CN112143419A - Preparation method of waterproof acrylic pressure-sensitive adhesive - Google Patents
Preparation method of waterproof acrylic pressure-sensitive adhesive Download PDFInfo
- Publication number
- CN112143419A CN112143419A CN202010905345.7A CN202010905345A CN112143419A CN 112143419 A CN112143419 A CN 112143419A CN 202010905345 A CN202010905345 A CN 202010905345A CN 112143419 A CN112143419 A CN 112143419A
- Authority
- CN
- China
- Prior art keywords
- parts
- sensitive adhesive
- emulsion
- acrylic pressure
- preparation
- 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
- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 38
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 42
- 239000000839 emulsion Substances 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 150000001336 alkenes Chemical class 0.000 claims abstract description 17
- 239000003999 initiator Substances 0.000 claims abstract description 17
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 6
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 6
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical group [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 16
- 235000010265 sodium sulphite Nutrition 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 230000002087 whitening effect Effects 0.000 abstract description 4
- 230000036632 reaction speed Effects 0.000 abstract description 3
- 238000001879 gelation Methods 0.000 abstract description 2
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical group [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001289 polyvinyl ether Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
-
- 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
- C08F220/1802—C2-(meth)acrylate, e.g. ethyl (meth)acrylate
-
- 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
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- 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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention provides a preparation method of a waterproof acrylic pressure-sensitive adhesive, which comprises the following steps: weighing ethyl acrylate, butyl acrylate, methyl methacrylate, acrylamide, acrylic acid and methacrylic acid, and uniformly mixing the raw materials in a reactor for later use; weighing olefin oxysulfonate and deionized water, adding the olefin oxysulfonate and the deionized water into a reactor, stirring, dropwise adding the mixed solution at a constant speed, and continuously stirring after dropwise adding is finished to obtain a pre-emulsion for later use; putting part of the pre-emulsion into a reaction kettle, adding olefin oxysulfonate, glycidyl methacrylate and deionized water, stirring, adding part of initiator when the temperature is raised to 50-60 ℃, and when the emulsion is blue; continuously heating to 60-70 ℃, preserving heat for 20-40min, then respectively dripping the rest pre-emulsion and the initiator, adjusting the pH value to 7-8, preserving heat for 1h, cooling to room temperature, filtering and discharging. The invention controls the reaction speed, reduces the phenomena of gelation and the like, and improves the water whitening resistance of the acrylic pressure-sensitive adhesive.
Description
Technical Field
The invention relates to the technical field of pressure-sensitive adhesives, in particular to a preparation method of a waterproof acrylic pressure-sensitive adhesive.
Background
Pressure-sensitive adhesives are pressure-sensitive adhesives which are adhesives that can be firmly bonded to an adherend by applying light finger pressure without the aid of solvents, heat or other means. It features easy adhesion, easy peeling, no damage, and no drying and solidification of adhesive layer in long time, so it is also called as pressure-sensitive adhesive. The pressure-sensitive adhesive can be divided into rubber pressure-sensitive adhesive, thermoplastic elastomer pressure-sensitive adhesive, polyacrylate pressure-sensitive adhesive, polyvinyl ether pressure-sensitive adhesive, organic silicon pressure-sensitive adhesive and the like from chemical components, wherein the acrylic acid pressure-sensitive adhesive has the excellent performances of toxic safety, environmental protection, excellent color retention, light resistance and weather resistance, difficult oxidation, insensitivity to ultraviolet degradation, high bonding strength, high shear strength and the like.
The acrylic pressure-sensitive adhesive generally has the defects of relatively poor water resistance, cold resistance, heat resistance, weather resistance and stability, and the development of a preparation method of the water-resistant acrylic pressure-sensitive adhesive is very meaningful.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of the waterproof acrylic pressure-sensitive adhesive, which controls the reaction speed, reduces the phenomena of gelation and the like, and improves the water-whitening resistance of the acrylic pressure-sensitive adhesive by adopting the application of a reactive emulsifier, the modification of a cross-linking agent and the adjustment of the pH value.
The technical scheme of the invention is realized as follows:
a preparation method of a waterproof acrylic pressure-sensitive adhesive comprises the following steps:
(1) weighing 120 parts of 100-120 parts of ethyl acrylate, 80-120 parts of butyl acrylate, 60-90 parts of methyl methacrylate, 80-90 parts of acrylamide, 50-60 parts of acrylic acid and 40-60 parts of methacrylic acid according to parts by weight, and uniformly mixing the raw materials in a reactor for later use;
(2) weighing 5-10 parts of olefin oxysulfonate according to parts by weight, adding into a reactor, adding 50-60 parts of deionized water, starting stirring at a stirring speed of 200-;
(3) dropwise adding the mixed solution obtained in the step (1) at a constant speed within 20-30min of stirring in the step (2), and after dropwise adding, continuously stirring for 10-20min to obtain a pre-emulsion for later use;
(4) firstly, putting part of the pre-emulsion prepared in the step (2) into a reaction kettle, then adding 5-10 parts of olefin oxysulfonate, 2-3 parts of glycidyl methacrylate and 20-30 parts of deionized water, and starting stirring at the stirring speed of 250-270 r/min;
(5) heating to 50-60 ℃, adding 3-5 parts of initiator, and when the emulsion is blue; continuously heating to about 60-70 deg.C, and keeping the temperature for 20-40 min;
(6) then respectively dripping 3-5 parts of the rest pre-emulsion and the initiator, finishing dripping the rest pre-emulsion within 3h, and finishing dripping the initiator within 4 h;
(7) adding ammonia water to adjust the pH value to 7-8, keeping the temperature for 1h after the dropwise addition, cooling to room temperature, filtering and discharging to obtain a finished product.
Preferably, the stirring speed in the step (2) is 250r/min, and the stirring time is 25 min.
Preferably, the stirring speed in the step (4) is 260 r/min.
Preferably, part of the initiator is added when the temperature of the step (5) is raised to 55 ℃.
Preferably, when the emulsion in step (5) appears blue; continuously heating to about 65 ℃, and keeping the temperature for 30 min.
Preferably, the initiator is an oxidant a-a reductant B.
Preferably, the oxidizing agent a is hydrogen peroxide.
Preferably, the reducing agent B is sodium sulfite.
Preferably, in the step (4), the 1/4 pre-emulsion prepared in the step (2) is firstly put into a reaction kettle.
Preferably, the initiator is added when the temperature is raised to 55 ℃ in the step (5).
The invention has the following beneficial effects: the preparation method of the waterproof acrylic pressure-sensitive adhesive is simple to operate, the temperature in the reaction process is low, the reaction speed is controlled, the gel phenomenon is reduced, and the raw materials are fully and uniformly emulsified and crosslinked; meanwhile, an oxidant-reducing agent is used as an initiating system, olefin oxysulfonate is used for reducing the migration of an emulsifier during the drying of the emulsion, the existence of water-soluble electrolyte in the emulsion is reduced or eliminated, and the water whitening resistance of the emulsion can be improved.
Detailed Description
For a more clear understanding of the technical features, objects and advantages of the present invention, reference is now made to the following detailed description of the embodiments of the present invention taken in conjunction with the accompanying drawings, which are included to illustrate and not to limit the scope of the present invention.
Example 1
A preparation method of a waterproof acrylic pressure-sensitive adhesive comprises the following steps:
(1) weighing 100 parts of ethyl acrylate, 120 parts of butyl acrylate, 60 parts of methyl methacrylate, 90 parts of acrylamide, 50 parts of acrylic acid and 60 parts of methacrylic acid according to parts by weight, and putting the raw materials into a reactor to be uniformly mixed for later use;
(2) weighing 5 parts of olefin oxysulfonate according to parts by weight, adding the olefin oxysulfonate into a reactor, adding 60 parts of deionized water, starting a stirring function, wherein the stirring speed is 200r/min, and the stirring time is 20 min;
(3) dropwise adding the mixed solution obtained in the step (1) at a constant speed within 20min of stirring in the step (2), and after dropwise adding, continuously stirring for 10min to obtain a pre-emulsion for later use;
(4) firstly, placing the 1/4 pre-emulsion prepared in the step (2) into a reaction kettle, adding 5 parts of olefin oxysulfonate, 3 parts of glycidyl methacrylate and 20 parts of deionized water, and starting stirring at the stirring speed of 250 r/min;
(5) heating to 50 ℃, adding 1 part of hydrogen peroxide and 2 parts of sodium sulfite when the emulsion is blue; continuously heating to about 60 ℃, and keeping the temperature for 20 min;
(6) then, respectively dripping the residual pre-emulsion, 1 part of hydrogen peroxide and 2 parts of sodium sulfite, finishing dripping the residual pre-emulsion within 3 hours, and finishing dripping the initiator within 4 hours;
(7) adding ammonia water to adjust the pH value to 7, keeping the temperature for 1h after the dropwise addition, cooling to room temperature, filtering and discharging to obtain a finished product.
Example 2
A preparation method of a waterproof acrylic pressure-sensitive adhesive comprises the following steps:
(1) weighing 120 parts of ethyl acrylate, 80 parts of butyl acrylate, 90 parts of methyl methacrylate, 80 parts of acrylamide, 60 parts of acrylic acid and 40 parts of methacrylic acid according to parts by weight, and putting the raw materials into a reactor to be uniformly mixed for later use;
(2) weighing 10 parts of alkene oxysulfonate according to parts by weight, adding the alkene oxysulfonate into a reactor, adding 50 parts of deionized water, and starting a stirring function, wherein the stirring speed is 300r/min, and the stirring time is 30 min;
(3) dropwise adding the mixed solution obtained in the step (1) at a constant speed within 30min of stirring in the step (2), and after dropwise adding, continuously stirring for 20min to obtain a pre-emulsion for later use;
(4) firstly, placing the 1/4 pre-emulsion prepared in the step (2) into a reaction kettle, adding 10 parts of olefin oxysulfonate, 2 parts of glycidyl methacrylate and 30 parts of deionized water, and starting stirring at a stirring speed of 270 r/min;
(5) heating to 60 ℃, adding 1 part of hydrogen peroxide and 2 parts of sodium sulfite when the emulsion is blue; continuously heating to about 70 ℃, and keeping the temperature for 40 min;
(6) then, respectively dripping the residual pre-emulsion, 1 part of hydrogen peroxide and 2 parts of sodium sulfite, finishing dripping the residual pre-emulsion within 3 hours, and finishing dripping the initiator within 4 hours;
(7) adding ammonia water to adjust the pH value to 8, preserving the temperature for 1h after the dropwise addition, cooling to room temperature, filtering and discharging to obtain a finished product.
Example 3
A preparation method of a waterproof acrylic pressure-sensitive adhesive comprises the following steps:
(1) weighing 110 parts of ethyl acrylate, 100 parts of butyl acrylate, 80 parts of methyl methacrylate, 85 parts of acrylamide, 55 parts of acrylic acid and 50 parts of methacrylic acid according to parts by weight, and putting the raw materials into a reactor to be uniformly mixed for later use;
(2) weighing 8 parts of olefin oxysulfonate according to parts by weight, adding the olefin oxysulfonate into a reactor, adding 55 parts of deionized water, and starting a stirring function, wherein the stirring speed is 250r/min, and the stirring time is 25 min;
(3) dropwise adding the mixed solution obtained in the step (1) at a constant speed within 25min of stirring in the step (2), and after dropwise adding, continuously stirring for 15min to obtain a pre-emulsion for later use;
(4) firstly, placing the 1/4 pre-emulsion prepared in the step (2) into a reaction kettle, adding 8 parts of olefin oxysulfonate, 2.5 parts of glycidyl methacrylate and 25 parts of deionized water, and starting stirring at the stirring speed of 260 r/min;
(5) heating to 55 ℃, adding 1 part of hydrogen peroxide and 2 parts of sodium sulfite when the emulsion is blue; continuously heating to about 65 ℃, and keeping the temperature for 30 min;
(6) then, respectively dripping the residual pre-emulsion, 1 part of hydrogen peroxide and 2 parts of sodium sulfite, finishing dripping the residual pre-emulsion within 3 hours, and finishing dripping the initiator within 4 hours;
(7) adding ammonia water to adjust the pH value to 8, preserving the temperature for 1h after the dropwise addition, cooling to room temperature, filtering and discharging to obtain a finished product.
First, performance test
The initial adhesion of the waterproof acrylic pressure-sensitive adhesive is determined as follows: measured according to GB 4852-1984; and (3) measuring the permanent viscosity: measured according to GB 4851-1998; 180 ° peel strength determination: measured according to GB 4851-1998: water-resistant method at 90 ℃: the prepared waterproof acrylic pressure-sensitive adhesive tape was placed in hot water at 90 ℃ with the adhesive side down, and the time from the beginning of soaking in water to the whitening of the tape was measured. Measurement of particle size: particle size distribution was measured by analyzing the particle size distribution using a Friedel (Shanghai) instruments and Equipment Co., Ltd, model M1. The results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the water-resistant acrylic pressure-sensitive adhesives prepared in examples 1-3 of the present invention have good water whitening resistance and good overall properties.
The above embodiments are merely provided to help understand the method and core principle of the present invention, and the main steps and embodiments of the present invention are described in detail by using specific examples. To those skilled in the art, the various conditions and parameters may be varied as desired in a particular implementation in accordance with the principles of the invention, and in view of the foregoing, the description is not to be taken as limiting the invention.
Claims (10)
1. A preparation method of a waterproof acrylic pressure-sensitive adhesive is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing 120 parts of 100-120 parts of ethyl acrylate, 80-120 parts of butyl acrylate, 60-90 parts of methyl methacrylate, 80-90 parts of acrylamide, 50-60 parts of acrylic acid and 40-60 parts of methacrylic acid according to parts by weight, and uniformly mixing the raw materials in a reactor for later use;
(2) weighing 5-10 parts of olefin oxysulfonate according to parts by weight, adding into a reactor, adding 50-60 parts of deionized water, starting stirring at a stirring speed of 200-;
(3) dropwise adding the mixed solution obtained in the step (1) at a constant speed within 20-30min of stirring in the step (2), and after dropwise adding, continuously stirring for 10-20min to obtain a pre-emulsion for later use;
(4) firstly, putting part of the pre-emulsion prepared in the step (2) into a reaction kettle, then adding 5-10 parts of olefin oxysulfonate, 2-3 parts of glycidyl methacrylate and 20-30 parts of deionized water, and starting stirring at the stirring speed of 250-270 r/min;
(5) heating to 50-60 ℃, adding 3-5 parts of initiator, and when the emulsion is blue; continuously heating to about 60-70 deg.C, and keeping the temperature for 20-40 min;
(6) then respectively dripping 3-5 parts of the rest pre-emulsion and the initiator, finishing dripping the rest pre-emulsion within 3h, and finishing dripping the initiator within 4 h;
(7) adding ammonia water to adjust the pH value to 7-8, keeping the temperature for 1h after the dropwise addition, cooling to room temperature, filtering and discharging to obtain a finished product.
2. The preparation method of the water-resistant acrylic pressure-sensitive adhesive according to claim 1, characterized in that: in the step (2), the stirring speed is 250r/min, and the stirring time is 25 min.
3. The preparation method of the water-resistant acrylic pressure-sensitive adhesive according to claim 1, characterized in that: the stirring speed in the step (4) is 260 r/min.
4. The preparation method of the water-resistant acrylic pressure-sensitive adhesive according to claim 1, characterized in that: and (5) adding part of initiator when the temperature is raised to 55 ℃ in the step of heating.
5. The preparation method of the water-resistant acrylic pressure-sensitive adhesive according to claim 1, characterized in that: when the emulsion is blue in the step (5); continuously heating to about 65 ℃, and keeping the temperature for 30 min.
6. The preparation method of the water-resistant acrylic pressure-sensitive adhesive according to claim 1, characterized in that: the initiator is an oxidant A-a reducing agent B.
7. The preparation method of the water-resistant acrylic pressure-sensitive adhesive according to claim 6, characterized in that: the oxidant A is hydrogen peroxide.
8. The preparation method of the water-resistant acrylic pressure-sensitive adhesive according to claim 6, characterized in that: the reducing agent B is sodium sulfite.
9. The preparation method of the water-resistant acrylic pressure-sensitive adhesive according to claim 1, characterized in that: in the step (4), the 1/4 pre-emulsion prepared in the step (2) is firstly put into a reaction kettle.
10. The preparation method of the water-resistant acrylic pressure-sensitive adhesive according to claim 1, characterized in that: and (3) adding an initiator when the temperature is raised to 55 ℃ in the step (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010905345.7A CN112143419A (en) | 2020-09-01 | 2020-09-01 | Preparation method of waterproof acrylic pressure-sensitive adhesive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010905345.7A CN112143419A (en) | 2020-09-01 | 2020-09-01 | Preparation method of waterproof acrylic pressure-sensitive adhesive |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112143419A true CN112143419A (en) | 2020-12-29 |
Family
ID=73890475
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010905345.7A Pending CN112143419A (en) | 2020-09-01 | 2020-09-01 | Preparation method of waterproof acrylic pressure-sensitive adhesive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112143419A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115287015A (en) * | 2022-08-26 | 2022-11-04 | 苏州泰仑电子材料有限公司 | Pressure-sensitive adhesive protective film and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104449485A (en) * | 2014-11-13 | 2015-03-25 | 苏州斯迪克新材料科技股份有限公司 | Preparation method of emulsion type polyacrylate pressure-sensitive adhesive for reflecting film |
| CN106010380A (en) * | 2015-11-16 | 2016-10-12 | 江苏景宏新材料科技有限公司 | Method for preparation of water blush resistant acrylic emulsion pressure sensitive adhesive by pickering emulsion polymerization |
| JP2018111754A (en) * | 2017-01-10 | 2018-07-19 | 日東電工株式会社 | Adhesive sheet |
| CN110982008A (en) * | 2019-12-30 | 2020-04-10 | 宣城研一新能源科技有限公司 | Aqueous binder for negative electrode of lithium ion battery |
| CN111057184A (en) * | 2019-12-30 | 2020-04-24 | 宣城研一新能源科技有限公司 | Preparation method of aqueous binder for negative pole piece |
| CN111363492A (en) * | 2020-05-09 | 2020-07-03 | 永大（中山）有限公司 | Water purifier filter element adhesive tape and preparation method thereof |
-
2020
- 2020-09-01 CN CN202010905345.7A patent/CN112143419A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104449485A (en) * | 2014-11-13 | 2015-03-25 | 苏州斯迪克新材料科技股份有限公司 | Preparation method of emulsion type polyacrylate pressure-sensitive adhesive for reflecting film |
| CN106010380A (en) * | 2015-11-16 | 2016-10-12 | 江苏景宏新材料科技有限公司 | Method for preparation of water blush resistant acrylic emulsion pressure sensitive adhesive by pickering emulsion polymerization |
| JP2018111754A (en) * | 2017-01-10 | 2018-07-19 | 日東電工株式会社 | Adhesive sheet |
| CN110982008A (en) * | 2019-12-30 | 2020-04-10 | 宣城研一新能源科技有限公司 | Aqueous binder for negative electrode of lithium ion battery |
| CN111057184A (en) * | 2019-12-30 | 2020-04-24 | 宣城研一新能源科技有限公司 | Preparation method of aqueous binder for negative pole piece |
| CN111363492A (en) * | 2020-05-09 | 2020-07-03 | 永大（中山）有限公司 | Water purifier filter element adhesive tape and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115287015A (en) * | 2022-08-26 | 2022-11-04 | 苏州泰仑电子材料有限公司 | Pressure-sensitive adhesive protective film and preparation method thereof |
| CN115287015B (en) * | 2022-08-26 | 2024-03-22 | 苏州泰仑电子材料有限公司 | Pressure-sensitive adhesive protective film and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107602760B (en) | Polyacrylate emulsion pressure-sensitive adhesive for electronic protective film, and preparation method and application thereof | |
| CN102533177B (en) | High water resistance emulsion polyacrylate pressure-sensitive adhesive and preparation method and application thereof | |
| CN107573469A (en) | A kind of preparation method of the Acrylate pressure-sensitive adhesive emulsion of block structure | |
| CN111518482B (en) | High-performance acrylic acid foaming body adhesive tape and preparation method thereof | |
| CN102516904A (en) | Single-component water-based adhesive for evaporative cooling wet curtain and preparation method thereof | |
| JP2019508545A (en) | UV crosslinkable hot melt pressure sensitive adhesive used for polyvinyl chloride insulating adhesive tape | |
| CN112250789A (en) | Emulsion type acrylate pressure-sensitive adhesive, preparation method thereof and double-sided adhesive tape | |
| CN103524667A (en) | Water-based pressure-sensitive adhesive for polyethylene protection film and polyethylene protection film and preparation method thereof | |
| CN102703003A (en) | Silane coupling agent modified resin easy-peel environment friendly water-based pressure-sensitive adhesive | |
| CN112409961A (en) | High-peeling-force acrylate pressure-sensitive adhesive and preparation method thereof | |
| CN112143419A (en) | Preparation method of waterproof acrylic pressure-sensitive adhesive | |
| CN113913134B (en) | Adhesive for battery cell protective film, protective film prepared from adhesive and application of protective film | |
| CN114835841B (en) | Aqueous emulsion, preparation method thereof and temperature-change-resistant construction real stone paint prepared by adopting aqueous emulsion | |
| CN106749875A (en) | A kind of self-crosslinking aqueous acrylic emulsion of low ammonia and preparation method thereof | |
| CN106479407A (en) | A kind of paper-plastic stick adhesive and preparation method thereof | |
| CN111269350A (en) | Environment-friendly water-based plastic-plastic composite adhesive and preparation method thereof | |
| CN108251047A (en) | A kind of preparation method of compound type starch adhesive | |
| CN109021886A (en) | A kind of heat insulation broken bridge aluminum profile protective film water-borne pressure sensitive adhesive and preparation method thereof | |
| CN112851882A (en) | Preparation method of epoxy resin modified styrene-acrylic emulsion for plastic ink | |
| CN102101996A (en) | Pressure-sensitive adhesive used for cotton paper or non-woven fabrics and preparation method thereof | |
| CN111909624B (en) | Emulsion type insect attracting plate adhesive for PET (polyethylene terephthalate) base material and preparation method thereof | |
| CN102634303A (en) | Hexahydroxy copolymer water-based pressure-sensitive adhesive without adhesive residue and preparation method of hexahydroxy copolymer water-based pressure-sensitive adhesive | |
| CN113388064A (en) | Water-based acrylic emulsion for battery protective film and preparation method thereof | |
| CN112080231A (en) | High-temperature-resistant acrylic pressure-sensitive adhesive and preparation method thereof | |
| CN102504128B (en) | Preparation method for organic silicon-modified printing 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 | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20220112 Address after: No.78, Fusheng Road, tiantoujiao village, Qiaotou town, Dongguan City, Guangdong Province, 523000 Applicant after: DONGGUAN FUYIN ADHESIVE TECHNOLOGY Co.,Ltd. Address before: 232100 No.400, Jidian team, Hougang village, yuezhangji Town, Fengtai County, Huainan City, Anhui Province Applicant before: Yue Gang |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201229 |