CN111849395A - Redispersible acrylate hot melt adhesive for paper products and preparation method thereof - Google Patents
Redispersible acrylate hot melt adhesive for paper products and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- 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
- C09J133/064—Copolymers with monomers not covered by C09J133/06 containing anhydride, COOH or COOM groups, with M being metal or onium-cation
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a redispersible acrylate hot melt adhesive for paper products and a preparation method thereof, wherein the hot melt adhesive is prepared by melting and uniformly mixing 79-93 parts by weight of paraffin-modified acrylate polymer, 1-15 parts by weight of dioctyl phthalate and 1-12 parts by weight of rosin; wherein the paraffin-modified acrylate polymer is formed by copolymerizing methyl methacrylate, lauryl methacrylate, vinyl acetate and acrylic acid in a paraffin emulsion; the hot melt adhesive can be redispersed in water in the form of tiny particles in the process of waste paper recovery, is convenient to remove, and does not damage the quality of machines and recycled paper; the melting temperature is 73-86 ℃ and the thermal decomposition temperature is 367-377 ℃ during use, the requirement of low-temperature hot melt adhesive is met, the operating temperature range is wide, formaldehyde gas is hardly generated, and the phenomena of peeling, carbon deposition, oxidative decomposition and other aging of the hot melt adhesive are avoided.
Description
Technical Field
The invention relates to the technical field of hot melt adhesives, and particularly relates to a redispersible acrylate hot melt adhesive for paper products and a preparation method thereof.
Background
At present, the consumption of paper products in China per year is reported to reach 3500 ten thousand tons, rich waste paper resources build the waste paper market in China, and the reasonable recycling of waste paper becomes a difficult problem in the environmental protection process in China. In the process of recycling paper products, various original impurities are removed to ensure the smooth proceeding of waste paper repulping. The removal of adhesive substances is mainly solved in the waste paper recovery process, the adhesive substances in the waste paper mainly comprise various pressure-sensitive adhesives, hot melt adhesives, wax substances, coating adhesives and the like, and the substances can remain in a forming net, a pressing felt, a pressing roller and a drying cylinder in the waste paper recovery process to influence the normal operation of the machine; on the other hand, the produced paper product has poor quality and cannot meet the daily use requirement.
The 2016 industry data published by the European paper industry Association indicates that the highest recovery of waste paper in Europe in 2015 is as high as 71.5%, and the 2020 is planned to increase the recovery of waste paper to 74%. The recovery rate of waste paper is estimated to reach 50% in 2020 of China, but is far less than that of other countries. On the basis of solving the problem of adhesive substances in waste paper recycling, water-soluble and redispersable adhesives are researched most, and the European and American countries stipulate the standard of a 'repulpable' pressure-sensitive adhesive which is divided into water-soluble and 'redispersable' pressure-sensitive adhesives and can be dissolved in water or dispersed in water in the form of tiny particles in the waste paper recycling process, so that the aim of removing the adhesives in paper product recycling is fulfilled; secondly, the product with high hydrophobicity and enough cohesive strength is produced, is not easy to disintegrate during pulping, can be filtered, screened and removed, but may cause damage to production due to incomplete treatment; and thirdly, the adhesive and the waste paper have larger density difference, so that the adhesive and the waste paper are removed by centrifugation, and the running cost is higher.
The adhesives mainly used for bonding paper products at present comprise starch glue, EVA (ethylene vinyl acetate), white latex (polyacrylates and polyvinyl alcohols) and the like, the cohesive strength of the starch adhesive is low, the starch adhesive is not suitable for packaging boxes which need to bear loads, and other types of colloids are difficult to remove in the waste paper recycling process, have high viscosity, are easy to deposit and remain in machines, damage the machines and possibly cause the quality problem of recycled paper products. Therefore, in order to avoid the problem of sticky substances from the source, an adhesive which has moderate bonding strength and cohesive strength and is easy to remove is urgently needed to be designed.
Disclosure of Invention
The invention aims to provide a redispersible acrylic acid ester hot melt adhesive for paper products, which has excellent bonding performance and can redisperse tiny particles in water for convenient removal in the process of recycling waste paper.
The invention also aims to provide a preparation method of the redispersible acrylic acid ester hot melt adhesive for paper products.
Therefore, the technical scheme of the invention is as follows:
a redispersible acrylate hot melt adhesive for paper products comprises 79-93 parts by weight of paraffin-modified acrylate polymer, 1-15 parts by weight of dioctyl phthalate and 1-12 parts by weight of rosin; wherein the paraffin-modified acrylate polymer is formed by copolymerizing methyl methacrylate, lauryl methacrylate, vinyl acetate and acrylic acid in a paraffin emulsion.
Preferably, the paraffin-modified acrylate polymer is prepared from the following raw materials in the following amount: 18-29 parts of methyl methacrylate, 1-12 parts of lauryl methacrylate, 3-7 parts of vinyl acetate, 3-7 parts of acrylic acid, 2-10 parts of paraffin emulsion and 50-58 parts of deionized water, and a persulfate initiator accounting for 0.1-0.4% of the total weight of the copolymer monomer, the paraffin emulsion and the deionized water, 0.4-1.8% of an emulsifier B, 0.1-0.3% of a buffering agent, 0.1-0.8% of a chain transfer agent and 0.1-1.2% of a cross-linking agent; wherein the paraffin emulsion is formed by mixing 15-25 parts of sliced paraffin, 5-15 parts of composite emulsifier A and 70-80 parts of deionized water; the emulsifier A is a composite emulsifier composed of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 8-12: 9; the emulsifier B is a composite emulsifier formed by mixing 3-4: 1 by weight of alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate.
Preferably, the buffer is sodium bicarbonate.
Preferably, the persulfate initiator is potassium persulfate.
Preferably, the chain transfer agent is n-dodecyl mercaptan or t-dodecyl mercaptan.
Preferably, the crosslinking agent is N- (butoxymethyl) acrylamide.
A preparation method of the redispersible acrylate hot melt adhesive for the paper products comprises the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing the sliced paraffin and the composite emulsifier A in a reaction container, setting the temperature at 75 ℃, starting stirring after the paraffin is completely melted, dropwise adding isothermal deionized water within 20 minutes after stirring uniformly, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 8-12: 9;
s2, mixing and stirring part of deionized water, the composite emulsifier B and sodium bicarbonate for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing 3-4: 1 by weight of alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate;
s3, uniformly mixing methyl methacrylate, lauryl methacrylate, vinyl acetate, acrylic acid and a chain transfer agent to obtain a monomer mixed solution;
s4, dissolving potassium persulfate in part of deionized water to prepare a potassium persulfate aqueous solution;
s5, setting the temperature of the mixed solution to be 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, after dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and the cross-linking agent within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and then cooling the obtained composite emulsion to room temperature; dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 2-10 times by using deionized water, and drying at 50 ℃ to obtain an acrylate polymer for the hot melt adhesive;
(II) preparing a paraffin-modified acrylate polymer:
preparing a hot melt adhesive: and uniformly mixing the paraffin-modified acrylate polymer, dioctyl phthalate and rosin in a molten state to obtain the redispersible acrylate hot melt adhesive for paper products.
Compared with the prior art, the redispersible acrylate hot melt adhesive for the paper product has the following beneficial effects:
(1) the dispersible hot melt adhesive can be redispersed in water in the form of tiny particles within 15-25 s in a dispersion effect test. The adhesive is applied to bonding paper products, and can avoid the problems of machine blockage, poor quality of recycled paper and the like in the waste paper recycling process, improve the waste paper recycling efficiency and reduce the energy loss in the recycling process;
(2) the dispersible hot melt adhesive has the melting temperature of 73-86 ℃, the thermal decomposition temperature of 367-377 ℃, belongs to a low-temperature hot melt adhesive, has low gluing temperature, and saves energy consumption during use; the cross-linking agent with high thermal stability is used, free formaldehyde is not generated at normal working temperature, the colloid is not easy to oxidize and decompose, and the problems of blocking a hot melt adhesive machine and the like are avoided;
(3) the T-shaped peel strength of the redispersible hot melt adhesive is 49-58N/25 mm under the test of the standard GB/T2791-1995, the higher T-shaped peel strength meets the bonding strength required by bonding paper products, and the bonding strength of the hot melt adhesive is further improved by adding rosin; the single lap shear strength of the redispersible hot melt adhesive can reach 3-4.5 Mpa under the standard GB/T33334-2016, high cohesive strength is shown, namely, the redispersible hot melt adhesive is not easy to damage, and the extrusion resistance strength of a paper package is increased; the redispersible hot melt adhesive has low melt viscosity of 15-20 Pa.s, has good fluidity by adding dioctyl phthalate, is convenient for gluing, and improves the production efficiency.
Detailed Description
The present invention will be further described with reference to the following examples, which are not intended to limit the invention in any way.
Example 1
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 11: 9;
s2, mixing 35 parts of deionized water, 0.4 part of composite emulsifier B and 0.1 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3.5: 1;
s3, uniformly mixing 18 parts of methyl methacrylate, 12 parts of lauryl methacrylate, 3 parts of vinyl acetate, 7 parts of acrylic acid and 0.1 part of n-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 10 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.1 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and then cooling the obtained composite emulsion to room temperature; dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 2 times by using deionized water, and drying at 50 ℃ to obtain a paraffin-modified acrylate polymer;
preparing a hot melt adhesive:
93 parts of paraffin-modified acrylate polymer, 1 part of dioctyl phthalate and 6 parts of rosin are uniformly mixed in a molten state, and the redispersible acrylate hot melt adhesive for paper products is obtained after cooling and forming.
Example 2
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 20 parts of slice paraffin and 5 parts of compound emulsifier A in a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 75 parts of isothermal deionized water in 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 11: 9;
s2, mixing and stirring 37 parts of deionized water, 0.6 part of composite emulsifier B and 0.2 part of sodium bicarbonate for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3.5: 1;
s3, uniformly mixing 21 parts of methyl methacrylate, 9 parts of lauryl methacrylate, 4 parts of vinyl acetate, 6 parts of acrylic acid and 0.2 part of n-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.2 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 8 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.3 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 4 times by using deionized water, and drying at 50 ℃ to obtain an acrylate polymer for the hot melt adhesive;
preparing a hot melt adhesive:
and melting and mixing 90 parts of paraffin-modified acrylate polymer, 4 parts of dioctyl phthalate and 6 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 3
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 15 parts of sliced paraffin and 5 parts of compound emulsifier A in a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water in 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 8: 9;
s2, mixing and stirring 39 parts of deionized water, 0.8 part of composite emulsifier B and 0.3 part of sodium bicarbonate for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3: 1;
s3, uniformly mixing 24 parts of methyl methacrylate, 6 parts of lauryl methacrylate, 5 parts of vinyl acetate, 5 parts of acrylic acid and 0.4 part of n-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.3 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 6 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.6 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 6 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and (3) melting and mixing 87 parts of paraffin-modified acrylate polymer, 7 parts of dioctyl phthalate and 6 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 4
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 15 parts of slice paraffin and 10 parts of compound emulsifier A in a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 75 parts of isothermal deionized water in 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 8: 9;
s2, mixing and stirring 41 parts of deionized water, 1 part of composite emulsifier B and 0.1 part of sodium bicarbonate for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 4: 1;
s3, 27 parts of methyl methacrylate, 3 parts of lauryl methacrylate, 6 parts of vinyl acetate, 4 parts of acrylic acid and 0.6 part of n-dodecyl mercaptan are uniformly mixed to obtain a monomer mixed solution;
s4, dissolving 0.4 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 4 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.9 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 8 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and melting and mixing 84 parts of paraffin-modified acrylate polymer, 10 parts of dioctyl phthalate and 6 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 5
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 15 parts of slice paraffin and 15 parts of compound emulsifier A in a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water in 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 10: 9;
s2, mixing 43 parts of deionized water, 1.2 parts of composite emulsifier B and 0.2 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 4: 1;
s3, mixing 29 parts of methyl methacrylate, 1 part of lauryl methacrylate, 7 parts of vinyl acetate, 3 parts of acrylic acid and 0.8 part of n-dodecyl mercaptan uniformly to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 2 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 1.2 parts by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 10 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
82 parts of paraffin-modified acrylate polymer, 12 parts of dioctyl phthalate and 6 parts of rosin are melted and mixed to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 6
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 1: 1;
s2, mixing and stirring 37 parts of deionized water, 1.4 parts of composite emulsifier B and 0.1 part of sodium bicarbonate for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3.5: 1;
s3, uniformly mixing 21 parts of methyl methacrylate, 9 parts of lauryl methacrylate, 4 parts of vinyl acetate, 6 parts of acrylic acid and 0.1 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.3 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 8 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.3 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 5 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and (3) melting and mixing 79 parts of paraffin-modified acrylate polymer, 15 parts of dioctyl phthalate and 6 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 7
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 20 parts of slice paraffin and 5 parts of compound emulsifier A in a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 75 parts of isothermal deionized water in 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 11: 9;
s2, mixing and stirring 39 parts of deionized water, 1.6 parts of composite emulsifier B and 0.2 part of sodium bicarbonate for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing 3.5:1 by weight of alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate
S3, uniformly mixing 24 parts of methyl methacrylate, 6 parts of lauryl methacrylate, 5 parts of vinyl acetate, 5 parts of acrylic acid and 0.2 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.4 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 6 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.6 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 7 times by using deionized water, and drying at 50 ℃ to obtain an acrylate polymer for the hot melt adhesive;
preparing a hot melt adhesive:
and melting and mixing 92 parts of paraffin-modified acrylate polymer, 7 parts of dioctyl phthalate and 1 part of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 8
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 15 parts of sliced paraffin and 5 parts of compound emulsifier A in a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 80 parts of isothermal deionized water in 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 10: 9;
s2, mixing and stirring 41 parts of deionized water, 1.8 parts of composite emulsifier B and 0.1 part of sodium bicarbonate for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3: 1;
s3, uniformly mixing 27 parts of methyl methacrylate, 3 parts of lauryl methacrylate, 6 parts of vinyl acetate, 4 parts of acrylic acid and 0.4 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 4 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.1 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 3 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and (3) melting and mixing 87 parts of paraffin-modified acrylate polymer, 7 parts of dioctyl phthalate and 6 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 9
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 4: 3;
s2, mixing 43 parts of deionized water, 0.6 part of composite emulsifier B and 0.1 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 4: 1;
s3, mixing 29 parts of methyl methacrylate, 1 part of lauryl methacrylate, 7 parts of vinyl acetate, 3 parts of acrylic acid and 0.6 part of tert-dodecyl mercaptan uniformly to obtain a monomer mixed solution;
s4, dissolving 0.2 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 2 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.3 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 9 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and melting and mixing 84 parts of paraffin-modified acrylate polymer, 7 parts of dioctyl phthalate and 9 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 10
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 11: 9;
s2, mixing 35 parts of deionized water, 0.4 part of composite emulsifier B and 0.1 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3.5: 1;
s3, uniformly mixing 18 parts of methyl methacrylate, 12 parts of lauryl methacrylate, 3 parts of vinyl acetate, 7 parts of acrylic acid and 0.8 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 10 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.1 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 5 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
81 parts of paraffin-modified acrylate polymer, 7 parts of dioctyl phthalate and 12 parts of rosin are melted and mixed to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 11
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 10: 9;
s2, mixing 35 parts of deionized water, 0.4 part of composite emulsifier B and 0.1 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3: 1;
s3, uniformly mixing 18 parts of methyl methacrylate, 12 parts of lauryl methacrylate, 3 parts of vinyl acetate, 7 parts of acrylic acid and 0.1 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 10 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.1 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 5 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and melting and mixing 84 parts of paraffin-modified acrylate polymer, 7 parts of dioctyl phthalate and 9 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 12
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 10: 9;
s2, mixing 35 parts of deionized water, 0.4 part of composite emulsifier B and 0.1 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution;
s3, uniformly mixing 18 parts of methyl methacrylate, 12 parts of lauryl methacrylate, 3 parts of vinyl acetate, 7 parts of acrylic acid and 0.1 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 10 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.1 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 5 times by using deionized water, and drying at 50 ℃ to obtain an acrylate polymer for the hot melt adhesive; the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and lauryl sodium sulfate in a weight ratio of 3: 1.
Preparing a hot melt adhesive:
and (3) melting and mixing 87 parts of paraffin-modified acrylate polymer, 7 parts of dioctyl phthalate and 6 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 13
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 11: 9;
s2, mixing 35 parts of deionized water, 0.4 part of composite emulsifier B and 0.1 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3.5: 1;
s3, uniformly mixing 18 parts of methyl methacrylate, 12 parts of lauryl methacrylate, 3 parts of vinyl acetate, 7 parts of acrylic acid and 0.1 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 10 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.1 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 5 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and melting and mixing 90 parts of paraffin-modified acrylate polymer, 7 parts of dioctyl phthalate and 3 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 14
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 11: 9;
s2, mixing 35 parts of deionized water, 0.4 part of composite emulsifier B and 0.1 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3.5: 1;
s3, uniformly mixing 18 parts of methyl methacrylate, 12 parts of lauryl methacrylate, 3 parts of vinyl acetate, 7 parts of acrylic acid and 0.1 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 10 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.1 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 5 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and melting and mixing 92 parts of paraffin-modified acrylate polymer, 7 parts of dioctyl phthalate and 1 part of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 15
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 11: 9;
s2, mixing 35 parts of deionized water, 0.4 part of composite emulsifier B and 0.1 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3.5: 1;
s3, uniformly mixing 18 parts of methyl methacrylate, 12 parts of lauryl methacrylate, 3 parts of vinyl acetate, 7 parts of acrylic acid and 0.1 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 10 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.1 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 5 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and (3) melting and mixing 93 parts of paraffin-modified acrylate polymer, 1 part of dioctyl phthalate and 6 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 16
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 11: 9;
s2, mixing 35 parts of deionized water, 0.4 part of composite emulsifier B and 0.1 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3.5: 1;
s3, uniformly mixing 18 parts of methyl methacrylate, 12 parts of lauryl methacrylate, 3 parts of vinyl acetate, 7 parts of acrylic acid and 0.1 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 10 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.1 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 5 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and (3) melting and mixing 89 parts of paraffin-modified acrylate polymer, 5 parts of dioctyl phthalate and 6 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 17
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 11: 9;
s2, mixing 35 parts of deionized water, 0.4 part of composite emulsifier B and 0.1 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3.5: 1;
s3, uniformly mixing 18 parts of methyl methacrylate, 12 parts of lauryl methacrylate, 3 parts of vinyl acetate, 7 parts of acrylic acid and 0.1 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 10 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.1 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 5 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and melting and mixing 84 parts of paraffin-modified acrylate polymer, 10 parts of dioctyl phthalate and 6 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
Example 18
A redispersible acrylate hot melt adhesive for paper products is prepared by the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing 25 parts of sliced paraffin and 5 parts of compound emulsifier A into a reaction container, heating to 75 ℃, starting stirring after paraffin is completely melted, dropwise adding 70 parts of isothermal deionized water within 20 minutes after uniform stirring, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 11: 9;
s2, mixing 35 parts of deionized water, 0.4 part of composite emulsifier B and 0.1 part of sodium bicarbonate, and stirring for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate in a weight ratio of 3.5: 1;
s3, uniformly mixing 18 parts of methyl methacrylate, 12 parts of lauryl methacrylate, 3 parts of vinyl acetate, 7 parts of acrylic acid and 0.1 part of tert-dodecyl mercaptan to obtain a monomer mixed solution;
s4, dissolving 0.1 part of potassium persulfate in 15 parts of deionized water to prepare a potassium persulfate aqueous solution;
s5, heating the mixed solution to 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding 10 parts by weight of paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and 0.1 part by weight of N- (butoxymethyl) acrylamide within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and cooling the obtained composite emulsion to room temperature; and (3) dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 5 times by using deionized water, and drying at 50 ℃ to obtain the acrylate polymer for the hot melt adhesive.
Preparing a hot melt adhesive:
and (3) melting and mixing 79 parts of paraffin-modified acrylate polymer, 15 parts of dioctyl phthalate and 6 parts of rosin to obtain the redispersible acrylate hot melt adhesive for paper products.
And (3) performance testing:
eighteen of the redispersible acrylate hot melt adhesives prepared in examples 1-18 were subjected to the following tests.
(I) testing dispersion effect: pressing a certain amount of hot melt adhesive into 0.2mm thin sheets, and cutting into 2cm2The square pieces of (1) were put into water and vigorously stirred, each sample was repeatedly tested 3 times to take an average value, and the complete dispersion time and the dispersion state were observed and recorded. The specific test results are shown in table 1.
Table 1:
from the test results in Table 1, it can be seen that the dispersion time of the eighteen redispersible hot melt adhesives prepared in examples 1-18 is between 15 and 25 seconds, and the adhesives are dispersed in water in the form of fine particles. One of the important parameters for the use of redispersible hot melt adhesives is the redispersion effect, although at present there are no relevant standards for testing redispersible hot melt adhesives, the eighteen redispersible hot melt adhesives of the present application have been tested to be dispersible in water in the form of granules in a short period of time, and to be easily removed. And the commercially available hot melt adhesive is not easy to treat in the waste paper recycling process, so that the waste paper recycling machine is blocked and the quality of recycled paper products is not good.
(II) T-type peel strength: eighteen of the redispersible hot melt adhesives prepared in examples 1-18 were tested for T-peel strength with reference to standard GB/T2791-1995. The specific test results are shown in table 2.
Table 2:
as can be seen from the test results in Table 2, the T-type peel strength of the eighteen redispersible hot melt adhesives prepared in examples 1-18 is 49-58N/25 mm on average; the peel strength of the commercially available hot melt adhesive for bonding paper products is generally 30-40N/25 mm at present, and the peel strength of the eighteen redispersible hot melt adhesives is obviously higher than that of the commercially available hot melt adhesive; therefore, the redispersible hot melt adhesive has excellent bonding strength to paper products.
(III) single lap shear strength test: the eighteen redispersible hot melt adhesives prepared in examples 1 to 18 were tested for their single lap shear strength with reference to the standard GB/T33334-2016. The specific test results are shown in table 3.
Table 3:
from the test results in table 3, it can be seen that the single lap shear strength of the eighteen redispersible hot melt adhesives prepared in examples 1-18 can reach 3-4.5 Mpa. The anti-extrusion strength of the material is increased while the bonding is realized, and the experimental result can show that the eighteen redispersible hot melt adhesives have high cohesive strength and the adhesive layer is not easy to break.
(IV) testing the melting temperature and the thermal decomposition temperature: melting points of the eighteen kinds of redispersible hot melt adhesives prepared in examples 1 to 18 were measured by a melting point tester, and an average value was obtained by performing parallel experiments for 3 times for each kind of redispersible hot melt adhesive; the thermal decomposition temperatures of the redispersible hot melt adhesives prepared in examples 1 to 18 were each measured using a comprehensive thermal analyzer, N2The temperature rise rate is 10 ℃/min, and the test range of the sample is 15-600 ℃. The specific test results are shown in table 4.
Table 4:
from the test results in table 4, it can be seen that the eighteen kinds of redispersible hot melt adhesives prepared in examples 1 to 18 have melting temperatures of 73 to 86 ℃ and thermal decomposition temperatures of 367 to 377 ℃, and belong to low-temperature hot melt adhesives. The low-temperature hot melt adhesive hardly generates the aging phenomena of peeling, carbon deposition, oxidative decomposition and the like of the hot melt adhesive at normal working temperature, has wide operating temperature range, is not easy to cause machine blockage, and can reduce the maintenance times of the machine. Therefore, the redispersible hot melt adhesive has the advantages of obviously low melting temperature, excellent creep resistance and bonding strength, short curing time, low-temperature melting, energy conservation and carbon emission reduction in the using process.
And (V) testing the melt viscosity of the hot melt adhesive with different dioctyl phthalate contents: and testing the melt viscosity of the hot melt adhesive by using a digital display viscometer, wherein the testing temperature is 130-140 ℃, and each sample is tested for 3 times and the average value is obtained. The melt viscosities of the four redispersible hot melt adhesives prepared in examples 15-18 were tested, and the four redispersible hot melt adhesives were distinguished by increasing the dioctyl phthalate content. The specific test results are shown in table 5.
Table 5:
| examples | 15 | 16 | 17 | 18 |
| Melt viscosity/(Pa. s) | 19 | 18 | 17 | 15 |
From the test results in table 5, it can be seen that the melt viscosities of the four redispersible hot melt adhesives prepared in examples 15 to 18 are between 15 Pa · s and 19 Pa · s, and the melt viscosities are significantly reduced as the addition amount of dioctyl phthalate increases, as viewed from the fluidity at the melting temperature. Therefore, the redispersible hot melt adhesive is convenient for gluing, can realize rapid bonding operation, and can effectively improve the production efficiency in practical application.
Sixthly, testing the adhesive strength of the hot melt adhesive with different rosin contents: the five redispersible hot melt adhesives prepared in examples 10 to 14 were tested for T-peel strength with reference to the standard GB/T2791-1995. The five redispersible hot melt adhesives differ from each other in the amount of rosin used. The specific test results are shown in table 6.
Table 6:
| examples | 10 | 11 | 12 | 13 | 14 |
| T-shaped peeling strength (N/25m) | 58 | 57 | 56 | 54 | 53 |
As can be seen from the test results in Table 6, the T-peel strength of the five redispersible hot melt adhesives prepared in examples 10-14 is 53-58N/25 mm on average. With the increase of the content of rosin, the T-shaped peeling strength of the redispersible hot melt adhesive is remarkably increased, and it can be seen that the peeling strength of the eighteen redispersible hot melt adhesives is obviously higher than that of the commercially available hot melt adhesives, and the redispersible hot melt adhesives have excellent bonding strength.
Claims (7)
1. A redispersible acrylate hot melt adhesive for paper products is characterized by comprising 79-93 parts by weight of paraffin-modified acrylate polymer, 1-15 parts by weight of dioctyl phthalate and 1-12 parts by weight of rosin; wherein the paraffin-modified acrylate polymer is formed by copolymerizing methyl methacrylate, lauryl methacrylate, vinyl acetate and acrylic acid in a paraffin emulsion.
2. The redispersible acrylate hot melt adhesive for paper products according to claim 1, wherein the paraffin-modified acrylate polymer is prepared from the following raw materials in the following amounts: 18-29 parts of methyl methacrylate, 1-12 parts of lauryl methacrylate, 3-7 parts of vinyl acetate, 3-7 parts of acrylic acid, 2-10 parts of paraffin emulsion and 50-58 parts of deionized water, and a persulfate initiator accounting for 0.1-0.4% of the total weight of the copolymer monomer, the paraffin emulsion and the deionized water, 0.4-1.8% of an emulsifier B, 0.1-0.3% of a buffering agent, 0.1-0.8% of a chain transfer agent and 0.1-1.2% of a cross-linking agent; wherein the paraffin emulsion is formed by mixing 15-25 parts of sliced paraffin, 5-15 parts of composite emulsifier A and 70-80 parts of deionized water; the emulsifier A is a composite emulsifier composed of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 8-12: 9; the emulsifier B is a composite emulsifier formed by mixing 3-4: 1 by weight of alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate.
3. The redispersible acrylate hot melt adhesive for paper products according to claim 2, characterized in that the buffering agent is sodium bicarbonate.
4. A redispersible acrylate hot melt adhesive for paper products as claimed in claim 2, characterized in that said persulfate initiator is potassium persulfate.
5. The redispersible acrylate hot melt adhesive for paper products according to claim 2, wherein the chain transfer agent is n-dodecyl mercaptan or t-dodecyl mercaptan.
6. A redispersible acrylate hot melt adhesive for paper products according to claim 2, characterized in that said crosslinking agent is N- (butoxymethyl) acrylamide.
7. A method for preparing the redispersible acrylate hot melt adhesive for paper products as claimed in claim 1, characterized by comprising the following steps:
preparing a paraffin modified acrylate polymer:
s1, placing the sliced paraffin and the composite emulsifier A in a reaction container, setting the temperature at 75 ℃, starting stirring after the paraffin is completely melted, dropwise adding isothermal deionized water within 20 minutes after stirring uniformly, continuing stirring for 40min under heat preservation, and cooling to obtain a paraffin emulsion; wherein the emulsifier A is a composite emulsifier of alkylphenol polyoxyethylene ether-10 and span 80 in a weight ratio of 8-12: 9;
s2, mixing and stirring part of deionized water, the composite emulsifier B and sodium bicarbonate for 10-15 minutes to obtain a mixed solution; wherein the emulsifier B is a composite emulsifier formed by mixing 3-4: 1 by weight of alkylphenol polyoxyethylene ether-10 and sodium dodecyl sulfate;
s3, uniformly mixing methyl methacrylate, lauryl methacrylate, vinyl acetate, acrylic acid and a chain transfer agent to obtain a monomer mixed solution;
s4, dissolving potassium persulfate in part of deionized water to prepare a potassium persulfate aqueous solution;
s5, setting the temperature of the mixed solution to be 40 ℃, adding 1/4 parts by weight of monomer mixed solution and 1/5 parts by weight of potassium persulfate aqueous solution into the mixed solution, uniformly stirring, continuously heating to 60 ℃, adding paraffin emulsion into the mixed solution, mixing and stirring for 10-15 minutes, continuously heating to 75-78 ℃, after dropwise adding the residual monomer mixed solution, the potassium persulfate aqueous solution and the cross-linking agent within 1.5-2 hours, continuously stirring and reacting at 75-78 ℃ for 1.5 hours, and then cooling the obtained composite emulsion to room temperature; dropwise adding a saturated sodium chloride solution into the composite emulsion, and violently stirring at the speed of 200-250 r/min until obvious polymer precipitation occurs in the system, stopping dropwise adding, washing the polymer precipitation for 2-10 times by using deionized water, and drying at 50 ℃ to obtain an acrylate polymer for the hot melt adhesive;
(II) preparing a paraffin-modified acrylate polymer:
preparing a hot melt adhesive: and uniformly mixing the paraffin-modified acrylate polymer, dioctyl phthalate and rosin in a molten state to obtain the redispersible acrylate hot melt adhesive for paper products.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0064893A1 (en) * | 1981-04-30 | 1982-11-17 | Société Chimique des Charbonnages | Compositions applied to the manufacture of hot melt adhesives and process for their preparation |
| AU1422199A (en) * | 1998-02-04 | 1999-08-26 | National Starch And Chemical Investment Holding Corporation | Low application temperature hot melt adhesive |
| JP2000204336A (en) * | 1999-01-13 | 2000-07-25 | Sekisui Chem Co Ltd | Hot-melt adhesive |
| CN107722876A (en) * | 2017-11-17 | 2018-02-23 | 东莞市中凌包装材料有限公司 | A kind of water-based Dispoable medical packing hot-fusible glue and manufacture craft |
| CN111234738A (en) * | 2020-03-26 | 2020-06-05 | 天津科技大学 | Hot melt adhesive for environment-friendly wax cartons and preparation method thereof |
-
2020
- 2020-07-23 CN CN202010716093.3A patent/CN111849395B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0064893A1 (en) * | 1981-04-30 | 1982-11-17 | Société Chimique des Charbonnages | Compositions applied to the manufacture of hot melt adhesives and process for their preparation |
| AU1422199A (en) * | 1998-02-04 | 1999-08-26 | National Starch And Chemical Investment Holding Corporation | Low application temperature hot melt adhesive |
| JP2000204336A (en) * | 1999-01-13 | 2000-07-25 | Sekisui Chem Co Ltd | Hot-melt adhesive |
| CN107722876A (en) * | 2017-11-17 | 2018-02-23 | 东莞市中凌包装材料有限公司 | A kind of water-based Dispoable medical packing hot-fusible glue and manufacture craft |
| CN111234738A (en) * | 2020-03-26 | 2020-06-05 | 天津科技大学 | Hot melt adhesive for environment-friendly wax cartons and preparation method thereof |
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