CN115368864B - Water-based jigsaw for cork and preparation method thereof - Google Patents

Water-based jigsaw for cork and preparation method thereof Download PDF

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CN115368864B
CN115368864B CN202210646244.1A CN202210646244A CN115368864B CN 115368864 B CN115368864 B CN 115368864B CN 202210646244 A CN202210646244 A CN 202210646244A CN 115368864 B CN115368864 B CN 115368864B
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polyvinyl alcohol
emulsion
parts
mass ratio
modified
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CN115368864A (en
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方珍英
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Youxing Shark Shanghai Technology Co ltd
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Youxing Shark Shanghai Technology Co ltd
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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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • 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
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • 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
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention relates to the field of C09J131/04, in particular to an aqueous jigsaw for cork and a preparation method thereof. The invention relates to a preparation raw material of an aqueous plate-splicing glue for cork, which comprises a main agent and a curing agent, wherein the preparation raw material of the main agent at least comprises the following components in parts by weight: 30-50 parts of polyvinyl alcohol solution, 60-100 parts of emulsion composition, 20-40 parts of inorganic filler, 2-5 parts of auxiliary agent and 6-10 parts of water. By controlling the mass ratio of the polyvinyl alcohol solution, the emulsion composition and the inorganic filler in the system, the cohesive strength, the adhesive property and the high temperature resistance of the laminating adhesive are improved, the product quality and the comprehensive performance of the laminating adhesive are improved, the practical application requirement of cork splicing is met, the provided water-based laminating adhesive is resistant to boiling at 100 ℃ for 4 hours and does not break, and the laminating adhesive is continuously baked in a baking oven at 60 ℃ for 18 hours.

Description

Water-based jigsaw for cork and preparation method thereof
Technical Field
The invention relates to the field of C09J131/04, in particular to an aqueous jigsaw for cork and a preparation method thereof.
Background
Along with the continuous development of furniture manufacturing industry and home decoration industry, the market demand of the plate-splicing glue is increasing, but most wood enterprises use imported plate-splicing glue at present, and the price is high.
CN112778941 a discloses a two-component jigsaw glue which can be placed for a long time and can be placed for a long time in an opening way, but the jigsaw glue foams when meeting water, so that the adhesive capacity is reduced, the water resistance is poor, and the resource loss is high.
CN104479596 a discloses a glue for splicing plates which does not contain formaldehyde and has better environmental protection performance, and by adding thixotropic agent, the agglomeration among particles is reduced, and the mechanical performance of the glue for splicing plates is enhanced, but the water resistance, the high temperature resistance and the storage stability are poor.
Disclosure of Invention
In order to solve the problems, the invention discloses an aqueous jigsaw puzzle for cork, which comprises a main agent and a curing agent, wherein the main agent is prepared from the following raw materials in parts by weight: 30-50 parts of polyvinyl alcohol solution, 60-100 parts of emulsion composition, 20-40 parts of inorganic filler, 2-5 parts of auxiliary agent and 6-10 parts of water.
As a preferable technical scheme, the mass ratio of the polyvinyl alcohol solution, the emulsion composition and the inorganic filler is (30-40): (70-90): (20-30).
Based on the system of the invention, the mass ratio of the polyvinyl alcohol solution, the emulsion composition and the inorganic filler in the system is controlled to be (30-40): (70-90): (20-30), at the moment, the stability of the system is higher, the cohesive strength is increased, the adhesive property and the high temperature resistance are good, the product quality and the comprehensive performance of the jigsaw glue are ensured, and the inventor finds that the addition amount of the polyvinyl alcohol solution and the inorganic filler is too high in the research process, so that the synergistic cooperation effect of the emulsion composition is seriously affected, the viscosity of the system is obviously increased, the construction difficulty is increased, the stability of the system is reduced, and the service life of the jigsaw glue is shortened.
The content of polyvinyl alcohol in the polyvinyl alcohol solution is 15-25wt%.
The preparation method of the polyvinyl alcohol solution comprises the following steps: the temperature is controlled to be 80-90 ℃, and the polyvinyl alcohol is added into deionized water to be completely dissolved, so that the polyvinyl alcohol solution with the mass concentration of 15-25% is obtained.
Further, the polyvinyl alcohol includes polyvinyl alcohol and modified polyvinyl alcohol.
Further, the mass ratio of the polyvinyl alcohol to the modified polyvinyl alcohol is (3-6): (1-3).
Further, the modified polyvinyl alcohol is one or more selected from alkyl phosphoric acid modified polyvinyl alcohol, succinic acid modified polyvinyl alcohol, crotonaldehyde modified polyvinyl alcohol, nano silicon dioxide modified polyvinyl alcohol, maleic modified polyvinyl alcohol, epoxy resin modified polyvinyl alcohol and sulfonic monomer modified polyvinyl alcohol
In a preferred embodiment, the modified polyvinyl alcohol is a combination of succinic acid modified polyvinyl alcohol and crotonaldehyde modified polyvinyl alcohol.
Further, the mass ratio of the succinic acid modified polyvinyl alcohol to the crotonaldehyde modified polyvinyl alcohol is (1-2): (3-5)
Based on the system of the invention, the hydrophilic polyvinyl alcohol is adopted to be matched with the modified polyvinyl alcohol, and the mass ratio of the polyvinyl alcohol to the modified polyvinyl alcohol is controlled to be (3-6): (1-3) to effectively improve the mechanical property and the water resistance of the laminating adhesive, and the inventor unexpectedly discovers that especially when the modified polyvinyl alcohol is prepared by the following components in mass ratio (1-2): when the succinic acid modified polyvinyl alcohol and the crotonaldehyde modified polyvinyl alcohol are combined, the provided jigsaw glue has excellent bonding strength and water resistance, and meets the practical use requirement of cork jigsaw glue. The polyvinyl alcohol solution in the system is a stable composite system of polyvinyl alcohol, succinic acid modified polyvinyl alcohol and crotonaldehyde modified polyvinyl alcohol, the irregularity degree of the polyvinyl alcohol molecular chain in the system is increased, the crystallinity of the polyvinyl alcohol is reduced, active groups in the polyvinyl alcohol solution interact with the emulsion composition and the inorganic filler in the system to form a multi-molecular association network system, the cohesive force of the system is effectively improved, and the impact resistance, the adhesive force performance, the adhesive strength and the water resistance of the jigsaw glue are remarkably improved. In addition, the inventor finds that when the content of the polyvinyl alcohol in the system is too high, the viscosity of the system is obviously increased, the construction difficulty is increased, the curing time is prolonged, cohesive failure of the jigsaw glue in the bonding process is caused, the curing effect is poor, and the practical application requirement of the cork jigsaw glue cannot be met.
The inorganic filler is one or more of nano calcium carbonate, silicon micropowder and nano calcium.
Further, the inorganic filler is a combination of nano calcium carbonate and silicon micropowder.
Further, the mass ratio of the nano calcium carbonate to the silicon micropowder is (1-2): (0.8-1.8).
In a preferred scheme, the mass ratio of the nano calcium carbonate to the silicon micropowder is 1.5:1.2.
further, the median particle diameter of the silicon micropowder is 7-26 mu m, and the particle diameter of the nano calcium carbonate is 50-100 nanometers.
In a preferred scheme, the median particle size of the silicon micro powder is 7-13 mu m, the particle size of the nano calcium carbonate is 80nm, the model of the silicon micro powder is BG-1000, the silicon micro powder is purchased from Huzhou Baozhi electrical materials, inc., and the nano calcium carbonate is purchased from Zhejiang Changshan Jin Xiong, inc.
Based on the system of the invention, the mass ratio is (1-2): (0.8-1.8) as inorganic filler, effectively controlling the rheological property of the system, optimizing the processing condition of the jigsaw, reducing the production cost, particularly adopting the silicon micropowder with the median particle diameter of 7-13 μm and the nano calcium carbonate with the particle diameter of 80nm to be uniformly dispersed in a polymer matrix, so that the provided jigsaw has excellent bonding strength, the inventor speculates that the reason is probably that the nano calcium carbonate with the small particle diameter and the silicon micropowder with the large particle diameter in the system are uniformly dispersed in the polymer matrix, effectively controlling the rheological property of the system, optimizing the processing condition of the jigsaw, playing the role of effective filling and reducing the cost of polymer raw materials; meanwhile, the nano calcium carbonate and the silicon micropowder interact with active groups in the polymer structure to form a stable multi-molecule association network system, so that the bonding strength of the jigsaw is effectively improved.
The preparation method of the succinic acid modified polyvinyl alcohol comprises the following steps: placing 56mL of PVA aqueous solution with mass concentration of 5-10% into a three-neck flask with a mechanical stirrer and a reflux condensing device, controlling the temperature to be 80-85 ℃, adding 8-12mL of succinic acid, stirring under a closed condition to react, and cooling to room temperature to obtain the aqueous solution;
the preparation method of the butenal modified polyvinyl alcohol comprises the following steps: placing 150-250mL of PVA aqueous solution with mass concentration of 5-10% into a three-neck flask equipped with a mechanical stirrer and a reflux condensing device, slowly and dropwise adding 0.5-1.5mL of concentrated hydrochloric acid while stirring at room temperature, fully and uniformly mixing, heating to 88-92 ℃, adding 1.0-1.5mL of crotonaldehyde and 3-5mL of acetaldehyde, and fully stirring for reacting for 3.5-4h to obtain the aqueous solution.
The emulsion composition at least comprises one or more of pure acrylic emulsion, vinyl acetate-ethylene copolymer emulsion, aqueous polyurethane emulsion, chloroprene rubber emulsion, SBS emulsion and modified rosin resin emulsion.
Further, the emulsion composition comprises an ethylene acetate-ethylene copolymer emulsion, an aqueous polyurethane emulsion and a modified rosin resin emulsion.
Further, the mass ratio of the vinyl acetate-ethylene copolymer emulsion, the aqueous polyurethane emulsion and the modified rosin resin emulsion is (1.8-2.5): (2-3): (0.8-1.5).
The modified rosin resin emulsion is selected from one or a combination of a plurality of polymerized rosin resin emulsion, hydrogenated rosin glyceride emulsion, modified rosin pentaerythritol ester emulsion and phenolic rosin resin emulsion.
Further, the modified rosin resin emulsion is a combination of a polymerized rosin resin emulsion, a hydrogenated rosin glyceride emulsion and a modified rosin pentaerythritol ester emulsion.
Further, the mass ratio of the polymerized rosin resin emulsion, the hydrogenated rosin glyceride emulsion and the modified rosin pentaerythritol ester emulsion is (1-3): (2-4): (4-6) the model of the polymerized rosin resin emulsion was AP9125, the model of the modified rosin pentaerythritol ester emulsion was AP9115, both purchased from Guangdong Weis Data New Material Co., ltd, and the model of the hydrogenated rosin glycerol ester emulsion was SBR8118.
The emulsion composition is used as a main function realization material of the panel glue, and has great influence on the adhesive property, high temperature resistance and solidification property of the product. The inventor finds that in the research process, an emulsion composition comprising an ethylene acetate-ethylene copolymer emulsion, a water-based polyurethane emulsion and a modified rosin resin emulsion is adopted in a system, and particularly the mass ratio of the ethylene acetate-ethylene copolymer emulsion, the water-based polyurethane emulsion and the modified rosin resin emulsion is controlled to be (1.8-2.5): (2-3): (0.8-1.5), the system has higher stability, so that the prepared jigsaw glue has excellent flexibility and bonding performance and simultaneously endows the jigsaw glue with excellent high temperature resistance. The inventors analyzed the cause may be: under the mass ratio, the modified rosin resin emulsion in the system exists, so that the compatibility between the aqueous polyurethane emulsion and the vinyl acetate-ethylene copolymer emulsion is effectively improved, the problem of poor system stability caused by concentrated aggregation due to charge effect between polymer emulsions is avoided, the combined action of the vinyl acetate-ethylene copolymer emulsion and the aqueous polyurethane emulsion is promoted, the prepared jigsaw has excellent flexibility and bonding performance, and meanwhile, the excellent high temperature resistance is provided for the jigsaw. The inventors have unexpectedly found during the exploration that when the mass ratio of the modified rosin resin emulsion in the system is (1-3): (2-4): when the polymerized rosin resin emulsion, the hydrogenated rosin glyceride emulsion and the modified rosin pentaerythritol ester emulsion are combined, on one hand, the pH of the system is controlled to be in a proper range, the problem that the water-based polyurethane emulsion cannot fully play a role due to the pH reduction caused by the existence of the vinyl acetate-ethylene copolymer emulsion in the system is avoided, and the stability of the system and the flexibility and the adhesive property of the product are ensured; on the other hand, the polymerized rosin resin emulsion, the hydrogenated rosin glyceride emulsion and the modified rosin pentaerythritol ester emulsion can play a synergistic compounding role, so that the jigsaw glue is endowed with higher cohesive force and heat-resistant strength, and the jigsaw glue provided is boiled in water at 100 ℃ for 4 hours after being used for bonding cork, and is baked in a baking oven at 60 ℃ for 18 hours without glue opening. And when the content of the modified rosin resin emulsion is too high, the vinyl acetate-ethylene copolymer emulsion in the system is hydrolyzed, so that the comprehensive performance of the jigsaw rubber is seriously affected.
In addition, as a preferable technical scheme, the auxiliary agent at least comprises an antifoaming agent, a preservative and a silane coupling agent, and the mass ratio is (0.5-1): (0.1-0.8): (1-1.5).
The defoaming agent is an organosilicon defoaming agent or a silicone defoaming agent.
The preparation method of the water-based panel glue for cork comprises at least the following steps:
(1) Stirring and mixing the emulsion composition, the inorganic filler and the auxiliary agent at 800-1000rpm for 50-60min to obtain a mixture A;
(2) Controlling the rotating speed to be 100-200rpm, mixing the mixture A with the polyvinyl alcohol solution and water for 20-40min, performing spot check and filtering to obtain a main agent;
(3) The mass ratio of the main agent to the curing agent is 100: (8-12), uniformly mixing the main agent and the curing agent to obtain the adhesive;
the curing agent is one or a combination of more of isocyanate curing agent, aziridine curing agent and polyethyleneimine curing agent.
The beneficial effects are that:
1. according to the system, the hydrophilic polyvinyl alcohol is adopted to be matched with the modified polyvinyl alcohol, so that the mechanical property and the water resistance of the jigsaw glue are effectively improved, and the problem that the adhesive is reduced in bonding capacity and high in resource loss due to foaming of the adhesive when meeting water is avoided.
2. According to the system, the mass ratio of the vinyl acetate-ethylene copolymer emulsion, the aqueous polyurethane emulsion and the modified rosin resin emulsion is controlled, so that the system has higher stability, and the jigsaw has excellent flexibility and bonding performance and simultaneously has excellent high-temperature resistance.
3. According to the system, the mass ratio of the polymerized rosin resin emulsion, the hydrogenated rosin glyceride emulsion and the modified rosin pentaerythritol ester emulsion is controlled, so that the synergistic compounding effect is exerted, and the high cohesive force and the high heat-resistant strength of the jigsaw glue are endowed.
4. According to the system, the mass ratio of the polyvinyl alcohol solution, the emulsion composition and the inorganic filler in the system is controlled, so that the cohesive strength is improved, the adhesive property and the high temperature resistance are good, and the product quality and the comprehensive performance of the jigsaw glue are improved.
5. The water-based plate-splicing adhesive meets the practical application requirement of cork splicing, is resistant to boiling at 100 ℃ for 4 hours without glue opening, and is continuously baked in a baking oven at 60 ℃ for 18 hours without glue opening.
Detailed Description
Example 1
The embodiment 1 of the invention discloses an aqueous jigsaw for cork, which comprises a main agent and a curing agent, wherein the main agent comprises the following preparation raw materials in parts by weight: 30 parts of polyvinyl alcohol solution, 70 parts of emulsion composition, 20 parts of inorganic filler, 2 parts of auxiliary agent and 6 parts of water.
The curing agent is isocyanate curing agent, and is purchased from Fujian Union blueprint material technology limited, and the model is Aquolin166.
The emulsion composition comprises an acetic acid ethylene-ethylene copolymer emulsion, a water-based polyurethane emulsion and a modified rosin resin emulsion.
The mass ratio of the vinyl acetate-ethylene copolymer emulsion, the aqueous polyurethane emulsion and the modified rosin resin emulsion is 1.8:2:0.8.
the modified rosin resin emulsion is a combination of polymerized rosin resin emulsion, hydrogenated rosin glyceride emulsion and modified rosin pentaerythritol ester emulsion.
The mass ratio of the polymerized rosin resin emulsion to the hydrogenated rosin glyceride emulsion to the modified rosin pentaerythritol ester emulsion is 1:2:4.
the model of the polymerized rosin resin emulsion is AP9125, the model of the modified rosin pentaerythritol ester emulsion is AP9115, and the modified rosin pentaerythritol ester emulsion is purchased from Guangdong Weis Danew material Co. The model of the hydrogenated rosin glyceride emulsion is SBR8118.
The inorganic filler is a combination of nano calcium carbonate and silicon micropowder, and the mass ratio is 1:0.8.
the model of the silicon micro powder is BG-1000, the silicon micro powder is purchased from Huzhou Baozhi electrical materials, inc., and the nano calcium carbonate is purchased from Zhejiang Changshan Jin Xiong, inc.
The content of polyvinyl alcohol in the polyvinyl alcohol solution is 15wt%.
The preparation method of the polyvinyl alcohol solution comprises the following steps: the temperature is controlled to be 80 ℃, and polyvinyl alcohol is added into deionized water to be completely dissolved, so that a polyvinyl alcohol solution with the mass concentration of 15% is obtained.
The polyvinyl alcohol comprises polyvinyl alcohol and modified polyvinyl alcohol, and the mass ratio is 3:3.
the modified polyvinyl alcohol is a combination of succinic acid modified polyvinyl alcohol and crotonaldehyde modified polyvinyl alcohol, and the mass ratio is 1:5.
the preparation method of the succinic acid modified polyvinyl alcohol comprises the following steps: putting 56mL of PVA aqueous solution with mass concentration of 5% into a three-neck flask with a mechanical stirrer and a reflux condensing device, controlling the temperature to be 80 ℃, adding 8mL of succinic acid, stirring under a closed condition to react, and cooling to room temperature to obtain the aqueous solution;
the preparation method of the butenal modified polyvinyl alcohol comprises the following steps: 150mL of PVA aqueous solution with mass concentration of 5% is placed into a three-neck flask equipped with a mechanical stirrer and a reflux condensing device, 0.5mL of concentrated hydrochloric acid is slowly added dropwise under stirring at room temperature, the mixture is fully and uniformly mixed, then the temperature is raised to 88 ℃, 1.0mL of butenal and 3mL of acetaldehyde are added, and the mixture is fully stirred for 3.5h to obtain the PVA aqueous solution.
The auxiliary agent comprises 0.5 part of defoamer, 0.1 part of preservative and 1 part of silane coupling agent.
The defoaming agent is an organic silicon defoaming agent, and is purchased from the Hengxin chemical industry Co., ltd, and the model is THIX-278.
The preservative was purchased from Shanghai Seisakusho materials science, inc., model number CI802.
The silane coupling agent is purchased from Shandong Haiyou organosilicon science and technology Co., ltd, and the model is KH570.
The embodiment 1 of the invention also discloses a preparation method of the water-based jigsaw for cork, which comprises the following steps:
(1) Stirring and mixing 70 parts of emulsion composition, 20 parts of inorganic filler and 2 parts of auxiliary agent at 800rpm for 50min to obtain a mixture A;
(2) Controlling the rotating speed to be 100rpm, mixing the mixture A with 30 parts of polyvinyl alcohol solution and 6 parts of water for 20min, performing spot check and filtering to obtain a main agent;
(3) The mass ratio of the main agent to the curing agent is 100: and 8, uniformly mixing the main agent and the curing agent to obtain the adhesive.
Example 2
The embodiment 2 of the invention discloses an aqueous jigsaw for cork, which comprises a main agent and a curing agent, wherein the main agent comprises the following preparation raw materials in parts by weight: 40 parts of polyvinyl alcohol solution, 90 parts of emulsion composition, 30 parts of inorganic filler, 5 parts of auxiliary agent and 10 parts of water.
The curing agent is isocyanate curing agent, and is purchased from Fujian Union blueprint material technology limited, and the model is Aquolin166.
The emulsion composition comprises an acetic acid ethylene-ethylene copolymer emulsion, a water-based polyurethane emulsion and a modified rosin resin emulsion.
The mass ratio of the vinyl acetate-ethylene copolymer emulsion, the aqueous polyurethane emulsion and the modified rosin resin emulsion is 2.5:3:1.5.
the modified rosin resin emulsion is a combination of polymerized rosin resin emulsion, hydrogenated rosin glyceride emulsion and modified rosin pentaerythritol ester emulsion.
The mass ratio of the polymerized rosin resin emulsion to the hydrogenated rosin glyceride emulsion to the modified rosin pentaerythritol ester emulsion is 3:4:6.
the model of the polymerized rosin resin emulsion is AP9125, the model of the modified rosin pentaerythritol ester emulsion is AP9115, and the modified rosin pentaerythritol ester emulsion is purchased from Guangdong Weis Danew material Co. The model of the hydrogenated rosin glyceride emulsion is SBR8118.
The inorganic filler is a combination of nano calcium carbonate and silicon micropowder, and the mass ratio is 2:1.8.
the model of the silicon micro powder is BG-1000, the silicon micro powder is purchased from Huzhou Baozhi electrical materials, inc., and the nano calcium carbonate is purchased from Zhejiang Changshan Jin Xiong, inc.
The polyvinyl alcohol content in the polyvinyl alcohol solution was 25wt%.
The preparation method of the polyvinyl alcohol solution comprises the following steps: the temperature is controlled to be 90 ℃, and polyvinyl alcohol is added into deionized water to be completely dissolved, so that a polyvinyl alcohol solution with the mass concentration of 25% is obtained.
The polyvinyl alcohol comprises polyvinyl alcohol and modified polyvinyl alcohol, and the mass ratio is 6:1.
the modified polyvinyl alcohol is a combination of succinic acid modified polyvinyl alcohol and crotonaldehyde modified polyvinyl alcohol, and the mass ratio is 2:3.
the preparation method of the succinic acid modified polyvinyl alcohol comprises the following steps: putting 56mL of PVA aqueous solution with mass concentration of 10% into a three-neck flask with a mechanical stirrer and a reflux condensing device, controlling the temperature to be 85 ℃, adding 12mL of succinic acid, stirring under a closed condition to react, and cooling to room temperature to obtain the aqueous solution;
the preparation method of the butenal modified polyvinyl alcohol comprises the following steps: 250mL of PVA aqueous solution with the mass concentration of 10% is placed into a three-neck flask provided with a mechanical stirrer and a reflux condensing device, 1.5mL of concentrated hydrochloric acid is slowly added dropwise under the condition of room temperature while stirring, the mixture is fully and uniformly mixed, then the temperature is raised to 92 ℃, 1.5mL of butenal and 5mL of acetaldehyde are added, and the mixture is fully stirred for 4 hours to obtain the PVA aqueous solution.
The auxiliary agent comprises 1 part of defoaming agent, 0.8 part of preservative and 1.5 parts of silane coupling agent.
The defoaming agent is an organic silicon defoaming agent, and is purchased from the Hengxin chemical industry Co., ltd, and the model is THIX-278.
The preservative was purchased from Shanghai Seisakusho materials science, inc., model number CI802.
The silane coupling agent is purchased from Shandong Haiyou organosilicon science and technology Co., ltd, and the model is KH570.
The embodiment 2 of the invention also discloses a preparation method of the water-based jigsaw for cork, which comprises the following steps:
(1) Mixing 90 parts of emulsion composition, 30 parts of inorganic filler and 5 parts of auxiliary agent under stirring at 1000rpm for 60min to obtain a mixture A;
(2) Controlling the rotating speed to be 200rpm, mixing the mixture A with 40 parts of polyvinyl alcohol solution and 10 parts of water for 40min, performing spot check and filtering to obtain a main agent;
(3) The mass ratio of the main agent to the curing agent is 100: and 12, uniformly mixing the main agent and the curing agent to obtain the modified epoxy resin.
Example 3
The embodiment 3 of the invention discloses an aqueous jigsaw for cork, which comprises a main agent and a curing agent, wherein the main agent comprises the following preparation raw materials in parts by weight: 35 parts of polyvinyl alcohol solution, 80 parts of emulsion composition, 25 parts of inorganic filler, 4 parts of auxiliary agent and 8 parts of water.
The curing agent is isocyanate curing agent, and is purchased from Fujian Union blueprint material technology limited, and the model is Aquolin166.
The emulsion composition comprises an acetic acid ethylene-ethylene copolymer emulsion, a water-based polyurethane emulsion and a modified rosin resin emulsion.
The mass ratio of the vinyl acetate-ethylene copolymer emulsion, the aqueous polyurethane emulsion and the modified rosin resin emulsion is 2:2.5:1.3.
the modified rosin resin emulsion is a combination of polymerized rosin resin emulsion, hydrogenated rosin glyceride emulsion and modified rosin pentaerythritol ester emulsion.
The mass ratio of the polymerized rosin resin emulsion to the hydrogenated rosin glyceride emulsion to the modified rosin pentaerythritol ester emulsion is 2:3:5.
the model of the polymerized rosin resin emulsion is AP9125, the model of the modified rosin pentaerythritol ester emulsion is AP9115, and the modified rosin pentaerythritol ester emulsion is purchased from Guangdong Weis Danew material Co. The model of the hydrogenated rosin glyceride emulsion is SBR8118.
The inorganic filler is a combination of nano calcium carbonate and silicon micropowder, and the mass ratio of the inorganic filler is 1.5:1.4.
the model of the silicon micro powder is BG-1000, the silicon micro powder is purchased from Huzhou Baozhi electrical materials, inc., and the nano calcium carbonate is purchased from Zhejiang Changshan Jin Xiong, inc.
The content of polyvinyl alcohol in the polyvinyl alcohol solution is 20wt%.
The preparation method of the polyvinyl alcohol solution comprises the following steps: the temperature is controlled to be 85 ℃, and the polyvinyl alcohol is added into deionized water to be completely dissolved, so that the polyvinyl alcohol solution with the mass concentration of 20% is obtained.
The polyvinyl alcohol comprises polyvinyl alcohol and modified polyvinyl alcohol, and the mass ratio is 4.5:2.
the modified polyvinyl alcohol is a combination of succinic acid modified polyvinyl alcohol and crotonaldehyde modified polyvinyl alcohol, and the mass ratio is 1.5:4.
the preparation method of the succinic acid modified polyvinyl alcohol comprises the following steps: putting 56mL of PVA aqueous solution with mass concentration of 8% into a three-neck flask with a mechanical stirrer and a reflux condensing device, controlling the temperature to 82 ℃, adding 10mL of succinic acid, stirring under a closed condition to react, and cooling to room temperature to obtain the aqueous solution;
the preparation method of the butenal modified polyvinyl alcohol comprises the following steps: 200mL of PVA aqueous solution with mass concentration of 8% is placed into a three-neck flask equipped with a mechanical stirrer and a reflux condensing device, 1mL of concentrated hydrochloric acid is slowly added dropwise under stirring at room temperature, the mixture is fully and uniformly mixed, then the temperature is raised to 90 ℃, 1.2mL of butenal and 4mL of acetaldehyde are added, and the mixture is fully stirred and reacted for 3.7h to obtain the PVA aqueous solution.
The auxiliary agent comprises 0.8 part of defoamer, 0.3 part of preservative and 1.2 parts of silane coupling agent.
The defoaming agent is an organic silicon defoaming agent, and is purchased from the Hengxin chemical industry Co., ltd, and the model is THIX-278.
The preservative was purchased from Shanghai Seisakusho materials science, inc., model number CI802.
The silane coupling agent is purchased from Shandong Haiyou organosilicon science and technology Co., ltd, and the model is KH570.
The embodiment 3 of the invention also discloses a preparation method of the water-based jigsaw for cork, which at least comprises the following steps:
(1) Stirring and mixing 80 parts of emulsion composition, 25 parts of inorganic filler and 4 parts of auxiliary agent at 900rpm for 55min to obtain a mixture A;
(2) Controlling the rotating speed to be 150rpm, mixing the mixture A with 35 parts of polyvinyl alcohol solution and 8 parts of water for 30min, performing spot check and filtering to obtain a main agent;
(3) The mass ratio of the main agent to the curing agent is 100: and 10, uniformly mixing the main agent and the curing agent to obtain the adhesive.
Comparative example 1
The content of polyvinyl alcohol in the polyvinyl alcohol solution is 30wt%; the mass ratio of the polyvinyl alcohol to the modified polyvinyl alcohol is 8:1, a step of; the mass ratio of the succinic acid modified polyvinyl alcohol to the crotonaldehyde modified polyvinyl alcohol is 1:6, the remainder being the same as in example 3.
Comparative example 2
The mass ratio of the polymerized rosin resin emulsion to the hydrogenated rosin glyceride emulsion to the modified rosin pentaerythritol ester emulsion is 5:1:3, the remainder being the same as in example 3.
Comparative example 3
The mass ratio of the nano calcium carbonate to the silicon micropowder is 3:2, the remainder being the same as in example 3.
Comparative example 4
The preparation method of the water-based jigsaw for cork comprises the following steps:
(1) 60 parts of emulsion composition, 40 parts of inorganic filler and 4 parts of auxiliary agent are stirred and mixed for 55min at 900rpm to obtain a mixture A;
(2) Controlling the rotating speed to be 150rpm, mixing the mixture A with 20 parts of polyvinyl alcohol solution and 8 parts of water for 30min, performing spot check and filtering to obtain a main agent;
(3) The mass ratio of the main agent to the curing agent is 100: and 10, uniformly mixing the main agent and the curing agent to obtain the modified polyurethane foam, wherein the rest is the same as the embodiment 3.
Performance test:
the performance test was carried out on the aqueous laminating adhesives prepared in examples 1 to 3 and comparative examples 1 to 4 by using a standard cork board with a flat and uniform surface of 10X 5cm as a test base material:
(1) And (3) glue quality detection: coating the water-based jigsaw glue on a substrate, wherein the glue distribution amount is 200g/m 2 Bonding and standing for 2min.
A) Boiling resistance test: placing the mixture in water at 100 ℃ for 4 hours, wherein the mixture is qualified if the mixture is not boiled, and if the mixture is boiled for 4 hours, the mixture is unqualified;
b) High temperature resistance test: boiling in water at 100 ℃ for 4 hours, and then placing in a baking oven at 60 ℃ for baking for 18 hours, and if the baking is carried out for 18 hours without glue spreading, the jigsaw is qualified; if the glue is opened after baking for 18 hours, the jigsaw glue is unqualified, and the result is shown in the following table:
(2) Bond strength: the aqueous plate-making adhesives prepared in examples 1 to 3 and comparative examples 1 to 4 were tested for dry compressive shear strength in accordance with the plate-making adhesive prescribed in Japanese Industrial Standard JIS K6806-1985. A: shear force >10Mpa; b:5Mpa < shear force <10Mpa; c: shear force <5Mpa. The results are tabulated below:
(3) Storage stability
Weighing 10g of main agent sample, placing into a test tube, lightly covering with a cork, placing the test tube into a constant temperature tank at 60+ -2deg.C, keeping the liquid level of the sample at about 20mm below the water tank page, recording the starting time, covering the stopper after about 10min, taking out the test tube every hour, tilting, observing fluidity until the sample is gelled or layered or becomes non-flowing, and recording the end time. A: the endpoint time is greater than 24 hours; b: endpoint time is greater than 12h and less than 24h; c: the endpoint time was less than 12 hours. The results are tabulated below.

Claims (3)

1. The water-based jigsaw for cork is characterized by comprising a main agent and a curing agent, wherein the main agent is prepared from the following raw materials in parts by weight: 30-50 parts of polyvinyl alcohol solution, 60-100 parts of emulsion composition, 20-40 parts of inorganic filler, 2-5 parts of auxiliary agent and 6-10 parts of water; the content of polyvinyl alcohol in the polyvinyl alcohol solution is 15-25wt%; the polyvinyl alcohol comprises polyvinyl alcohol and modified polyvinyl alcohol; the mass ratio of the polyvinyl alcohol to the modified polyvinyl alcohol is (3-6): (1-3); the modified polyvinyl alcohol is a combination of succinic acid modified polyvinyl alcohol and crotonaldehyde modified polyvinyl alcohol, and the mass ratio is (1-2): (3-5); the emulsion composition comprises vinyl acetate-ethylene copolymer emulsion, aqueous polyurethane emulsion and modified rosin resin emulsion, wherein the mass ratio of the emulsion composition to the modified rosin resin emulsion is (1.8-2.5): (2-3): (0.8-1.5); the modified rosin resin emulsion is a combination of polymerized rosin resin emulsion, hydrogenated rosin glyceride emulsion and modified rosin pentaerythritol ester emulsion, and the mass ratio is (1-3): (2-4): (4-6); the inorganic filler is the combination of nano calcium carbonate and silicon micropowder, and the mass ratio is (1-2): (0.8-1.8);
the curing agent is isocyanate curing agent.
2. The glue for splicing plates according to claim 1, wherein the median particle size of the silica micropowder is 7-26 μm, and the particle size of the nano calcium carbonate is 50-100 nm.
3. A method for preparing the water-based panel glue for cork according to claim 1 or 2, comprising at least the following steps:
(1) Stirring and mixing the emulsion composition, the inorganic filler and the auxiliary agent at 800-1000rpm for 50-60min to obtain a mixture A;
(2) Controlling the rotating speed to be 100-200rpm, mixing the mixture A with the polyvinyl alcohol solution and water for 20-40min, performing spot check and filtering to obtain a main agent;
(3) The mass ratio of the main agent to the curing agent is 100: (8-12), uniformly mixing the main agent and the curing agent.
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