CN110655884A - Nano-material modified acrylate pressure-sensitive adhesive and preparation method thereof - Google Patents
Nano-material modified acrylate pressure-sensitive adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN110655884A CN110655884A CN201911020976.4A CN201911020976A CN110655884A CN 110655884 A CN110655884 A CN 110655884A CN 201911020976 A CN201911020976 A CN 201911020976A CN 110655884 A CN110655884 A CN 110655884A
- Authority
- CN
- China
- Prior art keywords
- percent
- sensitive adhesive
- functional monomer
- titanium dioxide
- acrylate
- Prior art date
- 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.)
- Pending
Links
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
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/068—Copolymers with monomers not covered by C09J133/06 containing glycidyl groups
-
- 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
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
-
- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention disclosesA nano material modified acrylate pressure-sensitive adhesive comprises the following components in percentage by weight: 45-52% of soft monomer, 3-6% of hard monomer, 5-10% of functional monomer, 1.5-4.5% of emulsifier, 0.1-0.3% of initiator, 0.15-0.25% of oxidant, 0.5-1% of ammonia water and the balance of deionized water. The modified acrylate pressure-sensitive adhesive is prepared by adding a titanium dioxide and graphene oxide mixed modified functional monomer into a functional monomer, so that the surface resistivity of the pressure-sensitive adhesive can reach 1 x 105Omega, and can also make the pressure-sensitive adhesive aging-resistant, 70 ℃ yellowing-resistant performance improve notably, it is a transparent, esthetic new pressure-sensitive adhesive material.
Description
Technical Field
The invention relates to the technical field of pressure-sensitive adhesives, in particular to a nano-material modified acrylate pressure-sensitive adhesive and a preparation method thereof.
Background
The pressure-sensitive adhesive is an adhesive sensitive to pressure in the bonding process, and can form larger bonding under the action of smaller pressure. Because the acrylate pressure-sensitive adhesive has good light resistance, aging resistance and water resistance, and has good pressure-sensitive property, adhesiveness and stability, the acrylate pressure-sensitive adhesive is widely applied in many fields.
However, the traditional pressure-sensitive adhesive has poor performances in the aspects of electromagnetic shielding, high temperature resistance, yellowing resistance and the like, so that the prepared raw materials and the preparation method need to be modified. Therefore, the invention provides a nano material modified acrylate pressure-sensitive adhesive and a preparation method thereof.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a nano material modified acrylate pressure-sensitive adhesive and a preparation method thereof.
The technical scheme of the invention is as follows:
a nano material modified acrylate pressure-sensitive adhesive comprises the following components in percentage by weight:
45 to 52 percent of soft monomer
3 to 6 percent of hard monomer
5 to 10 percent of functional monomer
Emulsifier 1.5-4.5%
0.1 to 0.3 percent of initiator
0.15 to 0.25 percent of oxidant
0.5 to 1 percent of ammonia water
The balance of deionized water.
Preferably, one or more of n-butyl acrylate, isooctyl acrylate and ethyl acrylate are optionally combined; the hard monomer is one or the combination of more than two of methyl methacrylate, styrene and vinyl acetate.
Preferably, the functional monomer comprises a nanomaterial-modified functional monomer.
Preferably, the nanomaterial modified functional monomer is a titanium dioxide and graphene oxide mixed modified functional monomer.
Further preferably, in the titanium dioxide and graphene oxide mixed modified functional monomer, the weight percentage content of each component is as follows:
0.2 to 0.5 percent of graphene oxide
0.01 to 0.05 percent of triethylamine
0.02-0.08% of phenol
1.2 to 2.0 percent of nano titanium dioxide
The rest is glycidyl acrylate.
Further preferably, the preparation method of the titanium dioxide and graphene oxide mixed modified functional monomer comprises the following steps:
(1) uniformly mixing graphene oxide, triethylamine and phenol in proportion, introducing nitrogen, and heating to 90-120 ℃;
(2) slowly dropwise adding glycidyl acrylate for 3-5h, and reacting for 2-4h under the condition of heat preservation; adding deionized water, and adjusting the pH value to be between 1 and 2; then adding sodium dodecyl benzene sulfonate, and uniformly mixing to form emulsion; adding a titanium dioxide precursor into the mixed solution, and generating nano titanium dioxide particles through a hydrolytic condensation reaction, wherein the nano titanium dioxide particles are uniformly dispersed in the mixed solution;
(3) and standing the mixed solution for layering, taking the upper layer liquid, concentrating, and performing spray drying to obtain the modified functional monomer.
Preferably, the functional monomer further comprises one or any combination of more than two of acrylic acid, methacrylic acid, hydroxyethyl acrylate and glycidyl acrylate.
Preferably, the emulsifier is nonylphenol polyoxyethylene ether; the initiator is one or any combination of two of potassium persulfate and ammonium persulfate; the oxidant is hydrogen peroxide.
A preparation method of a nano material modified acrylate pressure-sensitive adhesive comprises the following steps:
A. emulsifying 48-55% of deionized water, 40-45% of emulsifier, 20-25% of initiator, and all soft monomers, hard monomers and functional monomers in a pre-emulsifier for 15-20min to obtain pre-emulsion;
B. adding the rest deionized water, emulsifier and initiator into a polymerization reactor, stirring and heating to 80-85 ℃, adding 15-20% of the weight of the pre-emulsion, reacting for 30-40min, dropwise adding the rest pre-emulsion, and controlling the reaction time to 3-3.5 h;
C. keeping the temperature for 2-2.5h, cooling to 60-65 ℃, adding an oxidant, and cooling to 45-50 ℃;
D. adding ammonia water to adjust the pH value to 7.5-8, filtering and discharging.
The invention has the advantages that: according to the nano-material modified acrylate pressure-sensitive adhesive, the functional monomer is modified by adding the titanium dioxide and the graphene oxide, so that the surface resistivity of the pressure-sensitive adhesive can reach 1 × 105Omega, and can also make the pressure-sensitive adhesive aging-resistant, 70 ℃ yellowing-resistant performance improve notably, it is a transparent, esthetic new pressure-sensitive adhesive material.
Detailed Description
Example 1
A nano material modified acrylate pressure-sensitive adhesive comprises the following components in percentage by weight:
n-butyl acrylate 32%
Isooctyl acrylate 12%
Ethyl acrylate 5%
Styrene 2%
2.5 percent of vinyl acetate
2.5 percent of nano material modified functional monomer
Acrylic acid 1.5%
2 percent of hydroxyethyl acrylate
1.5 percent of glycidyl acrylate
Polyoxyethylene nonyl phenyl ether 3%
Ammonium persulfate 0.25%
0.2 percent of hydrogen peroxide
0.8 percent of ammonia water
The balance of deionized water.
The nano material modified functional monomer is a titanium dioxide and graphene oxide mixed modified functional monomer.
In the titanium dioxide and graphene oxide mixed modified functional monomer, the weight percentage of each component is as follows:
0.35 percent of graphene oxide
0.03 percent of triethylamine
0.06 percent of phenol
1.7 percent of nano titanium dioxide
The rest is glycidyl acrylate.
The preparation method of the titanium dioxide and graphene oxide mixed modified functional monomer comprises the following steps:
(1) uniformly mixing graphene oxide, triethylamine and phenol in proportion, introducing nitrogen, and heating to 105 ℃;
(2) slowly dropwise adding glycidyl acrylate for 3.5h, and reacting for 3h under the condition of heat preservation; adding deionized water, and adjusting the pH value to 1.8; then adding sodium dodecyl benzene sulfonate, and uniformly mixing to form emulsion;
(3) adding tetraethyl titanate into the solution, and generating nano titanium dioxide particles through a hydrolytic condensation reaction, wherein the nano titanium dioxide particles are uniformly dispersed in the mixed solution;
(4) and standing the mixed solution for layering, taking the upper layer liquid, concentrating, and performing spray drying to obtain the modified functional monomer.
The preparation method of the nano material modified acrylate pressure-sensitive adhesive comprises the following steps:
A. emulsifying 52% of the total weight of the deionized water, 42% of the total weight of the emulsifier, 23% of the total weight of the initiator, all soft monomers, hard monomers and functional monomers in a pre-emulsifier for 18min to obtain pre-emulsion;
B. adding the rest deionized water, the emulsifier and the initiator into a polymerization reactor, stirring and heating to 82 ℃, adding 18% of the weight of the pre-emulsion, reacting for 35min, dropwise adding the rest pre-emulsion, and controlling the reaction time to be 3.2 h;
C. after preserving heat for 2.2h, cooling to 62 ℃, adding an oxidant, and cooling to 48 ℃;
D. adding ammonia water to adjust the pH value to 7.5-8, filtering and discharging.
The surface resistivity of the modified acrylate pressure-sensitive adhesive of example 1 was 5.8X 105Ω。
Example 2
A nano material modified acrylate pressure-sensitive adhesive comprises the following components in percentage by weight:
n-butyl acrylate 35%
10 percent of ethyl acrylate
Methyl methacrylate 3%
1 percent of styrene
Vinyl acetate 2%
2.5 percent of nano material modified functional monomer
Acrylic acid 1%
1.5 percent of glycidyl acrylate
4.5 percent of polyoxyethylene nonyl phenyl ether
Potassium persulfate and ammonium persulfate 0.1%
0.25 percent of hydrogen peroxide
0.5 percent of ammonia water
The balance of deionized water.
The nano material modified functional monomer is a titanium dioxide and graphene oxide mixed modified functional monomer.
In the titanium dioxide and graphene oxide mixed modified functional monomer, the weight percentage of each component is as follows:
0.2 percent of graphene oxide
0.05 percent of triethylamine
0.02 percent of phenol
2.0 percent of nano titanium dioxide
The rest is glycidyl acrylate.
The preparation method of the titanium dioxide and graphene oxide mixed modified functional monomer comprises the following steps:
(1) uniformly mixing graphene oxide, triethylamine and phenol in proportion, introducing nitrogen, and heating to 90 ℃;
(2) slowly dropwise adding glycidyl acrylate for 5h, and reacting for 2h under the condition of heat preservation; adding deionized water, and adjusting the pH value to be 2.0; then adding sodium dodecyl benzene sulfonate, and uniformly mixing to form emulsion;
(3) adding tetraethyl titanate into the solution, and generating nano titanium dioxide particles through a hydrolytic condensation reaction, wherein the nano titanium dioxide particles are uniformly dispersed in the mixed solution;
(4) and standing the mixed solution for layering, taking the upper layer liquid, concentrating, and performing spray drying to obtain the modified functional monomer.
The preparation method of the nano material modified acrylate pressure-sensitive adhesive comprises the following steps:
A. emulsifying 48 percent of the total weight of the deionized water, 45 percent of the total weight of the emulsifier, 20 percent of the total weight of the initiator, all soft monomers, hard monomers and functional monomers in a pre-emulsifier for 20min to obtain pre-emulsion;
B. adding the rest deionized water, the emulsifier and the initiator into a polymerization reactor, stirring and heating to 80 ℃, adding 20% of the weight of the pre-emulsion, reacting for 30min, dropwise adding the rest pre-emulsion, and controlling the reaction time to be 3.5 h;
C. after preserving heat for 2 hours, cooling, adding an oxidant, and cooling to 45 ℃;
D. adding ammonia water to adjust the pH value to 8, filtering and discharging.
The surface resistivity of the modified acrylate pressure-sensitive adhesive of example 2 was 6.2X 105Ω。
Example 3
A nano material modified acrylate pressure-sensitive adhesive comprises the following components in percentage by weight:
n-butyl acrylate 38%
8 percent of isooctyl acrylate
6 percent of ethyl acrylate
Methyl methacrylate 1.5%
Vinyl acetate 1.5%
3.5 percent of nano material modified functional monomer
Acrylic acid 2.5%
Methacrylic acid 1%
2 percent of hydroxyethyl acrylate
1 percent of glycidyl acrylate
Nonylphenol polyoxyethylene ether 1.5%
Potassium persulfate and ammonium persulfate 0.3%
0.15 percent of hydrogen peroxide
1 percent of ammonia water
The balance of deionized water.
The nano material modified functional monomer is a titanium dioxide and graphene oxide mixed modified functional monomer.
In the titanium dioxide and graphene oxide mixed modified functional monomer, the weight percentage of each component is as follows:
0.5 percent of graphene oxide
0.01 percent of triethylamine
0.08 percent of phenol
1.2 percent of nano titanium dioxide
The rest is glycidyl acrylate.
The preparation method of the titanium dioxide and graphene oxide mixed modified functional monomer comprises the following steps:
(1) uniformly mixing graphene oxide, triethylamine and phenol in proportion, introducing nitrogen, and heating to 120 ℃;
(2) slowly dropwise adding glycidyl acrylate for 3 hours, and reacting for 4 hours under the condition of heat preservation; adding deionized water, and adjusting the pH value to be 1.0; then adding sodium dodecyl benzene sulfonate, and uniformly mixing to form emulsion;
(3) adding tetraethyl titanate into the solution, and generating nano titanium dioxide particles through a hydrolytic condensation reaction, wherein the nano titanium dioxide particles are uniformly dispersed in the mixed solution;
(4) and standing the mixed solution for layering, taking the upper layer liquid, concentrating, and performing spray drying to obtain the modified functional monomer.
The preparation method of the nano material modified acrylate pressure-sensitive adhesive comprises the following steps:
A. emulsifying 55% of the total weight of the deionized water, 40% of the total weight of the emulsifier, 25% of the total weight of the initiator, all soft monomers, hard monomers and functional monomers in a pre-emulsifier for 15min to obtain pre-emulsion;
B. adding the rest deionized water, the emulsifier and the initiator into a polymerization reactor, stirring and heating to 85 ℃, adding 15% of the weight of the pre-emulsion, reacting for 40min, dropwise adding the rest pre-emulsion, and controlling the reaction time for 3 h;
C. keeping the temperature for 2.5h, cooling to 60 ℃, adding an oxidant, and cooling to 50 ℃;
D. adding ammonia water to adjust the pH value to 7.5-8, filtering and discharging.
The surface resistivity of the modified acrylate pressure-sensitive adhesive of example 3 was 9.6X 105Ω。
Comparative example 1
The nanomaterial modified functional monomer in example 1 was removed, and the rest of the formulation and preparation method were unchanged.
The pressure-sensitive adhesives of examples 1 to 3 and comparative example 1 were subjected to the application test below, and the specific test results are shown in table 1.
The test method comprises the following steps:
coating water-based acrylate pressure-sensitive adhesive on one side of the PET film, drying, and curling into an adhesive tape with the width of 48mm, the inner diameter of 300mm and the length of 200 m; the thickness of the coating of the pressure-sensitive adhesive is 25 μm;
adhesive force: according to PSTC-101;
retention force: according to PSTC-101;
temperature resistance: sticking the pressure sensitive adhesive coated on PET film with thickness of 25 μm on steel plate, standing in oven at 120 deg.C, 150 deg.C, 180 deg.C, 200 deg.C, 220 deg.C for 30min, taking out the steel plate, hot peeling and cold peeling, and observing whether there is residual adhesive;
yellowing resistance at 70 ℃: the temperature is 70 ℃, the humidity is 95% R.H., the constant temperature and the constant humidity are not interrupted for 720 hours, the width of the adhesive tape is 48mm, the inner diameter is 300mm, and the length is 200 m.
Table 1: results of application test of the pressure-sensitive adhesives of examples 1 to 3 and comparative example 1;
| example 1 | Example 2 | Example 3 | Comparative example 1 | |
| Pressure sensitive adhesive thickness μm | 25 | 25 | 25 | 25 |
| Adhesive force kgf/25mm | 0.65 | 0.69 | 0.55 | 0.62 |
| Retention force h/25 mm | ＞1000 | ＞1000 | ＞1000 | ＞1000 |
| Temperature resistance | ＞220 | ＞220 | ＞220 | 120 |
| Yellowing resistance at 70 DEG C | Does not turn yellow | Does not turn yellow | Does not turn yellow | Significant yellowing |
From the test data, the nanomaterial modified acrylate pressure-sensitive adhesive disclosed by the invention has very good temperature resistance and yellowing resistance.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The nano-material modified acrylate pressure-sensitive adhesive is characterized by comprising the following components in percentage by weight:
45 to 52 percent of soft monomer
3 to 6 percent of hard monomer
5 to 10 percent of functional monomer
Emulsifier 1.5-4.5%
0.1 to 0.3 percent of initiator
0.15 to 0.25 percent of oxidant
0.5 to 1 percent of ammonia water
The balance of deionized water.
2. The nanomaterial-modified acrylate pressure-sensitive adhesive according to claim 1, wherein the pressure-sensitive adhesive is one or any combination of two or more of n-butyl acrylate, isooctyl acrylate and ethyl acrylate; the hard monomer is one or the combination of more than two of methyl methacrylate, styrene and vinyl acetate.
3. The nanomaterial-modified acrylate pressure-sensitive adhesive of claim 1 wherein the functional monomer comprises a nanomaterial-modified functional monomer.
4. The nanomaterial-modified acrylate pressure-sensitive adhesive according to claim 3, wherein the nanomaterial-modified functional monomer is a mixed modified functional monomer of titanium dioxide and graphene oxide.
5. The nanomaterial-modified acrylate pressure-sensitive adhesive according to claim 4, wherein the mixed modified functional monomer of titanium dioxide and graphene oxide comprises the following components in percentage by weight:
0.2 to 0.5 percent of graphene oxide
0.01 to 0.05 percent of triethylamine
0.02-0.08% of phenol
1.2 to 2.0 percent of nano titanium dioxide
The rest is glycidyl acrylate.
6. The nanomaterial-modified acrylate pressure-sensitive adhesive according to claim 5, wherein the preparation method of the titanium dioxide and graphene oxide mixed modified functional monomer comprises the following steps:
(1) uniformly mixing graphene oxide, triethylamine and phenol in proportion, introducing nitrogen, and heating to 90-120 ℃;
(2) slowly dropwise adding glycidyl acrylate for 3-5h, and reacting for 2-4h under the condition of heat preservation; adding deionized water, and adjusting the pH value to be between 1 and 2; then adding sodium dodecyl benzene sulfonate, and uniformly mixing to form emulsion;
(3) adding a titanium dioxide precursor into the mixed solution, and generating nano titanium dioxide particles through a hydrolytic condensation reaction, wherein the nano titanium dioxide particles are uniformly dispersed in the mixed solution;
(4) and standing the mixed solution for layering, taking the upper layer liquid, concentrating, and performing spray drying to obtain the modified functional monomer.
7. The nanomaterial-modified acrylate pressure-sensitive adhesive according to any one of claims 3 to 6, wherein the functional monomer further comprises one or any combination of two or more of acrylic acid, methacrylic acid, hydroxyethyl acrylate and glycidyl acrylate.
8. The nanomaterial-modified acrylate pressure-sensitive adhesive of claim 1, wherein the emulsifier is nonylphenol polyoxyethylene ether; the initiator is one or any combination of two of potassium persulfate and ammonium persulfate; the oxidant is hydrogen peroxide.
9. The nanomaterial-modified acrylate pressure-sensitive adhesive according to claim 1, wherein the preparation method comprises the following steps:
A. emulsifying 48-55% of deionized water, 40-45% of emulsifier, 20-25% of initiator, and all soft monomers, hard monomers and functional monomers in a pre-emulsifier for 15-20min to obtain pre-emulsion;
B. adding the rest deionized water, emulsifier and initiator into a polymerization reactor, stirring and heating to 80-85 ℃, adding 15-20% of the weight of the pre-emulsion, reacting for 30-40min, dropwise adding the rest pre-emulsion, and controlling the reaction time to 3-3.5 h;
C. keeping the temperature for 2-2.5h, cooling to 60-65 ℃, adding an oxidant, and cooling to 45-50 ℃;
D. adding ammonia water to adjust the pH value to 7.5-8, filtering and discharging.
10. The nanomaterial-modified acrylate pressure-sensitive adhesive according to claim 1, which is composed of the following components in percentage by weight:
n-butyl acrylate 32%
Isooctyl acrylate 12%
Ethyl acrylate 5%
Styrene 2%
2.5 percent of vinyl acetate
2.5 percent of nano material modified functional monomer
Acrylic acid 1.5%
2 percent of hydroxyethyl acrylate
1.5 percent of glycidyl acrylate
Polyoxyethylene nonyl phenyl ether 3%
Ammonium persulfate 0.25%
0.2 percent of hydrogen peroxide
0.8 percent of ammonia water
The balance of deionized water;
the nano material modified functional monomer is a titanium dioxide and graphene oxide mixed modified functional monomer;
in the titanium dioxide and graphene oxide mixed modified functional monomer, the weight percentage of each component is as follows:
0.35 percent of graphene oxide
0.03 percent of triethylamine
0.06 percent of phenol
1.7 percent of nano titanium dioxide
The rest of glycidyl acrylate;
the preparation method of the titanium dioxide and graphene oxide mixed modified functional monomer comprises the following steps:
(1) uniformly mixing graphene oxide, triethylamine and phenol in proportion, introducing nitrogen, and heating to 105 ℃;
(2) slowly dropwise adding glycidyl acrylate for 3.5h, and reacting for 3h under the condition of heat preservation; adding deionized water, and adjusting the pH value to 1.8; then adding sodium dodecyl benzene sulfonate, and uniformly mixing to form emulsion;
(3) adding tetraethyl titanate into the solution, and generating nano titanium dioxide particles through a hydrolytic condensation reaction, wherein the nano titanium dioxide particles are uniformly dispersed in the mixed solution;
(4) standing the mixed solution for layering, taking the upper layer liquid, concentrating, and spray drying to obtain a modified functional monomer;
the preparation method of the nano material modified acrylate pressure-sensitive adhesive comprises the following steps:
A. emulsifying 52% of the total weight of the deionized water, 42% of the total weight of the emulsifier, 23% of the total weight of the initiator, all soft monomers, hard monomers and functional monomers in a pre-emulsifier for 18min to obtain pre-emulsion;
B. adding the rest deionized water, the emulsifier and the initiator into a polymerization reactor, stirring and heating to 82 ℃, adding 18% of the weight of the pre-emulsion, reacting for 35min, dropwise adding the rest pre-emulsion, and controlling the reaction time to be 3.2 h;
C. after preserving heat for 2.2h, cooling to 62 ℃, adding an oxidant, and cooling to 48 ℃;
D. adding ammonia water to adjust the pH value to 7.5-8, filtering and discharging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911020976.4A CN110655884A (en) | 2019-10-25 | 2019-10-25 | Nano-material modified acrylate pressure-sensitive adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911020976.4A CN110655884A (en) | 2019-10-25 | 2019-10-25 | Nano-material modified acrylate pressure-sensitive adhesive and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110655884A true CN110655884A (en) | 2020-01-07 |
Family
ID=69042212
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911020976.4A Pending CN110655884A (en) | 2019-10-25 | 2019-10-25 | Nano-material modified acrylate pressure-sensitive adhesive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110655884A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260479A (en) * | 2010-12-14 | 2011-11-30 | 上海凯鑫森产业投资控股有限公司 | Crylic acid grafted nano material aqueous pressure-sensitive adhesive for electronic-grade protective film |
| CN104774579A (en) * | 2015-04-24 | 2015-07-15 | 苏州市新广益电子有限公司 | High-temperature-resistant pressure-sensitive adhesive tape and heat-resistant pressure-sensitive adhesive used by same |
| CN105694772A (en) * | 2014-11-26 | 2016-06-22 | 邢国爱 | Acrylate emulsion pressure-sensitive adhesive with yellowing resistance |
| CN106366983A (en) * | 2016-09-06 | 2017-02-01 | 哈尔滨工业大学无锡新材料研究院 | Acrylic ester electromagnetic shielding pressure-sensitive adhesive and preparation method thereof |
| CN107236378A (en) * | 2017-04-14 | 2017-10-10 | 南通强生光电科技有限公司 | Solar cell backboard coating composition and its solar cell backboard |
| KR101864845B1 (en) * | 2018-01-05 | 2018-06-05 | 주식회사 태림산업 | Eco-friendly adhesive for PVC |
| CN108329869A (en) * | 2018-01-16 | 2018-07-27 | 广东鑫丰海电子科技有限公司 | A kind of optics acrylic acid adhesive and film protective film and preparation method |
-
2019
- 2019-10-25 CN CN201911020976.4A patent/CN110655884A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260479A (en) * | 2010-12-14 | 2011-11-30 | 上海凯鑫森产业投资控股有限公司 | Crylic acid grafted nano material aqueous pressure-sensitive adhesive for electronic-grade protective film |
| CN105694772A (en) * | 2014-11-26 | 2016-06-22 | 邢国爱 | Acrylate emulsion pressure-sensitive adhesive with yellowing resistance |
| CN104774579A (en) * | 2015-04-24 | 2015-07-15 | 苏州市新广益电子有限公司 | High-temperature-resistant pressure-sensitive adhesive tape and heat-resistant pressure-sensitive adhesive used by same |
| CN106366983A (en) * | 2016-09-06 | 2017-02-01 | 哈尔滨工业大学无锡新材料研究院 | Acrylic ester electromagnetic shielding pressure-sensitive adhesive and preparation method thereof |
| CN107236378A (en) * | 2017-04-14 | 2017-10-10 | 南通强生光电科技有限公司 | Solar cell backboard coating composition and its solar cell backboard |
| KR101864845B1 (en) * | 2018-01-05 | 2018-06-05 | 주식회사 태림산업 | Eco-friendly adhesive for PVC |
| CN108329869A (en) * | 2018-01-16 | 2018-07-27 | 广东鑫丰海电子科技有限公司 | A kind of optics acrylic acid adhesive and film protective film and preparation method |
Non-Patent Citations (3)
| Title |
|---|
| 惠会清等: "《普通化学实验》", 31 August 2005, 陕西科学技术出版社 * |
| 涂料工艺编委会: "《涂料工艺》", 31 December 1997, 化学工业出版社 * |
| 王全杰等: ""纳米二氧化钛共混发改性丙烯酸树脂涂饰剂的研究"", 《中国皮革》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106520033A (en) | Acrylic ester pressure-sensitive adhesive with high permanent adhesion performance at 80 DEG C and preparation method thereof | |
| CN113372854B (en) | Thin-coating high-viscosity water-based polyacrylate pressure-sensitive adhesive and preparation method and application thereof | |
| JP6510567B2 (en) | Acrylic emulsion pressure sensitive adhesive excellent in low temperature adhesion and holding power and method for producing the same | |
| CA2579987A1 (en) | Polymer dispersions, processes for the preparation thereof and the use thereof | |
| KR20150033008A (en) | Acrylic Emulsion Adhesive and Method for Preparing the Same | |
| CN110699019A (en) | High-temperature-resistant acrylate pressure-sensitive adhesive and double-sided adhesive without base material | |
| JPS6256168B2 (en) | ||
| WO2012176544A1 (en) | Water-based adhesive agent composition and method for producing same | |
| CN102167773A (en) | Acrylic acid emulsion and functional acrylic acid emulsion for unshadowed protective film | |
| KR102470448B1 (en) | Aqueous acrylic adhesive for clothes and method for preparing the same | |
| KR101614341B1 (en) | Acrylic Emulsion Resin with Excellent Adhesive and Preparation Method Thereof | |
| KR102600008B1 (en) | Aqueous acrylic adhesive for pet film and method for preparing the same | |
| CN107779138A (en) | A kind of modified propyl benzene emulsion water-base cement and preparation method thereof | |
| JP3142865B2 (en) | Manufacturing method of strong adhesive emulsion type pressure sensitive adhesive | |
| CN110655884A (en) | Nano-material modified acrylate pressure-sensitive adhesive and preparation method thereof | |
| KR102267592B1 (en) | Preparation method of aqueous adhesive composition for clothes | |
| JPS6123614A (en) | High-concentration tackifier composition and its production | |
| CN110746903B (en) | Water-based acrylate pressure-sensitive adhesive for automobile protective film and preparation method thereof | |
| CN111909624B (en) | Emulsion type insect attracting plate adhesive for PET (polyethylene terephthalate) base material and preparation method thereof | |
| KR102642297B1 (en) | Preparation method of aqueous adhesive composition and aqueous adhesive composition prepared using the same | |
| CN106590475A (en) | Novel acrylic ester glue and preparation method thereof | |
| JPS5822492B2 (en) | pressure sensitive adhesive | |
| CN114656905A (en) | Water-based pressure-sensitive adhesive and preparation method thereof | |
| KR20210148722A (en) | Acrylic emulsion pressure snsitive adhesive composition | |
| JP4362148B2 (en) | Method for producing water-dispersible acrylic pressure-sensitive adhesive |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200107 |
|
| RJ01 | Rejection of invention patent application after publication |