CN112552848A - Preparation method of paper-plastic composite adhesive - Google Patents
Preparation method of paper-plastic composite adhesive Download PDFInfo
- Publication number
- CN112552848A CN112552848A CN202011453877.8A CN202011453877A CN112552848A CN 112552848 A CN112552848 A CN 112552848A CN 202011453877 A CN202011453877 A CN 202011453877A CN 112552848 A CN112552848 A CN 112552848A
- Authority
- CN
- China
- Prior art keywords
- emulsion
- rosin
- paper
- plastic composite
- composite adhesive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/064—Copolymers with monomers not covered by C09J133/06 containing anhydride, COOH or COOM groups, with M being metal or onium-cation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
A preparation method of a paper-plastic composite adhesive comprises the steps of firstly, emulsifying rosin to prepare rosin tackifying emulsion, secondly, synthesizing the emulsion and preparing the paper-plastic composite adhesive, putting an emulsifier solution into a three-neck flask, and adding a mixed monomer into the mixture to react to obtain stable pre-emulsion; adding an emulsifier solution, an ammonium persulfate initiator, a 10 wt% sodium bicarbonate solution and a pre-emulsion into a three-neck flask for reaction to obtain a seed emulsion; dropwise adding the pre-emulsion and an ammonium persulfate initiator into the seed emulsion, keeping the temperature, cooling, adding the rosin tackifying emulsion, and stirring to obtain the paper-plastic composite adhesive; the composite adhesive obtained by changing the types and the compositions of the monomers, adding the emulsified rosin into the polymer emulsion and selecting the conditions such as the types and the dosage of the emulsifier, the dosage of the initiator, the polymerization temperature, the reaction time, the tackifying resin and the like has high bonding strength, good and stable brightness, and good stability and water resistance.
Description
Technical Field
The invention relates to preparation of an adhesive in the printing and packaging industry, in particular to a preparation method of a paper-plastic composite adhesive.
Background
At present, the flexible package printing industry in China is rapidly developed and becomes an important post industry in the economic development of China, and various plastic flexible packages with beautiful appearances become mainstream of commodity packages as can be understood from the packages of various commodities in supermarkets. The flexible package is rapidly developed, various functional materials are more and more widely applied, and meanwhile, as the nation advocates green and environment-friendly materials, many domestic enterprises begin to pay attention to the development of environment-friendly packaging materials.
The single-component adhesive taking toluene as a solvent is gradually replaced by a double-component polyurethane adhesive later along with the enhancement of national environmental protection consciousness, and the paper-plastic composite packaging in the market is mainly compounded by the double-component polyurethane adhesive basically. However, when the polyurethane adhesive is applied to paper-plastic lamination, some quality problems can also occur due to improper use. Most commonly, poor peel strength, blistering at the heat seal, curling, etc. are observed.
The reasons for quality problems are many inter-related. For example, the foaming at the heat sealing position, the poor glass strength, the corrugation and the like are all in certain relation, so when the double-component polyurethane adhesive is used for compounding paper and plastics, the following problems are mainly caused:
1. the double-component polyurethane adhesive is a reaction type adhesive, is sensitive to the content of moisture and alcohol in a solvent, and can influence the full crosslinking of the polyurethane adhesive because the compounded paper also has a certain amount of moisture.
2. The paper surface is rough and has more pores. Compared with paper-plastic compounding, the sizing amount is relatively large, otherwise the compounding strength is influenced or bubbles are generated, and the bubbling of the compound film is caused when the humidity of the compound paper is too high.
3. Because the polyurethane adhesive is a reactive two-component adhesive, the initial adhesive force is poor when paper is compounded, the temperature of a drying tunnel is not too high, the tension is not too high, the temperature of a compounding roller is not too high after a plastic film is coated during compounding, and the phenomenon of curling or wrinkling is easy to occur otherwise.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a paper-plastic composite adhesive, which obtains a novel paper-plastic composite adhesive with high bonding strength, good and stable brightness, and greatly improved stability and water resistance by changing the types and the compositions of monomers, adding a certain proportion of emulsified rosin into polymer emulsion, and selecting the conditions such as the types and the dosage of an emulsifier, the dosage of an initiator, the polymerization temperature, the reaction time, tackifying resin and the like, and not only can adapt to the process requirements of the existing paper-plastic compound machine, but also has important environmental protection value and economic significance due to no pollution, low cost and low energy consumption.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a paper-plastic composite adhesive comprises the following steps:
step one, preparation of emulsified rosin
(1) Adding 110-135 g rosin into a three-neck flask, adding 95-105 ml alcohol, heating to 80 ℃ until the rosin is dissolved, respectively adding 5.5-6.5 g rosin emulsifier and 55-65 ml hot water at 80 ℃, strongly stirring for 30min until the rosin is milky white, and cooling to 70 ℃;
(2) under strong stirring, dripping 35-45 ml of 10 wt% polyvinyl alcohol solution within 30min, continuing stirring for 30min, cooling and discharging to obtain a product which is light yellow viscous liquid with a solid content of 32-45%, namely rosin tackifying emulsion;
step two, emulsion synthesis and preparation of paper-plastic composite adhesive
(1) Pre-emulsification: 3.5-4.5 g of emulsifier solution is taken and put into a three-neck flask, and the mixed monomer is dripped into the three-neck flask within 1h under the stirring at the temperature of 20 ℃ to obtain stable pre-emulsion; the emulsifier solution is a mixture of sodium dodecyl sulfate and OP10, and the mass ratio of the sodium dodecyl sulfate to the OP10 is 1: 2; the mixed monomer is a mixture of the following three monomers: 90-110 g of butyl acrylate, 70-90 g of vinyl acetate and 10-30 g of acrylic acid, namely the mass ratio range of butyl acrylate: vinyl acetate: acrylic acid ═ (45-55): (35-45): (5-15);
(2) adding 1.8-2.2 g of emulsifier solution, 0.5-0.7 g of ammonium persulfate initiator, 5-10 g of 10 wt% sodium bicarbonate solution and 35-45 g of pre-emulsion into a three-neck flask, heating, and keeping the temperature at 75-77 ℃ until the reflux stops and blue light appears to obtain seed emulsion;
(3) dropwise adding 155-165 g of pre-emulsion and 0.9-1.1 g of ammonium persulfate initiator into the seed emulsion within 2-2.5 h;
(4) keeping the temperature for 1h at 75-80 ℃;
(5) cooling to 40-50 ℃, adding 90-110 g of rosin tackifying emulsion, and uniformly stirring to obtain the paper-plastic composite adhesive.
The invention has the advantages that:
1. the paper-plastic composite film with the water-based adhesive is relatively flat, rarely curls and has good adaptability.
2. The water-based adhesive composite product has good sanitary performance, no residual solvent, convenient cleaning and simple operation.
3. The composite product has good initial peel strength, and can be cut and rewound after being cured for 1-2 hours.
4. Solves the problem that the paper-plastic composite film is easy to generate bubbles and wrinkles.
5. No solvent volatilization (water is volatilized), and improved production environment.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example one
A preparation method of a paper-plastic composite adhesive comprises the following steps:
step one, preparation of emulsified rosin
(1) Adding 120 g of rosin into a three-neck flask, adding 100 ml of alcohol, heating to 80 ℃ until the rosin is dissolved, respectively adding 6 g of rosin emulsifier and 60 ml of hot water at 80 ℃,
stirring vigorously for 30min to milk white, and cooling to 70 deg.C;
(2) dripping 40 ml of 10 wt% polyvinyl alcohol solution under strong stirring, continuing stirring for 30min after dripping within 30min, cooling and discharging to obtain a product which is light yellow viscous liquid with a solid content of 42%, namely rosin tackifying emulsion;
step two, emulsion synthesis and preparation of paper-plastic composite adhesive
(1) Pre-emulsification: putting 4 g of emulsifier solution into a three-neck flask, and dropwise adding 200 g of mixed monomers under stirring for 1h to obtain stable pre-emulsion; the emulsifier solution is a mixture of sodium dodecyl sulfate and OP10, and the ratio of the sodium dodecyl sulfate to the OP10 is 1: 2; the mass ratio of the mixed monomers is as follows: butyl acrylate: vinyl acetate: acrylic acid 50:40: 10.
(2) Adding 2 g of emulsifier solution, 0.6 g of ammonium persulfate initiator, 8 g of 10 wt% sodium bicarbonate solution and 40 g of pre-emulsion into a three-neck flask, heating, and keeping the temperature at 75-77 ℃ until the reflux stops and blue light appears to obtain seed emulsion;
(3) 160 g of pre-emulsion and 1 g of ammonium persulfate initiator are dropwise added into the seed emulsion, and the seed emulsion is completely dropwise added within 2-2.5 h;
(4) keeping the temperature for 1h at 75-80 ℃;
(5) cooling to 40-50 ℃, adding 100 g of rosin tackifying emulsion, and uniformly stirring to obtain the paper-plastic composite adhesive.
The reason for selecting the components of this example is as follows:
selecting mixed monomers and designing a formula:
in the acrylate emulsion adhesive, the comonomer is generally divided into three parts: the first part is soft monomer, the glass transition temperature is low, and the adhesive is endowed with the adhesive property, such as methyl acrylate, ethyl acrylate, butyl acrylate, isooctyl acrylate and the like, and the butyl acrylate is preferably selected; the second part is hard monomer with high glass transition temperature, which endows cohesive force to the adhesive, such as methyl methacrylate, styrene, acrylonitrile, vinyl acetate, vinylidene chloride, etc., preferably vinyl acetate; the third part is a functional monomer. By introducing monomers with functional groups, adhesive reaction characteristics such as methylol acrylamide, acrylic acid and the like are endowed. Due to the surface of the paper-plastic composite adhesive: a non-polar biaxially oriented polypropylene (BOPP) film surface, which has a very low surface energy; one is a very polar paper printing ink surface (or paper surface). So that they are difficult to adhere to each other. In order to increase the cohesive strength of the copolymer and to improve the adhesion strength to the paper or printing surface, a polar acrylic monomer is chosen as the functional monomer, and its addition is very advantageous for emulsion stability.
The formula design of the mixed monomer is as follows:
in selecting the monomer ratio, the equation is based on Cordon-Taylor. The glass transition temperature of the emulsion copolymer was calculated. The Cordon-Tdylor equation is as follows:
1/Tg＝W1/Tg1+W2/Tg2+…+Wn/Tgn
(Note: WI, W2, …, Wn are the mass fractions of the comonomers)
The glass transition temperature of the paper-plastic composite adhesive is preferably-15 to 0 ℃. The Tg is too low, the initial adhesion is good, the composite gloss is good, but the cohesive strength is low, the creep resistance is poor, and the composite is easy to wrinkle and delaminate; the Tg is too high, the cohesive strength is improved, but the composite gloss is poor, the hot pressing speed is too slow during the compounding, and the cost is high. From this, the polymerized monomer butyl acrylate was determined: vinyl acetate: the ratio of acrylic acid is 50:40: and most preferably 10. In order to increase the initial viscosity of the finished product, emulsified rosin tackifying resin is added.
Selection of the type and amount of emulsifier:
the emulsifier used in the acrylate copolymer emulsion is a complex system of anionic and nonionic types. Generally, the dosage of the anionic emulsifier is less, and the dosage of the nonionic emulsifier is larger, so that the prepared emulsion has good stability. Therefore, a complex of sodium dodecyl sulfate and OP-10 is selected as an emulsifier, and the ratio of the sodium dodecyl sulfate to the OP-10 is 1: 2. When the using amount of the emulsifier is less, the concentration of the emulsifier is reduced, the number of micelles is reduced, the colloidal particles are increased, and finally large particles are generated, so that the reaction stability of the system is poor. When the concentration of the emulsifier is too high, the emulsion particles with smaller particle size are agglomerated, namely the particles are not uniformly distributed.
The dosage of the composite emulsifier has influence on the viscosity, stability and bonding strength of the emulsion type paper-plastic composite adhesive. The stability is improved along with the increase of the dosage of the composite emulsifier, but the bonding strength is reduced when the dosage is too high or too low. Experimental research shows that when the dosage of the emulsifier is about 3 percent (accounting for the total weight of the monomer), the emulsion has no agglomeration, is milky white, has blue light and has good stability.
Selection of the amount of initiator:
the synthesis of acrylate emulsion copolymer adhesive belongs to free radical polymerization reaction, and water soluble persulfate is used as initiator, such as ammonium persulfate, potassium persulfate, sodium persulfate, etc. and ammonium persulfate is selected as initiator. The amount of the initiator has a great influence on the conversion rate of the monomers and the bonding strength of the adhesive. When the dosage of the initiator is less, the monomer reaction is incomplete, the solid content can not meet the requirement designed in advance, and the odor of the emulsion adhesive is also great. The reaction tends to be complete by appropriately increasing the proportion of initiator. The viscosity and the conversion rate increase and then decrease with the increase of the amount of the initiator, because the amount of the initiator increases, the concentration of the radicals increases, that is, the nucleation rate increases, and under the condition of a certain amount of the monomer, the average diameter of the latex particles decreases, the contact area between the particles increases, and the friction force of mutual movement increases, so the surface viscosity of the latex particles increases, and the viscosity decreases, possibly because the particle size distribution of the latex particles is widened due to a higher initiator concentration, the viscosity of the latex decreases. The influence of the initiator amount on the adhesive strength of the adhesive is examined and is shown in table 1.
It can be seen from Table l that the solid content is maximized and the peel strength is maximized when the amount of the initiator is more than 0.8% based on the total amount of the monomers added. Therefore, the concentration is preferably about 0.8%.
Influence of the choice of polymerization temperature on the reaction:
when the temperature is too high, the chain growth rate is increased, so that the polymerization reaction rate is increased, when the temperature is too low, the reaction time is long, the loss of monomers in the polymerization process is easily caused, the polymerization temperature has great influence on the diameter and the number of emulsion particles and the stability of the emulsion, the higher the reaction temperature is, the faster the initiator rate is, the formation rate of free radicals and the emulsion particles is increased, more emulsion particles can be generated, the particle size is reduced, but the polymerization reaction temperature is increased, the emulsion particles become soft, the possibility of agglomeration of the particles due to collision in the polymerization process is increased, on the other hand, the temperature is increased, the adsorption effect of the emulsion particles on the emulsifier is weakened, and the possibility of particle coalescence is increased. The latex particle size decreases first with the increase of polymerization temperature, and increases again when reaching a certain degree.
TABLE 2 Effect of polymerization temperature on the reaction
As can be seen from Table 2, the polymerization temperature is suitably from 75 to 80 ℃.
The influence of the choice of time on the polymerization temperature on the reaction:
the emulsion has the advantages that the particles of the emulsion are enlarged due to too long reaction time, particularly, when the emulsion is stirred for a long time, the particles are enlarged continuously due to collision among the particles, the particles are gelled, the reaction time is too short, groups are not completely reacted, unpolymerized monomers are polymerized again, the emulsion is unstable, and after six hours, the appearance of the emulsion, the conversion rate of the monomers and other properties are good.
TABLE 3 Effect of reaction time on the reaction
After the reaction time is more than 6h, the emulsion is stable, milky white and has blue light. Therefore, 6 to 7 hours is preferable.
Effect of tackifying resin:
common tackifying resins are rosin, terpene, petroleum resins, and the like. The wettability of the adhesive to the surface of an adherend is improved with the addition of the tackifier resin, the peel strength exhibited between the two at the interface increases with the increase in the content of the tackifier resin, and after reaching a maximum value, the adhesive layer is broken due to the decrease in cohesive energy of the adhesive, and the peel strength is decreased. Emulsified rosin is selected as tackifying resin, and the influence of the dosage of the emulsified rosin on the bonding strength of an adhesive is examined
TABLE 4 Effect of emulsified rosin amount on peel strength of adhesives
As can be seen from Table 4, the peel strength of the adhesive was the greatest when the amount of the emulsified rosin tackifier resin was 50%. Therefore, the optimum amount of the emulsified rosin tackifier resin is 50%.
In the embodiment, a novel acrylate adhesive capable of meeting the requirements of paper-plastic composite tables is prepared by reasonably selecting a polymerization monomer and a design formula, the adhesive has the best service performance, and the peel strength reaches 4.4N/2.5cm2。
Example two
A preparation method of a paper-plastic composite adhesive comprises the following steps:
step one, preparation of emulsified rosin
(1) Adding 110 g of rosin into a three-neck flask, adding 95 ml of alcohol, heating to 80 ℃ until the rosin is dissolved, respectively adding 5.5 g of rosin emulsifier and 55 ml of 80 ℃ hot water, strongly stirring for 30min to be milk white, and cooling to 70 ℃;
(2) under strong stirring, dripping 35 ml of 10 wt% polyvinyl alcohol solution, finishing dripping within 30min, continuing stirring for 30min, cooling and discharging, wherein the product is light yellow viscous liquid, and the solid content is 32%, so that the rosin tackifying emulsion is obtained;
step two, emulsion synthesis and preparation of paper-plastic composite adhesive
(1) Pre-emulsification: 3.5 g of emulsifier solution is taken and put into a three-neck flask, and the mixed monomer is added into the three-neck flask dropwise within 1 hour under the stirring at the temperature of 20 ℃ to obtain stable pre-emulsion; the emulsifier solution is a mixture of sodium dodecyl sulfate and OP10, and the mass ratio of the sodium dodecyl sulfate to the OP10 is 1: 2; the mixed monomer is a mixture of the following three monomers: 90 g of butyl acrylate, 90 g of vinyl acetate and 10 g of acrylic acid;
(2) adding 1.8 g of emulsifier solution, 0.5 g of ammonium persulfate initiator, 5 g of 10 wt% sodium bicarbonate solution and 35 g of pre-emulsion into a three-neck flask, heating, and keeping the temperature at 75 ℃ until the reflux stops and blue light appears to obtain seed emulsion;
(3) dropwise adding 155 g of pre-emulsion and 0.9-g of ammonium persulfate initiator into the seed emulsion, and completing dropwise adding within 2-2.5 h;
(4) keeping the temperature for 1h at 75-80 ℃;
(5) cooling to 40-50 ℃, adding 90 g of rosin tackifying emulsion, and uniformly stirring to obtain the paper-plastic composite adhesive.
The effect is as follows: the peel strength of the obtained paper-plastic composite adhesive reaches 4.2N/2.5cm2。
EXAMPLE III
A preparation method of a paper-plastic composite adhesive comprises the following steps:
step one, preparation of emulsified rosin
(1) Adding 135 g of rosin into a three-neck flask, adding 105 ml of alcohol, heating to 80 ℃ until the rosin is dissolved, respectively adding 6.5 g of rosin emulsifier and 65 ml of 80 ℃ hot water, strongly stirring for 30min to be milk white, and cooling to 70 ℃;
(2) under strong stirring, dripping 45 milliliters of 10 weight percent polyvinyl alcohol solution within 30 minutes, continuing stirring for 30 minutes, cooling and discharging, wherein the product is light yellow viscous liquid, and the solid content is 45 percent, thus obtaining the rosin tackifying emulsion;
step two, emulsion synthesis and preparation of paper-plastic composite adhesive
(1) Pre-emulsification: 4.5 g of emulsifier solution is taken and put into a three-neck flask, and the mixed monomer is added into the three-neck flask dropwise within 1 hour under the stirring at the temperature of 20 ℃ to obtain stable pre-emulsion; the emulsifier solution is a mixture of sodium dodecyl sulfate and OP10, and the mass ratio of the sodium dodecyl sulfate to the OP10 is 1: 2; the mixed monomer is a mixture of the following three monomers: 110 g of butyl acrylate, 70 g of vinyl acetate and 30 g of acrylic acid;
(2) adding 2.2 g of emulsifier solution, 0.7 g of ammonium persulfate initiator, 10 g of 10 wt% sodium bicarbonate solution and 45 g of pre-emulsion into a three-neck flask, heating, and keeping the temperature at 75-77 ℃ until the reflux stops and blue light appears to obtain seed emulsion;
(3) dripping 165 g of pre-emulsion and 0.9-1.1 g of ammonium persulfate initiator into the seed emulsion within 2-2.5 h;
(4) keeping the temperature for 1h at 75-80 ℃;
(5) cooling to 40-50 ℃, adding 110 g of rosin tackifying emulsion, and uniformly stirring to obtain the paper-plastic composite adhesive.
The effect is as follows: the peel strength of the obtained paper-plastic composite adhesive reaches 4.3N/2.5cm2。
Claims (2)
1. The preparation method of the paper-plastic composite adhesive is characterized by comprising the following steps:
step one, preparation of emulsified rosin
(1) Adding 110-135 g rosin into a three-neck flask, adding 95-105 ml alcohol, heating to 80 ℃ until the rosin is dissolved, respectively adding 5.5-6.5 g rosin emulsifier and 55-65 ml hot water at 80 ℃, strongly stirring for 30min until the rosin is milky white, and cooling to 70 ℃;
(2) under strong stirring, dripping 35-45 ml of 10 wt% polyvinyl alcohol solution within 30min, continuing stirring for 30min, cooling and discharging to obtain a product which is light yellow viscous liquid with a solid content of 32-45%, namely rosin tackifying emulsion;
step two, emulsion synthesis and preparation of paper-plastic composite adhesive
(1) Pre-emulsification: 3.5-4.5 g of emulsifier solution is taken and put into a three-neck flask, and the mixed monomer is dripped into the three-neck flask within 1h under the stirring at the temperature of 20 ℃ to obtain stable pre-emulsion; the emulsifier solution is a mixture of sodium dodecyl sulfate and OP10, and the mass ratio of the sodium dodecyl sulfate to the OP10 is 1: 2; the mixed monomer is a mixture of the following three monomers: 90-110 g of butyl acrylate, 70-90 g of vinyl acetate and 10-30 g of acrylic acid, namely the mass ratio range of butyl acrylate: vinyl acetate: acrylic acid ═ (45-55): (35-45): (5-15);
(2) adding 1.8-2.2 g of emulsifier solution, 0.5-0.7 g of ammonium persulfate initiator, 5-10 g of 10 wt% sodium bicarbonate solution and 35-45 g of pre-emulsion into a three-neck flask, heating, and keeping the temperature at 75-77 ℃ until the reflux stops and blue light appears to obtain seed emulsion;
(3) dropwise adding 155-165 g of pre-emulsion and 0.9-1.1 g of ammonium persulfate initiator into the seed emulsion within 2-2.5 h;
(4) keeping the temperature for 1h at 75-80 ℃;
(5) cooling to 40-50 ℃, adding 90-110 g of rosin tackifying emulsion, and uniformly stirring to obtain the paper-plastic composite adhesive.
2. The preparation method of the paper-plastic composite adhesive according to claim 1, characterized by comprising the following steps:
step one, preparation of emulsified rosin
(1) Adding 120 g of rosin into a three-neck flask, adding 100 ml of alcohol, heating to 80 ℃ until the rosin is dissolved, respectively adding 6 g of rosin emulsifier and 60 ml of 80 ℃ hot water, strongly stirring for 30min to be milk white, and cooling to 70 ℃;
(2) dripping 40 ml of 10 wt% polyvinyl alcohol solution under strong stirring, continuing stirring for 30min after dripping within 30min, cooling and discharging to obtain a product which is light yellow viscous liquid with a solid content of 42%, namely rosin tackifying emulsion;
step two, emulsion synthesis and preparation of paper-plastic composite adhesive
(1) Pre-emulsification: putting 4 g of emulsifier solution into a three-neck flask, and dropwise adding 200 g of mixed monomers under stirring for 1h to obtain stable pre-emulsion; the emulsifier solution is a mixture of sodium dodecyl sulfate and OP10, and the ratio of the sodium dodecyl sulfate to the OP10 is 1: 2; the mass ratio of the mixed monomers is as follows: butyl acrylate: vinyl acetate: acrylic acid 50:40: 10;
(2) adding 2 g of emulsifier solution, 0.6 g of ammonium persulfate initiator, 8 g of 10 wt% sodium bicarbonate solution and 40 g of pre-emulsion into a three-neck flask, heating, and keeping the temperature at 75-77 ℃ until the reflux stops and blue light appears to obtain seed emulsion;
(3) 160 g of pre-emulsion and 1 g of ammonium persulfate initiator are dropwise added into the seed emulsion, and the seed emulsion is completely dropwise added within 2-2.5 h;
(4) keeping the temperature for 1h at 75-80 ℃;
(5) cooling to 40-50 ℃, adding 100 g of rosin tackifying emulsion, and uniformly stirring to obtain the paper-plastic composite adhesive.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011453877.8A CN112552848A (en) | 2020-12-12 | 2020-12-12 | Preparation method of paper-plastic composite adhesive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011453877.8A CN112552848A (en) | 2020-12-12 | 2020-12-12 | Preparation method of paper-plastic composite adhesive |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112552848A true CN112552848A (en) | 2021-03-26 |
Family
ID=75061558
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011453877.8A Pending CN112552848A (en) | 2020-12-12 | 2020-12-12 | Preparation method of paper-plastic composite adhesive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112552848A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023114407A1 (en) * | 2021-12-16 | 2023-06-22 | Basf Se | Rosin modified acrylic emulsions for liquid barrier coating compositions |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000309771A (en) * | 1999-04-27 | 2000-11-07 | Arakawa Chem Ind Co Ltd | Tackifying resin emulsion and aqueous pressure-sensitive adhesive composition |
-
2020
- 2020-12-12 CN CN202011453877.8A patent/CN112552848A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000309771A (en) * | 1999-04-27 | 2000-11-07 | Arakawa Chem Ind Co Ltd | Tackifying resin emulsion and aqueous pressure-sensitive adhesive composition |
Non-Patent Citations (2)
| Title |
|---|
| 唐宏科等: "新型纸塑复合胶粘剂的研制", 《化学与粘合》 * |
| 林芸等: "松香树脂的乳化及与天然胶乳的复合稳定性", 《高分子材料科学与工程》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023114407A1 (en) * | 2021-12-16 | 2023-06-22 | Basf Se | Rosin modified acrylic emulsions for liquid barrier coating compositions |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1263819C (en) | Adhesive compositions containing low molecular weight polymeric additives | |
| US5908908A (en) | Pressure-sensitive adhesive polymers | |
| CN101906278A (en) | Single-component polyvinylacetate binding agent and preparation method thereof | |
| CN101864258A (en) | Low temperature resistant seal adhesive and preparation method thereof | |
| CN113025243B (en) | Method for preparing acrylate composite adhesive by soap-free emulsion polymerization method | |
| CN103140518A (en) | Multistage preparation of aqueous pressure-sensitive adhesive dispersions for producing self-adhesive articles | |
| JP4800487B2 (en) | Pressure sensitive adhesive | |
| CN116285790B (en) | Polyacrylate pressure-sensitive adhesive for high-tear-resistance protective film, and preparation method and application thereof | |
| CN103031089B (en) | Polyacrylate adhesive for calcium plastic corrugated paper and preparation method thereof | |
| CN105950082A (en) | Colored pressure-sensitive adhesive, manufacturing method thereof, and manufactured pressure-sensitive adhesive tape | |
| WO2022205702A1 (en) | Heat-sealing-type acrylic emulsion for paper and preparation method therefor | |
| CN113563815A (en) | PE foam double-sided adhesive tape and preparation method thereof | |
| CN112552848A (en) | Preparation method of paper-plastic composite adhesive | |
| CN111234726A (en) | Pressure-sensitive adhesive tape capable of being repeatedly pasted and preparation method thereof | |
| CN111269350A (en) | Environment-friendly water-based plastic-plastic composite adhesive and preparation method thereof | |
| CN112375517A (en) | Paper-plastic composite adhesive | |
| CN110003813A (en) | A kind of biomass modified pressure sensitive adhesive and preparation method thereof | |
| CN108285508B (en) | Medium-high viscosity emulsion type acrylate pressure-sensitive adhesive for protective film, and preparation method and application thereof | |
| CN110536947A (en) | Multimodal polymer compositions | |
| CN109897576B (en) | Deep embossing paper-plastic composite water-based adhesive and preparation method thereof | |
| JPS62106976A (en) | Floor lining adhesive based on aqueous polymer dispersion | |
| JP3459301B2 (en) | Process for producing pressure-sensitive adhesive dispersions based on copolymers formed from butyl acrylate and (meth) acrylic acid | |
| CN114940881A (en) | High-solid low-viscosity pressure-sensitive adhesive for anilox roller | |
| EP3653681A1 (en) | Pressure-sensitive adhesive compositions and related aqueous polymer dispersions | |
| CN114044846A (en) | Preparation method of semi-oil semi-aqueous partial adhesive |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210326 |