CN111909647A - Preparation method of resin adhesive - Google Patents
Preparation method of resin adhesive Download PDFInfo
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- CN111909647A CN111909647A CN202010828625.2A CN202010828625A CN111909647A CN 111909647 A CN111909647 A CN 111909647A CN 202010828625 A CN202010828625 A CN 202010828625A CN 111909647 A CN111909647 A CN 111909647A
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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
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
- C09J171/02—Polyalkylene oxides
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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
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/324—Alkali metal phosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/327—Aluminium phosphate
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a preparation method of a resin adhesive, and particularly relates to the technical field of adhesive preparation, and the preparation method specifically comprises the following steps: the method comprises the following steps: preparing raw materials, and step two: the adhesive is prepared by the following specific steps: s1: preparing a matrix, S2: viscosity enhancement, S3: enhancing other properties, S4 vacuum defoamation, S5: and (4) environmental protection modification. According to the invention, the modified starch is added and the corresponding modification process is improved, ester substances and aldehyde substances contained in the starch are utilized, and the epoxy resin is further modified through a reasonable process on the premise of not influencing the self-characteristics of resin adhesive viscosity, so that the adhesive property of the adhesive is enhanced, the use of harmful substances is reduced, the pollution is reduced fundamentally, and the environment-friendly degree is improved.
Description
Technical Field
The invention relates to the technical field of adhesive preparation, in particular to a preparation method of a resin adhesive.
Background
The adhesive can be used for connecting same or two or more same or different workpieces (or materials) together, and after being cured, the adhesive has enough strength, and can be organic or inorganic, natural or synthetic substances, which are collectively called as adhesives or bonding agents, adhesives and conventionally called as glue. The adhesive agent is classified into natural high molecular compounds (starch, animal skin glue, bone glue, natural rubber, etc.), synthetic high molecular compounds (thermosetting resins such as epoxy resin, phenol resin, urea resin, and polyurethane, thermoplastic resins such as polyvinyl acetal and perchloroethylene, and synthetic rubbers such as chloroprene rubber and nitrile rubber), and inorganic compounds (silicates, phosphates, etc.). Curing agents, accelerators, reinforcing agents, olefinic release agents, fillers, and the like are often incorporated into the adhesive depending on the application requirements. According to the classification of the application, warm glue, sealant, structural glue and the like can be separated. The adhesive is classified into room temperature curing adhesive, pressure sensitive adhesive and the like according to the using process. The application of the adhesive can connect the dissimilar materials and the sheet materials, and the stress distribution at the glued joint is uniform. Epoxy resin, neoprene, sealants and the like are commonly used in the manufacture and repair of containers.
In recent years, organic adhesives are more and more widely applied, a bonding technology is developed and matured, and becomes one of three connection technologies of bonding, welding and mechanical connection, but not negligible, various additives are often used as fillers or reinforcing agents in the preparation process of the traditional resin adhesives, the added substances often cause great pollution, and the natural decomposition difficulty of certain harmful substances is great, so that the environmental pollution is great.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide a method for preparing a resin adhesive, in which modified starch is added and corresponding modification processes are improved, ester substances and aldehyde substances contained in the starch are utilized, and epoxy resin is further modified through a reasonable process on the premise of not affecting the viscosity of the resin adhesive, so that the adhesive property of the adhesive is enhanced, the use of harmful substances is reduced, pollution is reduced fundamentally, and the environmental protection degree is improved.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a resin adhesive specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely selecting the following raw materials in percentage by mass: 100-150 parts of epoxy acrylic acid, 100-150 parts of polyoxypropylene diol, 150-300 parts of deionized water, 30-50 parts of redispersible latex powder, 10-15 parts of curing agent, 10-20 parts of toughening agent, 15-20 parts of diluent, 5-10 parts of accelerator, 6-11 parts of coupling agent, 1-5 parts of initiator, 1-5 parts of crosslinking agent, 5-8 parts of reinforcing agent, 3-7 parts of accelerator, 1-5 parts of defoaming agent, 30-40 parts of 30% formaldehyde solution, sufficient alcohol substances and sufficient n-hexane;
step two: the adhesive is prepared by the following specific steps:
s1: preparing a matrix, adding sufficient n-hexane into a reaction kettle A as a solvent, and then synchronously adding the following raw materials in mass fraction into the reaction kettle A: 100-150 parts of epoxy acrylic acid, 100-150 parts of polyoxypropylene diol and 1-5 parts of initiator, introducing a group zero gas with stable property into a reaction kettle A to remove oxygen in the kettle, carrying out polymerization reaction at 80-90 ℃, keeping for 6-10 hours, naturally cooling to room temperature after the time is up, then adding sufficient alcohol substances with stable property into the reaction kettle A, taking out precipitates generated by the polymerization reaction, and drying in a vacuum environment to obtain an adhesive matrix;
s2: enhancing the viscosity, adding the adhesive matrix prepared by S1 into a stirring kettle, then synchronously adding 150-300 parts of deionized water and 30-50 parts of redispersible latex powder into the stirring kettle, keeping the temperature in the reaction kettle at 25-35 ℃, and uniformly stirring for 20-30 minutes to uniformly mix the mixture in the kettle to be pasty to obtain a material A;
s3: and (3) enhancing other properties, placing the material A obtained in the step S2 in a reaction kettle B, and adding the following raw materials in parts by weight: 10-15 parts of curing agent, 10-20 parts of toughening agent, 15-20 parts of diluent, 5-10 parts of accelerator and 6-11 parts of coupling agent, uniformly mixing, sealing, heating to 80-95 ℃, and preserving heat for 30-40 minutes to obtain a material B;
s4, performing vacuum defoaming, namely adding the material B obtained in the step S3 into a planetary stirrer, adding 1-5 parts of defoaming agent into the device, uniformly mixing, and performing vacuum defoaming to obtain a modified resin adhesive;
s5: and (2) performing environment-friendly modification, namely adding 30-40 parts of 30% formaldehyde solution, 1-5 parts of cross-linking agent, 5-8 parts of reinforcing agent and 3-7 parts of accelerating agent in parts by mass into the reaction kettle C, controlling the temperature in the reaction kettle to be 80-90 ℃, preserving heat, stirring for 30-60 minutes, naturally cooling to below 35 ℃, filtering and discharging to obtain the environment-friendly resin adhesive.
In a preferred embodiment, the initiator in the second step S1 is an iodonium salt, a sulfur salt and a ferrocenium salt, and the weight ratio is 1: 2: 3, mixing the mixture evenly, wherein the alcohol substance with stable property is one or a mixture of ethanol, propanol and butanol.
In a preferred embodiment, in the second step S3, the toughening agent is liquid silicone rubber and polyurethane, and the weight ratio is 1: 3 and the stirring rate of the stirrer in the second step S2 is 120 revolutions per minute.
In a preferred embodiment, the cross-linking agent comprises one or more of aluminum phosphate, sodium phosphate, modified starch and sodium chloride required for anti-swelling.
In a preferred embodiment, modified starch refers to starch-based further processed products such as starch acetate, starch phosphate, oxidized starch, dialdehyde starch, or a mixture of more than one of them.
In a preferred embodiment, the reinforcing agent comprises one or more of melamine, polyvinyl alcohol, phthalic acid and salts thereof.
In a preferred embodiment, the accelerator is dicyandiamide, melamine and hexamethylenetetramine in a weight ratio of 1: 1: 1 mixing the mixture.
The invention has the technical effects and advantages that:
1. according to the invention, the modified starch is added and the corresponding modified process is improved, the ester substances and the aldehyde substances contained in the starch are utilized, and the epoxy resin is further modified through a reasonable process on the premise of not influencing the self characteristics of the resin adhesive viscosity, so that the adhesive property of the adhesive is enhanced, the use of harmful substances is reduced, the pollution is reduced fundamentally, and the environmental protection degree is improved;
2. the invention eliminates oxygen in the kettle by the group zero gas with stable property, so that the epoxy acrylic acid and the polyoxypropylene diol are deoxidized while fully reacting to generate the ester, and the characteristics of the ester are enhanced under the condition of ensuring the mechanical characteristics and hardness of the epoxy, thereby reducing additives, reducing resource waste and improving the environment protection degree.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a preparation method of a resin adhesive, which specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely selecting the following raw materials in percentage by mass: 100 parts of epoxy acrylic acid, 100 parts of polyoxypropylene diol, 150 parts of deionized water, 30 parts of redispersible latex powder, 10 parts of curing agent, 10 parts of toughening agent, 15 parts of diluent, 5 parts of accelerator, 6 parts of coupling agent, 1 part of initiator, 1 part of crosslinking agent, 5 parts of reinforcing agent, 3 parts of accelerator, 1 part of defoaming agent, 30 parts of 30% formaldehyde solution, sufficient alcohol substance and sufficient n-hexane;
step two: the adhesive is prepared by the following specific steps:
s1: preparing a matrix, adding sufficient n-hexane into a reaction kettle A as a solvent, and then synchronously adding the following raw materials in mass fraction into the reaction kettle A: 100 parts of epoxy acrylic acid, 100 parts of polyoxypropylene diol and 1 part of initiator, wherein the initiator is iodized salt, sulfur salt and ferrocenium salt according to the weight ratio of 1: 2: 3, uniformly mixing the mixture, introducing a group zero gas with stable property into a reaction kettle A to remove oxygen in the kettle, carrying out polymerization reaction at the temperature of 80 ℃, keeping for 6 hours, naturally cooling to room temperature after the time is up, then adding a sufficient amount of alcohol substance with stable property into the reaction kettle A, wherein the alcohol substance is one or a mixture of ethanol, propanol and butanol, and is used for taking out a precipitate generated by the polymerization reaction and drying in a vacuum environment to obtain an adhesive matrix;
s2: enhancing the viscosity, adding the adhesive matrix prepared in S1 into a stirring kettle, then synchronously adding 150 parts of deionized water and 30 parts of redispersible latex powder into the stirring kettle, keeping the temperature in the reaction kettle at 25 ℃, and uniformly stirring for 20 minutes at a stirring speed of 120 revolutions per minute to uniformly mix the mixture in the kettle to form paste, thus obtaining a material A;
s3: and (3) enhancing other properties, placing the material A obtained in the step S2 in a reaction kettle B, and adding the following raw materials in parts by weight: uniformly mixing 10 parts of curing agent, 10 parts of toughening agent, 15 parts of diluent, 5 parts of accelerator and 6 parts of coupling agent, sealing, heating to 80 ℃, and preserving heat for 30 minutes to obtain a material B;
s4, performing vacuum defoaming, namely adding the material B obtained in the step S3 into a planetary stirrer, adding 1-5 parts of defoaming agent into the device, uniformly mixing, and performing vacuum defoaming to obtain a modified resin adhesive;
s5: adding 30 parts of 30% formaldehyde solution, 1 part of cross-linking agent, 5 parts of reinforcing agent and 3 parts of accelerating agent in parts by mass into a reaction kettle C, controlling the temperature in the reaction kettle to be 80 ℃, and stirring for 30 minutes under heat preservation, then naturally cooling to below 35 ℃, filtering and discharging to obtain the environment-friendly resin adhesive, the cross-linking agent comprises one or more of aluminum phosphate, sodium phosphate, modified starch and sodium chloride required by anti-swelling, the modified starch refers to one or more of starch deep-processing products such as starch acetate, starch phosphate, oxidized starch and dialdehyde starch, the reinforcing agent comprises one or more of melamine, polyvinyl alcohol, phthalic acid and salts thereof, and the accelerator is dicyandiamide, melamine and hexamethylenetetramine according to the weight ratio of 1: 1: 1 mixing the mixture.
Example 2:
the invention provides a preparation method of a resin adhesive, which specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely selecting the following raw materials in percentage by mass: 110 parts of epoxy acrylic acid, 110 parts of polyoxypropylene diol, 200 parts of deionized water, 35 parts of redispersible latex powder, 11 parts of curing agent, 12 parts of toughening agent, 16 parts of diluent, 6 parts of accelerator, 7 parts of coupling agent, 2 parts of initiator, 2 parts of crosslinking agent, 6 parts of reinforcing agent, 4 parts of accelerator, 2 parts of defoaming agent, 32 parts of 30% formaldehyde solution, sufficient alcohol substance and sufficient n-hexane;
step two: the adhesive is prepared by the following specific steps:
s1: preparing a matrix, adding sufficient n-hexane into a reaction kettle A as a solvent, and then synchronously adding the following raw materials in mass fraction into the reaction kettle A: 110 parts of epoxy acrylic acid, 110 parts of polyoxypropylene diol and 2 parts of initiator, wherein the initiator is iodized salt, sulfur salt and ferrocenium salt according to the weight ratio of 1: 2: 3, introducing group zero gas with stable property into the reaction kettle A to remove oxygen in the kettle, carrying out polymerization reaction at 84 ℃, keeping for 7 hours, naturally cooling to room temperature after the time is up, then adding enough alcohol substance with stable property into the reaction kettle A, wherein the alcohol substance is one or a mixture of ethanol, propanol and butanol, and is used for taking out the precipitate generated by the polymerization reaction and drying in a vacuum environment to obtain an adhesive matrix;
s2: enhancing the viscosity, adding the adhesive matrix prepared in S1 into a stirring kettle, then synchronously adding 200 parts of deionized water and 35 parts of redispersible latex powder into the stirring kettle, keeping the temperature in the reaction kettle at 28 ℃, and uniformly stirring for 22 minutes at a stirring speed of 120 revolutions per minute to uniformly mix the mixture in the kettle to form paste, thus obtaining a material A;
s3: and (3) enhancing other properties, placing the material A obtained in the step S2 in a reaction kettle B, and adding the following raw materials in parts by weight: uniformly mixing 11 parts of curing agent, 12 parts of toughening agent, 16 parts of diluent, 6 parts of accelerator and 7 parts of coupling agent, sealing, heating to 83 ℃, and keeping the temperature for 32 minutes to obtain a material B;
s4, performing vacuum defoaming, namely adding the material B obtained in the step S3 into a planetary stirrer, adding 2 parts of defoaming agent into the device, uniformly mixing, and performing vacuum defoaming to obtain a modified resin adhesive;
s5: adding 32 parts of 30% formaldehyde solution, 2 parts of cross-linking agent, 6 parts of reinforcing agent and 4 parts of accelerating agent in parts by mass into a reaction kettle C, controlling the temperature in the reaction kettle to be 82 ℃, and stirring for 40 minutes under heat preservation, then naturally cooling to below 35 ℃, filtering and discharging to obtain the environment-friendly resin adhesive, the cross-linking agent comprises one or more of aluminum phosphate, sodium phosphate, modified starch and sodium chloride required by anti-swelling, the modified starch refers to one or more of starch deep-processing products such as starch acetate, starch phosphate, oxidized starch and dialdehyde starch, the reinforcing agent comprises one or more of melamine, polyvinyl alcohol, phthalic acid and salts thereof, and the accelerator is dicyandiamide, melamine and hexamethylenetetramine according to the weight ratio of 1: 1: 1 mixture of
Example 3:
the invention provides a preparation method of a resin adhesive, which specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely selecting the following raw materials in percentage by mass: 130 parts of epoxy acrylic acid, 130 parts of polyoxypropylene diol, 240 parts of deionized water, 40 parts of redispersible latex powder, 12 parts of curing agent, 15 parts of toughening agent, 17 parts of diluent, 7 parts of accelerator, 8 parts of coupling agent, 3 parts of initiator, 3 parts of crosslinking agent, 7 parts of reinforcing agent, 5 parts of accelerator, 3 parts of defoaming agent, 35 parts of 30% formaldehyde solution, sufficient alcohol substance and sufficient n-hexane;
step two: the adhesive is prepared by the following specific steps:
s1: preparing a matrix, adding sufficient n-hexane into a reaction kettle A as a solvent, and then synchronously adding the following raw materials in mass fraction into the reaction kettle A: 130 parts of epoxy acrylic acid, 130 parts of polypropylene oxide dihydric alcohol and 3 parts of initiator, wherein the initiator is iodized salt, sulfur salt and ferrocenium salt according to the weight ratio of 1: 2: 3, uniformly mixing the mixture, introducing a group zero gas with stable property into a reaction kettle A to remove oxygen in the kettle, carrying out polymerization reaction at 85 ℃, keeping for 8 hours, naturally cooling to room temperature after the time is up, then adding a sufficient amount of alcohol substance with stable property into the reaction kettle A, wherein the alcohol substance is one or a mixture of ethanol, propanol and butanol, and is used for taking out a precipitate generated by the polymerization reaction and drying the precipitate in a vacuum environment to obtain an adhesive matrix;
s2: enhancing the viscosity, adding the adhesive matrix prepared in S1 into a stirring kettle, then synchronously adding 240 parts of deionized water and 40 parts of redispersible latex powder into the stirring kettle, keeping the temperature in the reaction kettle at 30 ℃, and uniformly stirring for 25 minutes at a stirring speed of 120 revolutions per minute to uniformly mix the mixture in the kettle to form paste, thus obtaining a material A;
s3: and (3) enhancing other properties, placing the material A obtained in the step S2 in a reaction kettle B, and adding the following raw materials in parts by weight: uniformly mixing 13 parts of curing agent, 15 parts of toughening agent, 17 parts of diluent, 7 parts of accelerator and 8 parts of coupling agent, sealing, heating to 90 ℃, and preserving heat for 35 minutes to obtain a material B;
s4, performing vacuum defoaming, namely adding the material B obtained in the step S3 into a planetary stirrer, adding 1-5 parts of defoaming agent into the device, uniformly mixing, and performing vacuum defoaming to obtain a modified resin adhesive;
s5: adding 35 parts of 30% formaldehyde solution, 3 parts of cross-linking agent, 7 parts of reinforcing agent and 5 parts of accelerating agent in parts by mass into a reaction kettle C, controlling the temperature in the reaction kettle at 85 ℃, stirring for 45 minutes under heat preservation, naturally cooling to below 35 ℃, filtering and discharging to obtain the environment-friendly resin adhesive, the cross-linking agent comprises one or more of aluminum phosphate, sodium phosphate, modified starch and sodium chloride required by anti-swelling, the modified starch refers to one or more of starch deep-processing products such as starch acetate, starch phosphate, oxidized starch and dialdehyde starch, the reinforcing agent comprises one or more of melamine, polyvinyl alcohol, phthalic acid and salts thereof, and the accelerator is dicyandiamide, melamine and hexamethylenetetramine according to the weight ratio of 1: 1: 1 mixture of
Example 4:
the invention provides a preparation method of a resin adhesive, which specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely selecting the following raw materials in percentage by mass: 140 parts of epoxy acrylic acid, 140 parts of polyoxypropylene diol, 280 parts of deionized water, 45 parts of redispersible latex powder, 14 parts of curing agent, 18 parts of toughening agent, 18 parts of diluent, 9 parts of accelerator, 10 parts of coupling agent, 4 parts of initiator, 4 parts of crosslinking agent, 7 parts of reinforcing agent, 6 parts of accelerator, 4 parts of defoaming agent, 38 parts of 30% formaldehyde solution, sufficient alcohol substance and sufficient n-hexane;
step two: the adhesive is prepared by the following specific steps:
s1: preparing a matrix, adding sufficient n-hexane into a reaction kettle A as a solvent, and then synchronously adding the following raw materials in mass fraction into the reaction kettle A: 140 parts of epoxy acrylic acid, 140 parts of polypropylene oxide dihydric alcohol and 4 parts of initiator, wherein the initiator is iodized salt, sulfur salt and ferrocenium salt according to the weight ratio of 1: 2: 3, uniformly mixing the mixture, introducing a group zero gas with stable property into a reaction kettle A to remove oxygen in the kettle, carrying out polymerization reaction at 88 ℃, keeping for 9 hours, naturally cooling to room temperature after the time is up, then adding a sufficient amount of alcohol substance with stable property into the reaction kettle A, wherein the alcohol substance is one or a mixture of ethanol, propanol and butanol, and is used for taking out a precipitate generated by the polymerization reaction and drying in a vacuum environment to obtain an adhesive matrix;
s2: enhancing the viscosity, adding the adhesive matrix prepared in S1 into a stirring kettle, then synchronously adding 280 parts of deionized water and 45 parts of redispersible latex powder into the stirring kettle, keeping the temperature in the reaction kettle at 33 ℃, and uniformly stirring for 28 minutes at a stirring speed of 120 revolutions per minute to uniformly mix the mixture in the kettle to form paste, thus obtaining a material A;
s3: and (3) enhancing other properties, placing the material A obtained in the step S2 in a reaction kettle B, and adding the following raw materials in parts by weight: 14 parts of curing agent, 14 parts of toughening agent, 19 parts of diluent, 9 parts of accelerator and 10 parts of coupling agent, uniformly mixing, sealing, heating to 92 ℃, and preserving heat for 38 minutes to obtain a material B;
s4, performing vacuum defoaming, namely adding the material B obtained in the step S3 into a planetary stirrer, adding 4 parts of defoaming agent into the device, uniformly mixing, and performing vacuum defoaming to obtain a modified resin adhesive;
s5: adding 30 parts of 30% formaldehyde solution, 4 parts of cross-linking agent, 7 parts of reinforcing agent and 6 parts of accelerating agent in parts by mass into a reaction kettle C, controlling the temperature in the reaction kettle at 88 ℃, stirring for 55 minutes under heat preservation, naturally cooling to below 35 ℃, filtering and discharging to obtain the environment-friendly resin adhesive, the cross-linking agent comprises one or more of aluminum phosphate, sodium phosphate, modified starch and sodium chloride required by anti-swelling, the modified starch refers to one or more of starch deep-processing products such as starch acetate, starch phosphate, oxidized starch and dialdehyde starch, the reinforcing agent comprises one or more of melamine, polyvinyl alcohol, phthalic acid and salts thereof, and the accelerator is dicyandiamide, melamine and hexamethylenetetramine according to the weight ratio of 1: 1: 1 mixture of
Example 5:
the invention provides a preparation method of a resin adhesive, which specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely selecting the following raw materials in percentage by mass: 150 parts of epoxy acrylic acid, 150 parts of polyoxypropylene diol, 300 parts of deionized water, 50 parts of redispersible latex powder, 15 parts of curing agent, 20 parts of toughening agent, 20 parts of diluent, 10 parts of accelerator, 11 parts of coupling agent, 5 parts of initiator, 5 parts of crosslinking agent, 8 parts of reinforcing agent, 7 parts of accelerator, 5 parts of defoaming agent, 40 parts of 30% formaldehyde solution, sufficient alcohol substance and sufficient n-hexane;
step two: the adhesive is prepared by the following specific steps:
s1: preparing a matrix, adding sufficient n-hexane into a reaction kettle A as a solvent, and then synchronously adding the following raw materials in mass fraction into the reaction kettle A: 150 parts of epoxy acrylic acid, 150 parts of polyoxypropylene diol and 5 parts of initiator, wherein the initiator is iodized salt, sulfur salt and ferrocenium salt according to the weight ratio of 1: 2: 3, uniformly mixing the mixture, introducing a group zero gas with stable property into a reaction kettle A to remove oxygen in the kettle, carrying out polymerization reaction at 90 ℃, keeping for 10 hours, naturally cooling to room temperature after the time is up, then adding a sufficient amount of alcohol substance with stable property into the reaction kettle A, wherein the alcohol substance is one or a mixture of ethanol, propanol and butanol, and is used for taking out a precipitate generated by the polymerization reaction and drying in a vacuum environment to obtain an adhesive matrix;
s2: enhancing the viscosity, adding the adhesive matrix prepared in S1 into a stirring kettle, then synchronously adding 300 parts of deionized water and 50 parts of redispersible latex powder into the stirring kettle, keeping the temperature in the reaction kettle at 35 ℃, and uniformly stirring for 30 minutes at a stirring speed of 120 revolutions per minute to uniformly mix the mixture in the kettle to form paste, thus obtaining a material A;
s3: and (3) enhancing other properties, placing the material A obtained in the step S2 in a reaction kettle B, and adding the following raw materials in parts by weight: 15 parts of curing agent, 20 parts of toughening agent, 20 parts of diluent, 10 parts of accelerant and 11 parts of coupling agent, uniformly mixing the components, sealing, heating to 95 ℃, and preserving heat for 40 minutes to obtain a material B;
s4, performing vacuum defoaming, namely adding the material B obtained in the step S3 into a planetary stirrer, adding 5 parts of defoaming agent into the device, uniformly mixing, and performing vacuum defoaming to obtain a modified resin adhesive;
s5: adding 40 parts of 30% formaldehyde solution, 5 parts of cross-linking agent, 8 parts of reinforcing agent and 7 parts of accelerating agent in parts by mass into a reaction kettle C, controlling the temperature in the reaction kettle at 90 ℃, and stirring for 60 minutes under heat preservation, then naturally cooling to below 35 ℃, filtering and discharging to obtain the environment-friendly resin adhesive, the cross-linking agent comprises one or more of aluminum phosphate, sodium phosphate, modified starch and sodium chloride required by anti-swelling, the modified starch refers to one or more of starch deep-processing products such as starch acetate, starch phosphate, oxidized starch and dialdehyde starch, the reinforcing agent comprises one or more of melamine, polyvinyl alcohol, phthalic acid and salts thereof, and the accelerator is dicyandiamide, melamine and hexamethylenetetramine according to the weight ratio of 1: 1: 1 mixing the mixture.
The eye creams prepared in the above examples 1 to 5 were respectively applied to 90 women of 30 years old who have fine lines on their eyes, each 30 women were used as one group, the eye creams prepared in the three examples were respectively tried in three groups, and after 3 months of use, the following data were obtained:
as can be seen from the above table, the raw material mixing ratio in example 3 is moderate, the resin adhesive prepared by the method has an obvious effect in the using process, volatilization of harmful substances such as formaldehyde in the resin adhesive can be greatly reduced, the epoxy resin is further modified by the added modified starch and ester substances and aldehyde substances contained in the starch, the use of the harmful substances is reduced while the adhesive property of the adhesive is enhanced, and pollution is reduced from the fundamental perspective, so that the environmental protection degree is improved.
And finally: the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (7)
1. A preparation method of a resin adhesive is characterized by comprising the following steps: the method specifically comprises the following steps:
the method comprises the following steps: preparing raw materials, namely selecting the following raw materials in percentage by mass: 100-150 parts of epoxy acrylic acid, 100-150 parts of polyoxypropylene diol, 150-300 parts of deionized water, 30-50 parts of redispersible latex powder, 10-15 parts of curing agent, 10-20 parts of toughening agent, 15-20 parts of diluent, 5-10 parts of accelerator, 6-11 parts of coupling agent, 1-5 parts of initiator, 1-5 parts of crosslinking agent, 5-8 parts of reinforcing agent, 3-7 parts of accelerator, 1-5 parts of defoaming agent, 30-40 parts of 30% formaldehyde solution, sufficient alcohol substances and sufficient n-hexane;
step two: the adhesive is prepared by the following specific steps:
s1: preparing a matrix, adding sufficient n-hexane into a reaction kettle A as a solvent, and then synchronously adding the following raw materials in mass fraction into the reaction kettle A: 100-150 parts of epoxy acrylic acid, 100-150 parts of polyoxypropylene diol and 1-5 parts of initiator, introducing a group zero gas with stable property into a reaction kettle A to remove oxygen in the kettle, carrying out polymerization reaction at 80-90 ℃, keeping for 6-10 hours, naturally cooling to room temperature after the time is up, then adding sufficient alcohol substances with stable property into the reaction kettle A, taking out precipitates generated by the polymerization reaction, and drying in a vacuum environment to obtain an adhesive matrix;
s2: enhancing the viscosity, adding the adhesive matrix prepared by S1 into a stirring kettle, then synchronously adding 150-300 parts of deionized water and 30-50 parts of redispersible latex powder into the stirring kettle, keeping the temperature in the reaction kettle at 25-35 ℃, and uniformly stirring for 20-30 minutes to uniformly mix the mixture in the kettle to be pasty to obtain a material A;
s3: and (3) enhancing other properties, placing the material A obtained in the step S2 in a reaction kettle B, and adding the following raw materials in parts by weight: 10-15 parts of curing agent, 10-20 parts of toughening agent, 15-20 parts of diluent, 5-10 parts of accelerator and 6-11 parts of coupling agent, uniformly mixing, sealing, heating to 80-95 ℃, and preserving heat for 30-40 minutes to obtain a material B;
s4, performing vacuum defoaming, namely adding the material B obtained in the step S3 into a planetary stirrer, adding 1-5 parts of defoaming agent into the device, uniformly mixing, and performing vacuum defoaming to obtain a modified resin adhesive;
s5: and (2) performing environment-friendly modification, namely adding 30-40 parts of 30% formaldehyde solution, 1-5 parts of cross-linking agent, 5-8 parts of reinforcing agent and 3-7 parts of accelerating agent in parts by mass into the reaction kettle C, controlling the temperature in the reaction kettle to be 80-90 ℃, preserving heat, stirring for 30-60 minutes, naturally cooling to below 35 ℃, filtering and discharging to obtain the environment-friendly resin adhesive.
2. The method of claim 1, wherein: in the second step S1, the initiator is iodized salt, sulfur salt and ferrocenium salt according to the weight ratio of 1: 2: 3, mixing the mixture evenly, wherein the alcohol substance with stable property is one or a mixture of ethanol, propanol and butanol.
3. The method of claim 1, wherein: in the second step S2, the toughening agent is liquid silicone rubber and polyurethane according to the weight ratio of 1: 3 and the stirring rate of the stirrer in the second step S2 is 120 revolutions per minute.
4. The method of claim 1, wherein: the cross-linking agent comprises one or more of aluminum phosphate, sodium phosphate, modified starch and sodium chloride required for resisting swelling.
5. The method of claim 1, wherein: the modified starch refers to one or more of starch deep-processing products such as starch acetate, starch phosphate, oxidized starch and dialdehyde starch.
6. The method of claim 1, wherein: the reinforcing agent comprises one or more of melamine, polyvinyl alcohol, phthalic acid and salts thereof.
7. The method of claim 1, wherein: the accelerator is dicyandiamide, melamine and hexamethylenetetramine according to the weight ratio of 1: 1: 1 mixing the mixture.
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