CN114316860B - Preparation method of pressure-sensitive adhesive with gradient structure and high peel strength and water resistance - Google Patents
Preparation method of pressure-sensitive adhesive with gradient structure and high peel strength and water resistance Download PDFInfo
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Abstract
The invention relates to the field of bonding materials, and provides a preparation method of a pressure-sensitive adhesive with a gradient structure and high peel strength and high water resistance, wherein in the preparation method, an emulsifier aqueous solution, butyl acrylate, a functional monomer and styrene are mixed to obtain a first-stage pre-emulsion, and the rest emulsifier aqueous solution, the rest functional monomer, an acrylic ester soft monomer, a molecular weight regulator and a silane coupling agent are mixed to obtain a second-stage pre-emulsion; mixing deionized water, an emulsifying agent and a pH buffering agent, heating, adding an initiator and a first-stage pre-emulsion to obtain seed liquid, dropwise adding the first-stage pre-emulsion and an initiator aqueous solution into the seed liquid while dropwise adding the second-stage pre-emulsion into the first-stage pre-emulsion, and preserving heat after dropwise adding; finally cooling, and regulating the pH of the emulsion to 7.5-8.5. Through the technical scheme, the problems of low peel strength and poor water resistance of the aqueous pressure-sensitive adhesive emulsion on the basis of high initial adhesion in the pressure-sensitive adhesive industry are solved.
Description
Technical Field
The invention relates to the field of bonding materials, in particular to a preparation method of a pressure-sensitive adhesive with a gradient structure, high peel strength and high water resistance.
Background
Pressure sensitive adhesives are a class of adhesives that have sensitivity to pressure. The most popular pressure-sensitive adhesive in the market at present is aqueous acrylic acid ester pressure-sensitive adhesive emulsion, and the aqueous acrylic acid ester pressure-sensitive adhesive emulsion has the advantages of environmental protection, safe and simple production operation and the like, so that the aqueous acrylic acid ester pressure-sensitive adhesive emulsion is widely applied to products such as adhesive tapes, labels and the like, particularly the application of some label adhesives, such as the pasting of labels on trucks, open-air signboards or bottles. However, the existing water-based acrylic pressure-sensitive adhesive emulsion on the market has the defects of low peel strength and deviation of water resistance, and limits the development and application fields of the water-based acrylic pressure-sensitive adhesive emulsion. In the pressure-sensitive adhesive industry, in order to achieve the performance of high initial adhesion and high peel strength, the performance of high peel strength is usually achieved by adopting a cold splicing mode of compounding two or more pressure-sensitive adhesive emulsions or splicing tackifying resin and the like, but the method has unstable product performance and water resistance deviation due to poor compatibility.
Disclosure of Invention
The invention provides a preparation method of a pressure-sensitive adhesive with a gradient structure and high peel strength and high water resistance, which solves the problems of low peel strength and poor water resistance of aqueous pressure-sensitive adhesive emulsion on the basis of high initial adhesion in the pressure-sensitive adhesive industry.
The technical scheme of the invention is realized as follows:
a preparation method of a pressure-sensitive adhesive with a gradient structure and high peel strength and water resistance comprises the following steps:
s1, adding 4-5 parts by weight of an emulsifier into 100-200 parts by weight of water to obtain a first emulsifier aqueous solution, and then adding 200-280 parts by weight of butyl acrylate, 20-130 parts by weight of styrene and 2.5-10 parts by weight of a functional monomer into the first emulsifier aqueous solution to obtain a stable first-stage pre-emulsion;
s2, adding 4-10 parts by weight of an emulsifier into 100-200 parts by weight of water to obtain a second emulsifier aqueous solution, and then adding 200-270 parts by weight of an acrylic ester soft monomer, 2.5-12 parts by weight of a functional monomer, 0.1-1 part by weight of a molecular weight regulator and 0.1-5 parts by weight of a silane coupling agent into the second emulsifier aqueous solution to obtain a stable secondary pre-emulsion;
s3, mixing 150-200 parts by weight of water, 1-2 parts by weight of an emulsifying agent and 0.5-2 parts by weight of a pH buffering agent, heating to 80-85 ℃, adding 0.3-3.25 parts by weight of an initiator and 30-40 parts by weight of the primary pre-emulsion in the step S1, and reacting after the addition is finished to obtain seed liquid;
s4, adding 1-2 parts by weight of initiator into 30-40 parts by weight of water to obtain an initiator aqueous solution;
s5, dropwise adding a second-level pre-emulsion into the first-level pre-emulsion left in the step S1 to obtain a mixed solution;
s6, dropwise adding the aqueous solution of the initiator in the step S4 and the mixed solution in the step S5 into the seed solution in the step S3 at the same time, and preserving heat at 80-85 ℃ after the dropwise adding is finished;
s7, cooling after heat preservation is finished, and regulating the pH value of the prepared emulsion to 7.5-8.5 to obtain the acrylic emulsion pressure-sensitive adhesive product.
As a further technical scheme, the mass ratio of the butyl acrylate to the styrene in the step S1 is 1:1-10:1.
As a further technical scheme, the functional monomer in the steps S1 and S2 is at least one or a combination of more than one of acrylic acid, methacrylic acid and hydroxyethyl acrylate.
As a further technical scheme, the molecular weight regulator in the step S2 is at least one or a combination of more of n-dodecyl mercaptan, tert-dodecyl mercaptan and octyl mercaptan.
As a further technical scheme, the emulsifying agent in the steps S1, S2 and S3 is one or two of 2A1 and SR-10.
As a further technical scheme, the acrylic ester soft monomer in the step S2 is one or two of butyl acrylate and octyl acrylate.
As a further technical scheme, the reaction time in the step S3 is 5-15min, and the pH buffer is ammonium bicarbonate, sodium bicarbonate or sodium dihydrogen phosphate.
As a further technical scheme, the initiator in the steps S3 and S4 is ammonium persulfate, sodium persulfate or potassium persulfate.
As a further technical scheme, in the step S6, the initiator aqueous solution of the step S4 and the mixed solution of the step S5 are dropwise added to the seed solution of the step S3 at the same time of the step S5, the dropwise adding time is 3.5-4h, and the heat preservation time is 45-90min after the dropwise adding is finished.
As a further technical scheme, the temperature is reduced to 40-55 ℃ after the heat preservation in the step S7 is finished.
The working principle and the beneficial effects of the invention are as follows:
the invention provides a preparation method of a pressure-sensitive adhesive with a gradient structure and high peel strength and high water resistance, wherein the preparation method utilizes an acrylic ester soft monomer to solve the defect of low primary adhesion of the pressure-sensitive adhesive, adopts a power-level semi-continuous dropping method, and drops a secondary pre-emulsion into a primary pre-emulsion drop and simultaneously drops a primary pre-emulsion into a seed solution to prepare a pressure-sensitive adhesive emulsion with a core-shell structure. The pressure-sensitive adhesive particle core layer is composed of styrene and butyl acrylate, and the cohesive force is controlled on the premise of not influencing the viscoelastic state of the surface layer of the latex particle due to the gradient architecture of the styrene; the glass transition temperature of the shell monomer is gradually changed from inside to outside: namely, the butyl acrylate and the octyl acrylate of the shell layer are increased in a gradient manner from inside to outside, so that the primary bonding strength is increased, and the styrene of the shell layer is decreased in a gradient manner from inside to outside, so that latex particles can be fused with each other better to form a film, and the pressure-sensitive adhesive emulsion has high primary bonding performance and high peel strength at the same time; meanwhile, the silane coupling agent of the shell layer is increased from inside to outside in a gradient manner, so that the water resistance of the pressure-sensitive adhesive emulsion is obviously improved, and the beneficial effects of high initial adhesion, high peel strength and high water resistance are achieved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
S1, adding 4.5 g of a 2A1 emulsifier into 100 g of deionized water to obtain a first emulsifier aqueous solution, adding 240 g of butyl acrylate, 30 g of styrene, 2.5 g of acrylic acid and 4 g of hydroxyethyl acrylate into the first emulsifier aqueous solution, and stirring and dispersing for 15min to obtain a stable first-stage pre-emulsion;
s2, adding 4.5 g of 2A1 emulsifier into 100 g of deionized water to obtain a second emulsifier aqueous solution, slowly adding 200 g of butyl acrylate, 70 g of octyl acrylate, 2.5 g of acrylic acid, 4 g of hydroxyethyl acrylate, 0.3 g of n-dodecyl mercaptan and 1 g of KH151 silane coupling agent into the second emulsifier aqueous solution, and stirring and dispersing for 15min to obtain a stable secondary pre-emulsion;
s3, adding 180 g of deionized water into a reaction kettle, heating to 82 ℃, and then adding 1 g of 2A1 emulsifier, 1 g of ammonium bicarbonate, 1.8 g of ammonium persulfate and 37 g of primary pre-emulsion of the step S1 into the reaction kettle to react for 15min to obtain seed liquid;
s4, adding 1 gram of ammonium persulfate into 35 grams of water to obtain an ammonium persulfate aqueous solution;
s5, dripping the second-level pre-emulsion into the first-level pre-emulsion left in the step S1 at a constant speed to obtain a mixed solution;
s6, dropwise adding the ammonium persulfate aqueous solution of the step S4 and the mixed solution of the step S5 into the seed solution of the step S3 at a constant speed while maintaining the temperature of the reaction kettle at 85+/-2 ℃, wherein the step S5 and the step S6 are dropwise added simultaneously and 210min simultaneously, and the temperature is kept at 85 ℃ for 60min after the completion of dropwise addition;
and S7, cooling to 43 ℃ after heat preservation is finished, adding ammonia water into the prepared emulsion to adjust the pH value to 8.5, obtaining an acrylic emulsion pressure-sensitive adhesive product, and filtering and packaging by a 180-mesh filter screen for use.
Example 2
S1, adding 4.5 g of a 2A1 emulsifier into 100 g of deionized water to obtain a first emulsifier aqueous solution, adding 230 g of butyl acrylate, 40 g of styrene, 2.5 g of acrylic acid and 4 g of hydroxyethyl acrylate into the first emulsifier aqueous solution, and stirring and dispersing for 15min to obtain a stable first-stage pre-emulsion;
s2, adding 4.5 g of a 2A1 emulsifier into 100 g of deionized water to obtain a second emulsifier aqueous solution, adding 200 g of butyl acrylate, 70 g of octyl acrylate, 2.5 g of acrylic acid, 4 g of hydroxyethyl acrylate, 0.3 g of n-dodecyl mercaptan and 1 g of KH151 silane coupling agent into the second emulsifier aqueous solution, and stirring and dispersing for 15min to obtain a stable secondary pre-emulsion;
s3, adding 180 g of deionized water into a reaction kettle, heating to 82 ℃, and then adding 1 g of 2A1 emulsifier, 1 g of ammonium bicarbonate, 1.8 g of ammonium persulfate and 37 g of primary pre-emulsion of the step S1 into the reaction kettle to react for 15min to obtain seed liquid;
s4, adding 1 gram of ammonium persulfate into 35 grams of water to obtain an ammonium persulfate aqueous solution;
s5, dripping the second-level pre-emulsion into the first-level pre-emulsion left in the step S1 at a constant speed to obtain a mixed solution;
s6, dropwise adding the ammonium persulfate aqueous solution of the step S4 and the mixed solution of the step S5 into the seed solution of the step S3 at a constant speed while maintaining the temperature of the reaction kettle at 85+/-2 ℃, wherein the step S5 and the step S6 are dropwise added simultaneously and 210min simultaneously, and the temperature is kept at 85 ℃ for 60min after the completion of dropwise addition;
and S7, cooling to 43 ℃ after heat preservation is finished, adding ammonia water into the prepared emulsion to adjust the pH value to 8.5, obtaining an acrylic emulsion pressure-sensitive adhesive product, and filtering and packaging by a 180-mesh filter screen for use.
Example 3
S1, adding 4.5 g of a 2A1 emulsifier into 100 g of deionized water to obtain a first emulsifier aqueous solution, adding 220 g of butyl acrylate, 50 g of styrene, 2.5 g of acrylic acid and 4 g of hydroxyethyl acrylate into the first emulsifier aqueous solution, and stirring and dispersing for 15min to obtain a stable first-stage pre-emulsion;
s2, adding 4.5 g of a 2A1 emulsifier into 100 g of deionized water to obtain a second emulsifier aqueous solution, adding 200 g of butyl acrylate, 70 g of octyl acrylate, 2.5 g of acrylic acid, 4 g of hydroxyethyl acrylate, 0.3 g of n-dodecyl mercaptan and 1 g of KH151 silane coupling agent into the second emulsifier aqueous solution, and stirring and dispersing for 15min to obtain a stable secondary pre-emulsion;
s3, adding 180 g of deionized water into a reaction kettle, heating to 82 ℃, and then adding 1 g of 2A1 emulsifier, 1 g of ammonium bicarbonate, 1.8 g of ammonium persulfate and 37 g of primary pre-emulsion of the step S1 into the reaction kettle to react for 15min to obtain seed liquid;
s4, adding 1 gram of ammonium persulfate into 35 grams of water to obtain an ammonium persulfate aqueous solution;
s5, dripping the second-level pre-emulsion into the first-level pre-emulsion left in the step S1 at a constant speed to obtain a mixed solution;
s6, dropwise adding the ammonium persulfate aqueous solution of the step S4 and the mixed solution of the step S5 into the seed solution of the step S3 at a constant speed while maintaining the temperature of the reaction kettle at 85+/-2 ℃, wherein the step S5 and the step S6 are dropwise added simultaneously and 210min simultaneously, and the temperature is kept at 85 ℃ for 60min after the completion of dropwise addition;
and S7, cooling to 43 ℃ after heat preservation is finished, adding ammonia water into the prepared emulsion to adjust the pH value to 8.5, obtaining an acrylic emulsion pressure-sensitive adhesive product, and filtering and packaging by a 180-mesh filter screen for use.
Example 4
S1, adding 4.0 g of a 2A1 emulsifier into 100 g of deionized water to obtain a first emulsifier aqueous solution, adding 200 g of butyl acrylate, 20 g of styrene and 2.5 g of hydroxyethyl acrylate into the first emulsifier aqueous solution, and stirring and dispersing for 15min to obtain a stable first-stage pre-emulsion;
s2, adding 4.0 g of a 2A1 emulsifier into 100 g of deionized water to obtain a second emulsifier aqueous solution, adding 150 g of butyl acrylate, 50 g of octyl acrylate, 2.5 g of hydroxyethyl acrylate, 0.1 g of n-dodecyl mercaptan and 0.1 g of KH151 silane coupling agent into the second emulsifier aqueous solution, and stirring and dispersing for 15min to obtain a stable secondary pre-emulsion;
s3, adding 150 g of deionized water into a reaction kettle, heating to 82 ℃, and then adding 1 g of 2A1 emulsifier, 0.5 g of sodium bicarbonate, 0.3 g of sodium persulfate and 30 g of primary pre-emulsion in the step S1 into the reaction kettle to react for 5min to obtain seed liquid;
s4, adding 1 gram of sodium persulfate into 30 grams of water to obtain a sodium persulfate aqueous solution;
s5, dripping the second-level pre-emulsion into the first-level pre-emulsion left in the step S1 at a constant speed to obtain a mixed solution;
s6, under the condition that the temperature of the reaction kettle is maintained at 85+/-2 ℃, dropwise adding the sodium persulfate aqueous solution of the step S4 and the mixed solution of the step S5 into the seed solution of the step S3 at a constant speed while carrying out the step S5, dropwise adding the sodium persulfate aqueous solution and the mixed solution of the step S5 simultaneously with the step S6 for 210min, and carrying out heat preservation for 45min at 80 ℃ after the completion of dropwise adding;
and S7, cooling to 40 ℃ after heat preservation is finished, adding ammonia water into the prepared emulsion to adjust the pH value to 7.5, obtaining an acrylic emulsion pressure-sensitive adhesive product, and filtering and packaging the acrylic emulsion pressure-sensitive adhesive product by a 180-mesh filter screen.
Example 5
S1, adding 5.0 g of a 2A1 emulsifier into 200 g of deionized water to obtain a first emulsifier aqueous solution, adding 280 g of butyl acrylate, 130 g of styrene and 10 g of hydroxyethyl acrylate into the first emulsifier aqueous solution, and stirring and dispersing for 15min to obtain a stable first-stage pre-emulsion;
s2, adding 10 g of 2A1 emulsifier into 200 g of deionized water to obtain a second emulsifier aqueous solution, adding 200 g of butyl acrylate, 70 g of octyl acrylate, 12 g of hydroxyethyl acrylate, 1.0 g of n-dodecyl mercaptan and 5 g of KH151 silane coupling agent into the second emulsifier aqueous solution, and stirring and dispersing for 15min to obtain a stable secondary pre-emulsion;
s3, adding 200 g of deionized water into a reaction kettle, heating to 82 ℃, and then adding 2 g of 2A1 emulsifier, 2 g of sodium dihydrogen phosphate, 3.25 g of potassium persulfate and 40 g of primary pre-emulsion in the step S1 into the reaction kettle to react for 15min to obtain seed liquid;
s4, adding 2 g of potassium persulfate into 40 g of water to obtain a potassium persulfate aqueous solution;
s5, dripping the second-level pre-emulsion into the first-level pre-emulsion left in the step S1 at a constant speed to obtain a mixed solution;
s6, under the condition that the temperature of the reaction kettle is maintained at 85+/-2 ℃, dropwise adding the potassium persulfate aqueous solution of the step S4 and the mixed solution of the step S5 into the seed solution of the step S3 at a constant speed while carrying out the step S5, dropwise adding the potassium persulfate aqueous solution and the mixed solution of the step S5 simultaneously with the step S6 for 240min, and carrying out heat preservation for 90min at 85 ℃ after finishing dropwise adding;
and S7, cooling to 55 ℃ after heat preservation is finished, adding ammonia water into the prepared emulsion to adjust the pH value to 8.5, obtaining an acrylic emulsion pressure-sensitive adhesive product, and filtering and packaging by a 180-mesh filter screen for use.
The pressure sensitive adhesives of examples 1-5 and market samples 1-2 were coated onto protective films and tested for performance as follows:
1. initial tack: testing the initial tackiness of the sample according to the test method specified in GB/T4852-2002 "pressure sensitive adhesive tape initial tackiness test method (Rolling ball method)";
2. peel strength: the peel strength of the sample is tested according to the test method specified in GB/T2792-2014 test method for peel strength of adhesive tape;
3. water resistance duration: the water resistance of the samples was tested with reference to ASTM D1003-00, test method: the prepared pressure-sensitive adhesive tape is glued with the surface facing downwards, put into deionized water, and the time from the beginning of soaking water to the whitening of the adhesive tape is measured and recorded as the water-resistant time.
The test results are shown in table 1:
table 1 examples 1-5 and market samples 1-2 were applied to protective films for initial adhesion, 180 ° peel performance, and water resistance time
| Primary adhesion | 180 degree peel strength (N/cm) | Water resistant time (h) | |
| Example 1 | 15# | 6.2 | 84 |
| Example 2 | 15# | 6.3 | 84 |
| Example 3 | 15# | 6.4 | 84 |
| Example 4 | 15# | 6.1 | 79 |
| Example 5 | 15# | 6.6 | 86 |
| Market sample 1 | 15# | 5.4 | 60 |
| Market sample 2 | 14# | 6.0 | 65 |
As can be seen from the data in Table 1, the acrylic emulsion pressure-sensitive adhesive products prepared in examples 1 to 5 of the present invention achieve the effect of high peel strength and good water resistance on the basis of high initial adhesion 15# with a peel strength of 6.6N/cm and a water resistance time of 86 hours, whereas market sample 1 has low peel strength and poor water resistance on the basis of the same initial adhesion 15# with a peel strength of only 5.4N/cm and a water resistance time of 60 hours. Market sample 2 had a peel strength of 6.0N/cm based on initial tack 14# but had poor water resistance for only 65 hours.
In conclusion, the data show that the pressure-sensitive adhesive prepared by the preparation method provided by the invention achieves higher peel strength on the basis of high initial adhesion, improves water resistance, and is obviously superior to market samples. The acrylic emulsion pressure-sensitive adhesive product provided by the invention solves the problems of unstable product performance and deviation in water resistance caused by the effect of high initial adhesion and high stripping by adopting a cold splicing mode of compounding two or more pressure-sensitive adhesive emulsions or splicing tackifying resin and the like in the preparation process of the traditional aqueous emulsion pressure-sensitive adhesive, and widens the application field of the acrylic emulsion pressure-sensitive adhesive.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (7)
1. The preparation method of the pressure-sensitive adhesive with the gradient structure and high peel strength and water resistance is characterized by comprising the following steps of:
s1, adding 4-5 parts by weight of an emulsifier into 100-200 parts by weight of water to obtain a first emulsifier aqueous solution, and then adding 200-280 parts by weight of butyl acrylate, 20-130 parts by weight of styrene and 2.5-10 parts by weight of a functional monomer into the first emulsifier aqueous solution to obtain a stable first-stage pre-emulsion;
wherein the mass ratio of the butyl acrylate to the styrene is 1:1-10:1;
s2, adding 4-10 parts by weight of an emulsifier into 100-200 parts by weight of water to obtain a second emulsifier aqueous solution, and then adding 200-270 parts by weight of an acrylic ester soft monomer, 2.5-12 parts by weight of a functional monomer, 0.1-1 part by weight of a molecular weight regulator and 0.1-5 parts by weight of a silane coupling agent into the second emulsifier aqueous solution to obtain a stable secondary pre-emulsion; the acrylic ester soft monomer is butyl acrylate and octyl acrylate;
the functional monomers in the steps S1 and S2 are at least one or a combination of more than one of acrylic acid, methacrylic acid and hydroxyethyl acrylate;
s3, mixing 150-200 parts by weight of water, 1-2 parts by weight of an emulsifying agent and 0.5-2 parts by weight of a pH buffering agent, heating to 80-85 ℃, adding 0.3-3.25 parts by weight of an initiator and 30-40 parts by weight of the primary pre-emulsion in the step S1, and reacting after the addition is finished to obtain seed liquid;
s4, adding 1-2 parts by weight of initiator into 30-40 parts by weight of water to obtain an initiator aqueous solution;
s5, dropwise adding a second-level pre-emulsion into the first-level pre-emulsion left in the step S1 to obtain a mixed solution;
s6, dropwise adding the aqueous solution of the initiator in the step S4 and the mixed solution in the step S5 into the seed solution in the step S3 at the same time, and preserving heat at 80-85 ℃ after the dropwise adding is finished;
s7, cooling after heat preservation is finished, and regulating the pH value of the prepared emulsion to 7.5-8.5 to obtain an acrylic emulsion pressure-sensitive adhesive product;
in the formed pressure-sensitive adhesive product, the glass transition temperature of the shell monomer is gradually changed from inside to outside: namely, the butyl acrylate and the octyl acrylate of the shell layer are gradually increased from inside to outside, and the styrene of the shell layer is gradually decreased from inside to outside.
2. The method for preparing the pressure-sensitive adhesive with the gradient structure and high peel strength and high water resistance according to claim 1, wherein the molecular weight regulator in the step S2 is at least one or a combination of more of n-dodecyl mercaptan, tert-dodecyl mercaptan and octyl mercaptan.
3. The method for preparing the pressure-sensitive adhesive with the gradient structure and high peel strength and high water resistance according to claim 1, wherein the emulsifying agent in the steps S1, S2 and S3 is one or two of 2A1 and SR-10.
4. The method for preparing the pressure-sensitive adhesive with the gradient structure and high peel strength and high water resistance according to claim 1, wherein the reaction time in the step S3 is 5-15min, and the pH buffering agent is ammonium bicarbonate, sodium bicarbonate or sodium dihydrogen phosphate.
5. The method for preparing the pressure-sensitive adhesive with the gradient structure and high peel strength and high water resistance according to claim 1, wherein the initiator in the steps S3 and S4 is ammonium persulfate, sodium persulfate or potassium persulfate.
6. The preparation method of the pressure-sensitive adhesive with the gradient structure and high peel strength and high water resistance according to claim 1, wherein in the step S6, the initiator aqueous solution in the step S4 and the mixed solution in the step S5 are dropwise added to the seed solution in the step S3 at the same time, the dropwise adding time is 3.5-4h, and the heat preservation time is 45-90min after the dropwise adding is completed.
7. The method for preparing the pressure-sensitive adhesive with the gradient structure and high peel strength and high water resistance according to claim 1, wherein the temperature is reduced to 40-55 ℃ after the heat preservation in the step S7 is finished.
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| WO2012038202A1 (en) * | 2010-09-23 | 2012-03-29 | Basf Se | Multistage preparation of aqueous pressure-sensitive adhesive dispersions for producing self-adhesive articles |
| CN104710562A (en) * | 2014-12-31 | 2015-06-17 | 佛山市顺德区巴德富实业有限公司 | Styrene-modified acrylate pressure-sensitive adhesive emulsion and preparation method thereof |
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| WO2012038202A1 (en) * | 2010-09-23 | 2012-03-29 | Basf Se | Multistage preparation of aqueous pressure-sensitive adhesive dispersions for producing self-adhesive articles |
| CN104710562A (en) * | 2014-12-31 | 2015-06-17 | 佛山市顺德区巴德富实业有限公司 | Styrene-modified acrylate pressure-sensitive adhesive emulsion and preparation method thereof |
| CN108752532A (en) * | 2018-05-17 | 2018-11-06 | 北京化工大学 | One kind having gradient damping structure styrene-acrylic emulsion and can toast heavy sizing aqueous damping paint and preparation |
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