CN112724844A - Acrylate adhesive suitable for full-flow plastic spraying process - Google Patents
Acrylate adhesive suitable for full-flow plastic spraying process Download PDFInfo
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- CN112724844A CN112724844A CN202011465897.7A CN202011465897A CN112724844A CN 112724844 A CN112724844 A CN 112724844A CN 202011465897 A CN202011465897 A CN 202011465897A CN 112724844 A CN112724844 A CN 112724844A
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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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides an acrylate adhesive suitable for a full-flow plastic spraying process, which comprises the following components in volume ratio of 1: 8-12.5 of an oxidant component and a reducing agent component, wherein the oxidant component comprises methyl methacrylate, dibutyl phthalate, epoxy resin, nano calcium carbonate and an initiator, the epoxy resin is cured epoxy resin with the heat-resistant temperature of the maleic anhydride being more than 200 ℃, specifically 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate, and the reducing agent component comprises methyl methacrylate, liquid nitrile rubber, chlorosulfonated polyethylene, an accelerator, maleic acid and naphthoquinone. The acrylate adhesive suitable for the full-flow plastic spraying process provided by the invention selects the specific alkali-washing-resistant and high-temperature-resistant epoxy resin to form the oxidant component, and is matched with the reducing agent component containing the liquid nitrile rubber, so that the alkali-washing-resistant and high-temperature-resistant performance of the acrylate adhesive is improved, and the requirement suitable for the full-flow plastic spraying process is met.
Description
Technical Field
The invention belongs to the technical field of adhesive preparation, and particularly relates to an acrylate adhesive suitable for a full-flow plastic spraying process.
Background
The acrylate adhesive is one of the glue with the largest use amount, and plays an important role in national economic construction, national defense construction and daily life of people; the adhesive has the advantages of wide raw material sources, simple preparation process, quick drying and forming, good transparency and the like, has good adhesive property to various materials, also has good weather resistance, water resistance and chemical resistance, can be used for bonding materials such as metal, plastic, glue, wood, paper and the like, and has good adhesive property.
With the change of national environmental protection policy, the painting process of the parts of the passenger car is relatively changed. Under the current environmental protection policy, the whole on-line of a large-scale electrophoresis workshop is increasingly difficult, and the miniaturized and clean plastic spraying process is gradually applied widely.
In the prior art, the plastic spraying process has the following flow:
the first step is as follows: performing alkali washing at 120 ℃ for 60min, wherein the pH value of the alkali solution is more than or equal to 12;
the second step is that: washing, neutralizing and drying to pH 6-7;
the third step: spraying plastics, and baking at 220 deg.C for 60 min.
The parts of the passenger car are firstly bonded and then sprayed with plastic. The conditions of the plastic spraying process have extremely high performance requirements on the acrylate adhesive; the method specifically comprises the steps of requiring the product to be capable of enduring the whole process of 120 ℃ alkali washing for 60min (the pH value of alkali solution is more than or equal to 12), plastic spraying and 220 ℃ baking for 60min after curing, and after the plastic spraying is finished, carrying out the detection of breaking and dismantling of the finished part, wherein the cohesive failure of the bonding part is 100% and the strength attenuation rate is less than 15%.
The Chinese invention patent application with the application number of 201410763146.1 discloses an acrylate adhesive for a 180 ℃ finished automobile electrophoresis process, which improves the temperature resistance effect of the acrylate adhesive by selecting a maleimide compound as a modification auxiliary agent and can be used for 180 ℃ finished automobile electrophoresis; the product is tested by a whole-process powder spraying process, after being baked for 60min at 220 ℃, the product is broken and disassembled, the bonding interface is broken into 100 percent interface damage, and the strength is extremely low, which indicates that the product can not bear the high temperature of 220 ℃.
The Chinese patent application with the application number of CN201710435346.8 discloses a 5# acrylate adhesive, in particular to a single-component acrylate adhesive mainly comprising bisphenol ethylene glycol dimethacrylate, which can not meet the requirement of the whole process of the plastic spraying process.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide the acrylate adhesive suitable for the full-flow plastic spraying process, and the acrylate adhesive suitable for the full-flow plastic spraying process is prepared by building a novel redox system and efficiently initiating special alicyclic epoxy resin.
In order to achieve the purpose, the invention adopts the following technical scheme:
an acrylate adhesive suitable for a full-flow plastic spraying process comprises the following components in volume ratio of 1: an oxidant component and a reductant component of 8-12.5;
wherein:
the oxidant component comprises methyl methacrylate, dibutyl phthalate, epoxy resin, nano calcium carbonate and an initiator, wherein the epoxy resin is cured epoxy resin with the heat-resistant temperature of the maleic anhydride being more than 200 ℃;
the reducing agent component comprises methyl methacrylate, liquid nitrile rubber, chlorosulfonated polyethylene, an accelerator, maleic acid and naphthoquinone.
In the technical scheme, the epoxy resin is 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexyl formate.
Specifically, the structural formula of the 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexyl formate is shown as follows:
further, in the above technical solution, the epoxy resin is 20 to 40% by weight of the oxidant component.
In a preferred embodiment of the present invention, the oxidant component consists of, by weight, 10-30 parts of methyl methacrylate, 10-30 parts of dibutyl phthalate, 20-40 parts of epoxy resin, 18-24 parts of nano calcium carbonate, and 12-24 parts of an initiator.
In the technical scheme, the liquid nitrile rubber accounts for 10-30% of the reducing agent component in parts by weight.
In a preferred embodiment of the present invention, the reducing agent component consists of 30-70 parts by weight of methyl methacrylate, 10-30 parts by weight of liquid nitrile rubber, 5-40 parts by weight of chlorosulfonated polyethylene, 1-10 parts by weight of an accelerator, 2-3.6 parts by weight of maleic acid and 0.8-1.5 parts by weight of naphthoquinone.
Still further, in the above technical scheme, the acrylate adhesive suitable for the full-flow plastic spraying process is prepared from the following components in a volume ratio of 1: 10 of an oxidant component and a reductant component;
wherein:
the oxidant component comprises, by weight, 20-30 parts of methyl methacrylate, 10-18 parts of dibutyl phthalate, 24-36 parts of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate, 20 parts of nano calcium carbonate and 15 parts of an initiator;
the reducing agent comprises, by weight, 50-60 parts of methyl methacrylate, 10-20 parts of liquid nitrile rubber, 18-25 parts of chlorosulfonated polyethylene, 6 parts of an accelerator, 3 parts of maleic acid and 1 part of naphthoquinone.
Still further, in the above technical solution, the initiator is one or more of cumene hydroperoxide, benzoyl peroxide and tert-butyl peroxybenzoate.
Still further, in the above technical solution, the liquid nitrile rubber is one or more of carboxyl-terminated liquid nitrile rubber CTBN, amino-terminated liquid nitrile rubber ATBN, vinyl-terminated liquid nitrile rubber VTBN and epoxy-terminated liquid nitrile rubber, and is preferably vinyl-terminated liquid nitrile rubber VTBN.
Still further, in the above technical solution, the accelerator is one or more of tetramethylthiourea, ethylenethiourea, N-dimethyl-p-toluidine, triethylenediamine, diethylenetriamine, cobalt naphthenate, copper naphthenate, and vanadyl acetylacetonate.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the acrylate adhesive suitable for the full-flow plastic spraying process, the specific alkali-washing-resistant and high-temperature-resistant epoxy resin is selected to form the oxidant component, and the oxidant component is matched with the reducing agent component containing the liquid nitrile rubber, so that the alkali-washing-resistant and high-temperature-resistant performance of the acrylate adhesive is improved, and the requirement suitable for the full-flow plastic spraying process is met;
(2) the preparation method of the acrylate adhesive suitable for the full-flow plastic spraying process is simple and controllable, the used raw materials are common and easy to obtain, and the equipment used in the production process is common equipment in the industry.
Detailed Description
The present invention is further described in detail below with reference to specific examples so that those skilled in the art can more clearly understand the present invention.
The following examples are provided only for illustrating the present invention and are not intended to limit the scope of the present invention.
Unless otherwise specified, the technical means used in the examples of the present invention are conventional means well known to those skilled in the art.
The starting materials used in the examples of the present invention are all commercially available products unless otherwise specified.
All other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
The embodiment of the invention provides an acrylate adhesive suitable for a full-flow plastic spraying process, which comprises the following components in volume ratio of 1: an oxidant component and a reductant component of 8-12.5.
Wherein:
the oxidant component comprises, by weight, 10-30 parts of methyl methacrylate, 10-30 parts of dibutyl phthalate, 20-40 parts of epoxy resin, 18-24 parts of nano calcium carbonate and 12-24 parts of an initiator.
Specifically, the initiator is one or more of cumene hydroperoxide, benzoyl peroxide and tert-butyl peroxybenzoate.
The reducing agent comprises, by weight, 30-70 parts of methyl methacrylate, 10-30 parts of liquid nitrile rubber, 5-40 parts of chlorosulfonated polyethylene, 1-10 parts of an accelerator, 2-3.6 parts of maleic acid and 0.8-1.5 parts of naphthoquinone.
Specifically, the liquid nitrile rubber is one or more of carboxyl-terminated liquid nitrile rubber CTBN, amino-terminated liquid nitrile rubber ATBN, vinyl-terminated liquid nitrile rubber VTBN and epoxy-terminated liquid nitrile rubber.
Specifically, the accelerant is one or more of tetramethyl thiourea, ethylene thiourea, N-dimethyl-p-toluidine, triethylene diamine, diethylenetriamine, cobalt naphthenate, copper naphthenate and vanadyl acetylacetonate.
The embodiment of the invention also provides a preparation method of the acrylate adhesive suitable for the full-flow plastic spraying process, which specifically comprises the following steps:
s1, preparation of an oxidant component: weighing methyl methacrylate, dibutyl phthalate and nano calcium carbonate according to a ratio, adding the weighed materials into a reaction kettle, heating to 75 ℃, stirring for 150min until the materials are uniformly mixed, cooling to normal temperature, adding 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate and an initiator until the materials are uniformly mixed, vacuumizing, and discharging to obtain an oxidant component;
s2, preparation of a reducing agent component: weighing methyl methacrylate and chlorosulfonated polyethylene according to the proportion, adding into a reaction kettle, stirring at normal temperature until the methyl methacrylate and the chlorosulfonated polyethylene are completely dissolved, then adding liquid nitrile rubber and naphthoquinone, stirring for 150min until the nitrile rubber and the naphthoquinone are completely mixed uniformly, adding an accelerator and maleic acid, stirring for 90min until the nitrile rubber and the naphthoquinone are uniformly mixed, vacuumizing, and discharging to obtain the reducing agent component.
Through a large number of experiments, in the acrylate adhesive suitable for the full-process plastic spraying process, the optimal volume ratio of the oxidant component to the reducing agent component is 1: 10.
example 1
The embodiment of the invention provides an acrylate adhesive suitable for a full-flow plastic spraying process.
(1) The raw material ratio is as follows:
the volume ratio of the oxidant component to the reducing agent is 1: 10.
oxidant component
Reducing agent component
(2) The preparation method comprises the following steps:
s1, preparation of an oxidant component: weighing methyl methacrylate, dibutyl phthalate and nano calcium carbonate according to a ratio, adding the weighed materials into a reaction kettle, heating to 75 ℃, stirring for 150min until the materials are uniformly mixed, cooling to normal temperature, adding 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate and an initiator until the materials are uniformly mixed, vacuumizing, and discharging to obtain an oxidant component;
s2, preparation of a reducing agent component: weighing methyl methacrylate and chlorosulfonated polyethylene according to a ratio, adding into a reaction kettle, stirring at normal temperature until the methyl methacrylate and the chlorosulfonated polyethylene are completely dissolved, then adding liquid nitrile rubber and naphthoquinone, stirring for 150min until the nitrile rubber and the naphthoquinone are completely mixed uniformly, adding an accelerator and maleic acid, stirring for 90min until the nitrile rubber and the naphthoquinone are uniformly mixed, vacuumizing, and discharging to obtain a reducing agent component;
s3, mixing an oxidant component and a reducing agent component according to a volume ratio of 1: 10, and obtaining the acrylate adhesive suitable for the full-flow plastic spraying process.
Example 2
The embodiment of the invention provides an acrylate adhesive suitable for a full-flow plastic spraying process.
(1) The raw material ratio is as follows:
the volume ratio of the oxidant component to the reducing agent is 1: 10.
oxidant component
Reducing agent component
(2) The preparation method comprises the following steps:
similar to embodiment 1, further description is omitted here.
Example 3
The embodiment of the invention provides an acrylate adhesive suitable for a full-flow plastic spraying process.
(1) The raw material ratio is as follows:
the volume ratio of the oxidant component to the reducing agent is 1: 10.
oxidant component
Reducing agent component
(2) The preparation method comprises the following steps:
similar to embodiment 1, further description is omitted here.
Example 4
The embodiment of the invention provides an acrylate adhesive suitable for a full-flow plastic spraying process.
(1) The raw material ratio is as follows:
the volume ratio of the oxidant component to the reducing agent is 1: 10.
oxidant component
Reducing agent component
(2) The preparation method comprises the following steps:
similar to embodiment 1, further description is omitted here.
Example 5
The embodiment of the invention provides an acrylate adhesive suitable for a full-flow plastic spraying process.
(1) The raw material ratio is as follows:
the volume ratio of the oxidant component to the reducing agent is 1: 10.
oxidant component
Reducing agent component
(2) The preparation method comprises the following steps:
similar to embodiment 1, further description is omitted here.
Example 6
The embodiment of the invention provides an acrylate adhesive suitable for a full-flow plastic spraying process.
(1) The raw material ratio is as follows:
the volume ratio of the oxidant component to the reducing agent is 1: 8.5.
oxidant component
Reducing agent component
(2) The preparation method comprises the following steps:
similar to embodiment 1, further description is omitted here.
Example 7
The embodiment of the invention provides an acrylate adhesive suitable for a full-flow plastic spraying process.
(1) The raw material ratio is as follows:
the volume ratio of the oxidant component to the reducing agent is 1: 11.8.
oxidant component
Reducing agent component
(2) The preparation method comprises the following steps:
similar to embodiment 1, further description is omitted here.
Comparative example 1
The invention provides an acrylate adhesive suitable for a full-flow plastic spraying process.
(1) The raw material ratio is as follows:
the volume ratio of the oxidant component to the reducing agent is 1: 10.
oxidant component
Reducing agent component
(2) The preparation method comprises the following steps:
similar to embodiment 1, further description is omitted here.
Comparative example 2
The embodiment of the invention provides an acrylate adhesive suitable for a full-flow plastic spraying process.
(1) The raw material ratio is as follows:
the volume ratio of the oxidant component to the reducing agent is 1: 10.
oxidant component
Reducing agent component
(2) The preparation method comprises the following steps:
similar to embodiment 1, further description is omitted here.
Test examples
After the preparation of the acrylate adhesive is completed, the peel strength of the cured product and the peel strength of the cured product after aging are tested, and the specific test method is as follows:
(1) method for testing normal temperature peel strength
Using an aluminum alloy test piece with the model of 6063 to manufacture a test sample piece, standing at normal temperature for 24 hours, and testing according to a standard GB/T2792-2014 adhesive tape peel strength measuring method;
(2) method for testing peel strength after aging
The first step is as follows: performing alkali washing at 120 ℃ for 60min, wherein the pH value of the alkali solution is more than or equal to 12;
the second step is that: washing, neutralizing and drying to pH 6-7;
the third step: spraying plastics, and baking at 220 deg.C for 60 min;
the fourth step: standing at normal temperature for 4h, and testing according to a standard GB/T2792-2014 determination method for adhesive tape peel strength.
The test results were as follows:
the above results were analyzed to find that:
1. when 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate is not selected as epoxy resin in the acrylate adhesive, the retention rate of the peeling strength after the whole-process aging is only 50%, the strength is at a lower level and is easy to crack, and meanwhile, when the using amount of the 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate is reduced, the retention rate of the peeling strength after the whole-process aging is gradually reduced, namely the 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate can effectively improve the peeling strength of the product after the whole-process aging, and plays a main role in maintaining the peeling strength after the whole-process aging;
2. the liquid nitrile rubber has a relatively obvious effect on the improvement of normal-temperature peeling, the retention rate of the peeling strength after the whole process is aged is gradually reduced along with the reduction of the using amount of the liquid nitrile rubber, but the influence on the reduction range is less than that of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate, and the liquid nitrile rubber and the 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate synergistically improve the retention of the peeling strength after the whole process is aged.
Finally, the method of the present invention is only a preferred embodiment and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An acrylate adhesive suitable for a full-flow plastic spraying process is characterized in that,
comprises the following components in a volume ratio of 1: an oxidant component and a reductant component of 8-12.5;
wherein:
the oxidant component comprises methyl methacrylate, dibutyl phthalate, epoxy resin, nano calcium carbonate and an initiator, wherein the epoxy resin is cured epoxy resin with the heat-resistant temperature of the maleic anhydride being more than 200 ℃;
the reducing agent component comprises methyl methacrylate, liquid nitrile rubber, chlorosulfonated polyethylene, an accelerator, maleic acid and naphthoquinone.
2. The acrylate adhesive suitable for the full-flow plastic spraying process according to claim 1,
the epoxy resin is 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate.
3. The acrylate adhesive suitable for the full-flow plastic spraying process according to claim 1 or 2,
the weight percentage of the epoxy resin in the oxidant component is 20-40%.
4. The acrylate adhesive suitable for the full-flow plastic spraying process according to any one of claims 1 to 3,
the oxidant component comprises, by weight, 10-30 parts of methyl methacrylate, 10-30 parts of dibutyl phthalate, 20-40 parts of epoxy resin, 18-24 parts of nano calcium carbonate and 12-24 parts of an initiator.
5. The acrylate adhesive suitable for the full-flow plastic spraying process according to claim 1,
the weight percentage content of the liquid nitrile rubber in the reducing agent component is 10-30%.
6. The acrylate adhesive suitable for the full-flow plastic spraying process according to claim 1 or 5,
the reducing agent comprises, by weight, 30-70 parts of methyl methacrylate, 10-30 parts of liquid nitrile rubber, 5-40 parts of chlorosulfonated polyethylene, 1-10 parts of an accelerator, 2-3.6 parts of maleic acid and 0.8-1.5 parts of naphthoquinone.
7. The acrylate adhesive suitable for the full-flow plastic spraying process according to any one of claims 1 to 6,
the volume ratio of 1: 10 of an oxidant component and a reductant component;
wherein:
the oxidant component comprises, by weight, 20-30 parts of methyl methacrylate, 10-18 parts of dibutyl phthalate, 24-36 parts of 3, 4-epoxy cyclohexyl methyl-3, 4-epoxy cyclohexyl formate, 20 parts of nano calcium carbonate and 15 parts of an initiator;
the reducing agent comprises, by weight, 50-60 parts of methyl methacrylate, 10-20 parts of liquid nitrile rubber, 18-25 parts of chlorosulfonated polyethylene, 6 parts of an accelerator, 3 parts of maleic acid and 1 part of naphthoquinone.
8. The acrylate adhesive suitable for the full-flow plastic spraying process according to any one of claims 1 to 7,
the initiator is one or more of cumene hydroperoxide, benzoyl peroxide and tert-butyl peroxybenzoate.
9. The acrylate adhesive suitable for the full-flow plastic spraying process according to any one of claims 1 to 7,
the liquid nitrile rubber is one or more of carboxyl-terminated liquid nitrile rubber CTBN, amino-terminated liquid nitrile rubber ATBN, vinyl-terminated liquid nitrile rubber VTBN and epoxy-terminated liquid nitrile rubber, and is preferably vinyl-terminated liquid nitrile rubber VTBN.
10. The acrylate adhesive suitable for the full-flow plastic spraying process according to any one of claims 1 to 7,
the accelerant is one or more of tetramethyl thiourea, ethylene thiourea, N-dimethyl-p-toluidine, triethylene diamine, diethylenetriamine, cobalt naphthenate, copper naphthenate and vanadyl acetylacetonate.
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Cited By (1)
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CN110577804A (en) * | 2019-09-17 | 2019-12-17 | 湖北回天新材料股份有限公司 | Environment-friendly acrylate adhesive with low TVOC (total volatile organic compound) |
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CN106634728A (en) * | 2016-12-14 | 2017-05-10 | 湖北回天新材料股份有限公司 | Acrylate adhesive for bonding car SMC (sheet molding compound) spoilers |
CN106752984A (en) * | 2016-12-14 | 2017-05-31 | 湖北回天新材料股份有限公司 | A kind of SGA for being bonded motor-car skirting |
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