CN106085302A - A kind of mill base adhesive utilizing acrylic resin to prepare - Google Patents
A kind of mill base adhesive utilizing acrylic resin to prepare Download PDFInfo
- Publication number
- CN106085302A CN106085302A CN201610411317.3A CN201610411317A CN106085302A CN 106085302 A CN106085302 A CN 106085302A CN 201610411317 A CN201610411317 A CN 201610411317A CN 106085302 A CN106085302 A CN 106085302A
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- China
- Prior art keywords
- polymer
- acrylic resin
- mixed liquor
- adhesive
- mill base
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- 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
- C09J133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/10—Homopolymers or copolymers of methacrylic acid esters
- C09J133/12—Homopolymers or copolymers of methyl methacrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of mill base adhesive utilizing acrylic resin to prepare, relate to technical field of adhesive preparation, its preparation method comprises the steps: that (1) acrylic resin is polymerized, (2) polymer latting drown, (3) polymer inspection, (4) polymer filtration, prepared by (5) adhesive.The present invention at acrylic resin polymerization stage by the way of batch charging, improve polyreaction degree and raw material availability, polymer is again under the synergism of auxiliary agent, make the adhesive prepared have viscosity is suitable, glueability is excellent feature, and the uniform coloring of pigment can be improved, the weatherability after mill base film forming is made to strengthen, it is not easy to fade and efflorescence, thus extend the service life of paint film.
Description
Technical field:
The present invention relates to technical field of adhesive preparation, be specifically related to a kind of mill base utilizing acrylic resin to prepare gluing
Agent.
Background technology:
Mill base is the semi-products being dispersed in paint vehicle by pigment or pigment and inserts.Title with pure oil as adhesive
Oil pastes, the title resin mill base with resin paint vehicle as adhesive, adds the face of surfactant-dispersed with water for medium
Extender paste is referred to as aqueous color paste.Owing to paint vehicle kind is a lot, mill base kind is the most a lot.
The resin that acrylic resin is made up of esters of acrylic acid and methyl acrylic ester and other olefinic type monomers copolymerization,
By selecting different resin structures, different formula, production technology and solvent to form, dissimilar, different performance can be synthesized
Acrylic resin with different application occasion.The mill base adhesive utilizing olefin(e) acid resin-made standby can improve the uniform coloring of pigment
Property, the weatherability after mill base film forming is stronger, it is not easy to fade and efflorescence.
Summary of the invention:
The technical problem to be solved is to provide one, and preparation cost is low, raw material availability is high and properties of product
The excellent mill base adhesive utilizing acrylic resin to prepare.
The technical problem to be solved uses following technical scheme to realize:
A kind of mill base adhesive utilizing acrylic resin to prepare, its preparation method comprises the steps:
(1) acrylic resin polymerization: monomer, solvent and initiator are mixed to form mixed liquor, mixed liquor by processing compound
It is dividedly in some parts, first first mixed liquor is squeezed in reactor, be warming up to 80-150 DEG C, in 2-5h, then drip second batch mix
Close liquid and carry out polyreaction, insulation reaction 1-2h, then carry out the 3rd batch of mixed liquor dropping, after 1-2h, carry out the 4th batch of mixing drop
Add, insulation reaction 1-2h, finally residual mixed liquor is all dripped, stopped reaction after insulation 3h, obtain polymer, reacted
The waste gas produced in journey enters tail-gas combustion stove burning after collecting;
(2) polymer latting drown: upwards add butyl acetate in step resulting polymers, carry out viscosity adjustment;
(3) polymer inspection: by the polymer after latting drown is tested, as viscosity is qualified, be then directly entered lower step
Filtration stage;As viscosity is defective, by using butyl acetate, carry out viscosity adjustment, after the assay was approved, enter back into filtration rank
Section;
(4) polymer filtration: by filter, polymer bigger to material unreacted in resin and granule etc. is miscellaneous
Matter filters, and filtering residue has transferred to danger useless process qualification processed in units, and filtrate enters warehouse for finished product after packaging, obtains acrylic resin molten
Liquid;
(5) prepared by adhesive: mixed according to weight ratio 1:0.05 with auxiliary agent by above-mentioned gained acrylic resin soln, mixing
Thing is prior to supersound process 30min under supersonic frequency 40kHz, power 100W, micro-under microwave frequency 2450MHz, power 700W
Ripple processes 10min, and pending thing naturally cools to room temperature, then stands overnight at 0-5 DEG C, finally utilizes ball mill to be milled to
Fineness is less than 10 μm;
Described auxiliary agent is made up of the raw material of following parts by weight: chlorosulfonated polyethylene 10-15 part, rubber powder 7-10 part, work
Property hargil 5-8 part, hydrogenated rosin 5-8 part, petroleum coke 4-6 part, rice bran wax 4-6 part, nanometer rubber powder 3-5 part, chlorobutanol 2-3
Part, thiourea 2-3 part, bone black powder 1-2 part, nanometer aluminium powder 1-2 part, Matrii Sulfas Exsiccatus 1-2 part, sodium selenite 0.5-1 part, ethylenediamine two amber
Amber acid trisodium 0.5-1 part, its preparation method is: first chlorosulfonated polyethylene, hydrogenated rosin and petroleum coke are sufficiently mixed, in microwave
Microwave treatment 5min under frequency 2450MHz, power 700W, adds rubber powder, rice bran wax and nanometer rubber powder, continues microwave treatment
10min, pending thing adds active hargil, chlorobutanol, bone black powder and nanometer aluminium powder after naturally cooling to 80-90 DEG C, fills
Divide sealing and standing 3h after mixing, be eventually adding thiourea, Matrii Sulfas Exsiccatus, sodium selenite and EDDS trisodium, be fully ground
Make its mix homogeneously.
Described monomer is pressed certain by methyl methacrylate, butyl acrylate, 2-(Acryloyloxy)ethanol, styrene and acrylic acid
Ratio forms, and solvent is dimethylbenzene, and initiator is dibenzoyl peroxide.
The waste gas produced in polymerization process is mainly acrylic acid, butyl acrylate, styrene, acrylic acid hydroxyl second
Ester, dimethylbenzene, methyl methacrylate, impurity, BPO, water and carbon dioxide, enter tail-gas combustion stove burning after collecting, keep away
Exempt from direct exhaust emission air.
The invention has the beneficial effects as follows: the present invention, improves at acrylic resin polymerization stage by the way of batch charging
Polyreaction degree and raw material availability, polymer, again under the synergism of auxiliary agent, makes the adhesive prepared have viscosity and fits
Preferably, the excellent feature of glueability, and the uniform coloring of pigment can be improved, make the weatherability after mill base film forming strengthen,
It is not easy to fade and efflorescence, thus extends the service life of paint film.
Detailed description of the invention:
For the technological means making the present invention realize, creation characteristic, reach purpose and be easy to understand with effect, below knot
Close specific embodiment, the present invention is expanded on further.
Embodiment 1
(1) acrylic resin polymerization: by processing compound by monomer (methyl methacrylate, butyl acrylate, acrylic acid hydroxyl
Ethyl ester, styrene and acrylic acid), dimethylbenzene and dibenzoyl peroxide be mixed to form mixed liquor, mixed liquor is dividedly in some parts, and first will
First mixed liquor is squeezed in reactor, is warming up to 80-150 DEG C, then drips second batch mixed liquor in 3h and carries out polymerization instead
Should, insulation reaction 1h, then carry out the 3rd batch of mixed liquor dropping, carry out the 4th batch of mixed liquor after 2h and drip, insulation reaction 1h, finally
Residual mixed liquor all being dripped, stopped reaction after insulation 3h, obtain polymer, the waste gas produced in course of reaction is through collecting
Rear entrance tail-gas combustion stove burns;
(2) polymer latting drown: upwards add butyl acetate in step resulting polymers, carry out viscosity adjustment;
(3) polymer inspection: by the polymer after latting drown is tested, as viscosity is qualified, be then directly entered lower step
Filtration stage;As viscosity is defective, by using butyl acetate, carry out viscosity adjustment, after the assay was approved, enter back into filtration rank
Section;
(4) polymer filtration: by filter, polymer bigger to material unreacted in resin and granule etc. is miscellaneous
Matter filters, and filtering residue has transferred to danger useless process qualification processed in units, and filtrate enters warehouse for finished product after packaging, obtains acrylic resin molten
Liquid;
(5) prepared by adhesive: mixed according to weight ratio 1:0.05 with auxiliary agent by above-mentioned gained acrylic resin soln, mixing
Thing is prior to supersound process 30min under supersonic frequency 40kHz, power 100W, micro-under microwave frequency 2450MHz, power 700W
Ripple processes 10min, and pending thing naturally cools to room temperature, then stands overnight at 0-5 DEG C, finally utilizes ball mill to be milled to
Fineness is less than 10 μm;
The preparation of auxiliary agent: first 10 parts of chlorosulfonated polyethylenes, 6 parts of hydrogenated rosins and 4 parts of petroleum cokes are sufficiently mixed, in microwave
Microwave treatment 5min under frequency 2450MHz, power 700W, adds 8 parts of rubber powders, 4 parts of rice bran waxs and 3 parts of nanometer rubber powders, continues
Continuous microwave treatment 10min, pending thing add after naturally cooling to 80-90 DEG C 5 parts of active hargil, 2 parts of chlorobutanols, 1 part
Bone black powder and 2 parts of nanometer aluminium powders, be sufficiently mixed rear sealing and standing 3h, is eventually adding 2 parts of thiourea, 1 part of Matrii Sulfas Exsiccatus, 0.5 part of sub-selenium
Acid sodium and 0.5 part of EDDS trisodium, be fully ground and make its mix homogeneously.
Embodiment 2
(1) acrylic resin polymerization: by processing compound by monomer (methyl methacrylate, butyl acrylate, acrylic acid hydroxyl
Ethyl ester, styrene and acrylic acid), dimethylbenzene and dibenzoyl peroxide be mixed to form mixed liquor, mixed liquor is dividedly in some parts, and first will
First mixed liquor is squeezed in reactor, is warming up to 80-150 DEG C, then drips second batch mixed liquor in 3h and carries out polymerization instead
Should, insulation reaction 2h, then carry out the 3rd batch of mixed liquor dropping, carry out the 4th batch of mixed liquor after 1h and drip, insulation reaction 1h, finally
Residual mixed liquor all being dripped, stopped reaction after insulation 3h, obtain polymer, the waste gas produced in course of reaction is through collecting
Rear entrance tail-gas combustion stove burns;
(2) polymer latting drown: upwards add butyl acetate in step resulting polymers, carry out viscosity adjustment;
(3) polymer inspection: by the polymer after latting drown is tested, as viscosity is qualified, be then directly entered lower step
Filtration stage;As viscosity is defective, by using butyl acetate, carry out viscosity adjustment, after the assay was approved, enter back into filtration rank
Section;
(4) polymer filtration: by filter, polymer bigger to material unreacted in resin and granule etc. is miscellaneous
Matter filters, and filtering residue has transferred to danger useless process qualification processed in units, and filtrate enters warehouse for finished product after packaging, obtains acrylic resin molten
Liquid;
(5) prepared by adhesive: mixed according to weight ratio 1:0.05 with auxiliary agent by above-mentioned gained acrylic resin soln, mixing
Thing is prior to supersound process 30min under supersonic frequency 40kHz, power 100W, micro-under microwave frequency 2450MHz, power 700W
Ripple processes 10min, and pending thing naturally cools to room temperature, then stands overnight at 0-5 DEG C, finally utilizes ball mill to be milled to
Fineness is less than 10 μm;
The preparation of auxiliary agent: first 15 parts of chlorosulfonated polyethylenes, 6 parts of hydrogenated rosins and 4 parts of petroleum cokes are sufficiently mixed, in microwave
Microwave treatment 5min under frequency 2450MHz, power 700W, adds 8 parts of rubber powders, 5 parts of rice bran waxs and 3 parts of nanometer rubber powders, continues
Continuous microwave treatment 10min, pending thing add after naturally cooling to 80-90 DEG C 8 parts of active hargil, 2 parts of chlorobutanols, 1 part
Bone black powder and 1 part of nanometer aluminium powder, be sufficiently mixed rear sealing and standing 3h, is eventually adding 2 parts of thiourea, 1 part of Matrii Sulfas Exsiccatus, 0.5 part of sub-selenium
Acid sodium and 0.5 part of EDDS trisodium, be fully ground and make its mix homogeneously.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.The technology of the industry
Personnel, it should be appreciated that the present invention is not restricted to the described embodiments, simply illustrating this described in above-described embodiment and description
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and
Equivalent defines.
Claims (2)
1. the mill base adhesive that a kind utilizes acrylic resin to prepare, it is characterised in that its preparation method comprises the steps:
(1) acrylic resin polymerization: by processing compound, monomer, solvent and initiator being mixed to form mixed liquor, mixed liquor is in batches
Add, first first mixed liquor is squeezed in reactor, be warming up to 80-150 DEG C, in 2-5h, then drip second batch mixed liquor
Carry out polyreaction, insulation reaction 1-2h, then carry out the 3rd batch of mixed liquor dropping, after 1-2h, carry out the 4th batch of mixed liquor dropping,
Insulation reaction 1-2h, finally all drips residual mixed liquor, stopped reaction after insulation 3h, obtains polymer, course of reaction
The waste gas of middle generation enters tail-gas combustion stove burning after collecting;
(2) polymer latting drown: upwards add butyl acetate in step resulting polymers, carry out viscosity adjustment;
(3) polymer inspection: by testing the polymer after latting drown, as viscosity is qualified, then be directly entered lower step and filter
Stage;As viscosity is defective, by using butyl acetate, carry out viscosity adjustment, after the assay was approved, enter back into filtration stage;
(4) polymer filtration: by filter, by impurity mistakes such as polymer bigger to material unreacted in resin and granule
Filtering, filtering residue has transferred to danger useless process qualification processed in units, and filtrate enters warehouse for finished product after packaging, obtains acrylic resin soln;
(5) prepared by adhesive: mixed according to weight ratio 1:0.05 with auxiliary agent by above-mentioned gained acrylic resin soln, and mixture is first
Supersound process 30min under supersonic frequency 40kHz, power 100W, under microwave frequency 2450MHz, power 700W at microwave
Reason 10min, pending thing naturally cools to room temperature, then stands overnight at 0-5 DEG C, finally utilizes ball mill to be milled to fineness
Less than 10 μm;
Described auxiliary agent is made up of the raw material of following parts by weight: chlorosulfonated polyethylene 10-15 part, rubber powder 7-10 part, activity are in vain
Soil 5-8 part, hydrogenated rosin 5-8 part, petroleum coke 4-6 part, rice bran wax 4-6 part, nanometer rubber powder 3-5 part, chlorobutanol 2-3 part,
Thiourea 2-3 part, bone black powder 1-2 part, nanometer aluminium powder 1-2 part, Matrii Sulfas Exsiccatus 1-2 part, sodium selenite 0.5-1 part, ethylenediamine two succinum
Acid trisodium 0.5-1 part, its preparation method is: first chlorosulfonated polyethylene, hydrogenated rosin and petroleum coke are sufficiently mixed, in Microwave Frequency
Microwave treatment 5min under rate 2450MHz, power 700W, adds rubber powder, rice bran wax and nanometer rubber powder, continues microwave treatment
10min, pending thing adds active hargil, chlorobutanol, bone black powder and nanometer aluminium powder after naturally cooling to 80-90 DEG C, fills
Divide sealing and standing 3h after mixing, be eventually adding thiourea, Matrii Sulfas Exsiccatus, sodium selenite and EDDS trisodium, be fully ground
Make its mix homogeneously.
The mill base adhesive utilizing acrylic resin to prepare the most according to claim 1, it is characterised in that: described monomer by
Methyl methacrylate, butyl acrylate, 2-(Acryloyloxy)ethanol, styrene and acrylic acid form by a certain percentage, and solvent is two
Toluene, initiator is dibenzoyl peroxide.
Priority Applications (1)
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CN201610411317.3A CN106085302A (en) | 2016-06-03 | 2016-06-03 | A kind of mill base adhesive utilizing acrylic resin to prepare |
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CN201610411317.3A CN106085302A (en) | 2016-06-03 | 2016-06-03 | A kind of mill base adhesive utilizing acrylic resin to prepare |
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CN106085302A true CN106085302A (en) | 2016-11-09 |
Family
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CN201610411317.3A Pending CN106085302A (en) | 2016-06-03 | 2016-06-03 | A kind of mill base adhesive utilizing acrylic resin to prepare |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108001023A (en) * | 2017-11-25 | 2018-05-08 | 茆莉娟 | A kind of gluing set composite of MULTILAYER COMPOSITE heavy wrapping corrugated board |
CN115819688A (en) * | 2022-12-30 | 2023-03-21 | 安徽聚合辐化化工有限公司 | Acrylic resin and preparation method thereof |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101921357A (en) * | 2010-08-17 | 2010-12-22 | 江门市制漆厂有限公司 | High-solid low-viscosity hydroxy acrylic resin and preparation process thereof |
CN101974276A (en) * | 2010-11-02 | 2011-02-16 | 江南大学 | Preparation method of self-crosslinked thermoplastic acrylate resin |
CN102952227A (en) * | 2012-11-06 | 2013-03-06 | 江苏三木化工股份有限公司 | Recoatable thermosetting acrylic acid resin for coating material and preparation method thereof |
CN103910825A (en) * | 2014-03-28 | 2014-07-09 | 江门市三木化工有限公司 | Novel resin and preparation method thereof |
-
2016
- 2016-06-03 CN CN201610411317.3A patent/CN106085302A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101921357A (en) * | 2010-08-17 | 2010-12-22 | 江门市制漆厂有限公司 | High-solid low-viscosity hydroxy acrylic resin and preparation process thereof |
CN101974276A (en) * | 2010-11-02 | 2011-02-16 | 江南大学 | Preparation method of self-crosslinked thermoplastic acrylate resin |
CN102952227A (en) * | 2012-11-06 | 2013-03-06 | 江苏三木化工股份有限公司 | Recoatable thermosetting acrylic acid resin for coating material and preparation method thereof |
CN103910825A (en) * | 2014-03-28 | 2014-07-09 | 江门市三木化工有限公司 | Novel resin and preparation method thereof |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108001023A (en) * | 2017-11-25 | 2018-05-08 | 茆莉娟 | A kind of gluing set composite of MULTILAYER COMPOSITE heavy wrapping corrugated board |
CN115819688A (en) * | 2022-12-30 | 2023-03-21 | 安徽聚合辐化化工有限公司 | Acrylic resin and preparation method thereof |
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Application publication date: 20161109 |