fluorubber lotion adhesive according to claim 1 or 4, it is characterised in that: the aqueous ring
Oxygen resin includes water-soluble epoxy resin, nonionic external emulsion epoxy resin emulsion, the epoxy for being modified nonionic emulsifier preparation
The mixture of one of resin emulsion or in which several compositions, including aqueous epoxy resins MHR-36, aqueous phenolic aldehyde asphalt mixtures modified by epoxy resin
Rouge BH652 lotion, aqueous epoxy resins H220A, aqueous epoxy resins E-20 lotion.
6. a kind of aqueous fluorubber lotion adhesive according to claim 1 or 4, it is characterised in that: the amine curing
Agent is m-phenylene diamine (MPD), diaminodiphenylmethane, N, the bis- cortex cinnamomi fork -1,6- hexamethylene diamines of N-, trimethylhexamethylenediamine, 3,9- bis-
(3- aminopropyl) -2,4,8,10- four oxaspiro (5,5) hendecane, aliphatic polyamine H220B, water-soluble aliphatic cyclic amine EA50B,
The mixture of one of aromatic amine BH560 or in which several compositions.
7. a kind of preparation method of aqueous fluorubber lotion adhesive described in a kind of one of claim 1-6, it is characterised in that:
Include the following steps:
Step 1, the aqueous fluorubber lotion for weighing certain mass respectively according to non-volatile part parts by weight, aqueous epoxy resins,
Amine hardener, acid absorbent, emulsion film forming auxiliary agent, for use；
Step 2 pours into the load weighted aqueous fluorubber lotion of step 1, aqueous epoxy resins in reaction vessel, at room temperature machine
Tool after mixing evenly, for use；
Step 3 the load weighted amine hardener of step 1, acid absorbent, emulsion film forming auxiliary agent is added in the reaction vessel of step 2, machine
After mixing evenly, a kind of aqueous fluorubber lotion adhesive is made in tool.
8. a kind of preparation method of aqueous fluorubber lotion adhesive according to claim 7, it is characterised in that: step 2
Middle mechanical agitator revolving speed is set as 200~500rpm mechanical stirring time for 10~30min.
9. a kind of preparation method of aqueous fluorubber lotion adhesive according to claim 7, it is characterised in that: step 3
Middle mechanical agitator revolving speed is set as 200~10000rpm mechanical stirring time for 10~30min.
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Effective date of registration: 20191212 Address after: 150066 Xinhua Industrial community, Pingfang District, Harbin City, Heilongjiang Province Patentee after: Harbin Jingxin Technology Co., Ltd Address before: 150040 No. 164, Zhongshan Road, Heilongjiang, Harbin Patentee before: Institute of Petrochemistry, HLJ Academy of Science |