CN108841346B - High-bonding-strength environment-friendly supramolecular physical gel adhesive and preparation method thereof - Google Patents
High-bonding-strength environment-friendly supramolecular physical gel adhesive and preparation method thereof Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/02—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to polysaccharides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- 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
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- 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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- 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
- C09J133/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/02—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides
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- 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
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
Abstract
An environment-friendly supramolecular physical gel adhesive with high bonding strength and a preparation method thereof belong to the technical field of water-based adhesive preparation. Dissolving nano particles in deionized water, stirring until the nano particles are completely dissolved, adding one or two monomers into the deionized water, and stirring until the nano particles are completely dissolved; dissolving an initiator in deionized water, performing ultrasonic treatment until the initiator is completely dissolved, adding an initiator solution into a prepolymerization solution containing nano particles and monomers, finally adding a catalyst, stirring, and standing at room temperature to obtain the gel adhesive. The gel adhesive is formed based on multiple weak interaction hydrogen bonds among polymers, chain entanglement and physical adsorption between nano particles and the polymers, the forming process is simple and efficient, no organic solvent is required to be added in the preparation process, no peculiar smell, no toxicity and environmental protection are realized, the used raw materials are common chemical raw materials, and the price is low. The adhesive is applied to the adhesion of various materials such as optical glass, metal, wood, plastic and the like, and has high adhesion strength.
Description
Technical Field
The invention belongs to the technical field of water-based adhesives, and particularly relates to a high-bonding-strength environment-friendly supramolecular physical gel adhesive and a preparation method thereof.
Background
Water-based adhesives are adhesives made from film-forming materials that are dispersible or soluble in water, also commonly referred to as aqueous adhesives. Wherein, the film forming material comprises organic polymer, animal glue, starch, dextrin, serum protein, albumin, methylcellulose, polyvinyl alcohol and the like, and also comprises soluble intermediates of phenolic aldehyde and novolac resin. Although some existing water-based adhesives such as adhesives, phenolic glue and urea-formaldehyde glue which are most commonly used in the artificial board industry have low cost, high bonding strength and wide application, the adhesives not only have the problems of air and water pollution and the like in the processing process, but also release carcinogenic substances such as free formaldehyde, phenol and the like in the use process, thereby causing serious threats to the environment and the health of human beings. Therefore, it is necessary to develop a new non-toxic, harmless, green and environment-friendly water-based adhesive.
The hydrogel is a high molecular material with a chemical or physical crosslinked three-dimensional network structure and containing a large amount of moisture. The polymer chains that make up the gel are capable of binding water, but the presence of the crosslinked network prevents the hydrogel from dissolving in water, allowing the gel to swell but not dissolve in water. The physical crosslinked hydrogel is a supermolecule aggregate formed on the basis of weak interaction force among molecules such as static electricity, hydrogen bonds, coordination bonds, chain entanglement and host-guest interaction, most of the supermolecule aggregate does not need to be chemically modified, so that the physical crosslinked hydrogel is low in toxicity and is particularly suitable for the field of biological medical treatment. In addition, the specific physical hydrogel has good ductility, compressibility and strong toughness, so that the physical hydrogel can well permeate into tiny cavities and pores on the surface of an adherend when being used as an adhesive, specific acting groups on the surface of the gel can act with surface groups to be bonded, and after moisture is volatilized, the gel adhesive is cured to mechanically lock the bonding material. The hydrogel is convenient to transport and store due to high viscosity and low fluidity, and the gel adhesive can be packaged in a tube for extrusion and use due to good ductility.
At present, gel adhesives which can be applied in a large scale are few, and CN105462523A discloses a method for preparing a high-adhesion-performance water-based adhesive based on a polymer compound, wherein two polymer solutions are blended to obtain a precipitated compound, and a compact high-adhesion-performance water-based gel adhesive can be obtained by centrifuging. Since the gel is the precipitate portion of the blending process, a large amount of waste water is generated and a centrifugation step is required to collect the gel binder. It is therefore significant and challenging to optimize the gel adhesive manufacturing process flow, and retain its properties of environmental protection and high bond strength.
Disclosure of Invention
The invention aims to provide a high-bonding-strength environment-friendly supramolecular physical gel adhesive and a preparation method thereof, wherein the method comprises the following steps:
1) preparation of prepolymerization solution: dissolving the nanoparticles in deionized water, and stirring for 10-50 minutes until the nanoparticles are completely dissolved, wherein the concentration is 5.0-20.0 mg/mL; adding a monomer into the solution, stirring the solution for 20 to 70 minutes until the monomer is completely dissolved, and preparing a prepolymerization solution with the monomer concentration of 7 to 15 wt%;
2) preparation of supramolecular physical gel: dissolving an initiator in deionized water, and carrying out ultrasonic treatment for 10-30 minutes until the initiator is completely dissolved to obtain a solution with the concentration of 4-18 mg/mL; adding 1-7 mL of the solution into 10-17 mL of the prepolymerization solution obtained in the step 1), finally adding a catalyst with the mass ratio of the catalyst to the initiator being 1: 10-10: 1, stirring for 3-10 minutes, and standing at room temperature for 10-20 hours to obtain the high-bonding-strength environment-friendly supramolecular physical gel adhesive.
The invention relates to a high-bonding-strength environment-friendly supramolecular physical gel adhesive which is characterized by being prepared by the method.
The nano particles used in the invention are one or more than two of graphene oxide, carbon nano tubes, montmorillonite, cellulose nanocrystals or nano carbon dots, and the particle size is 10-200 nm; the monomer is one or more than two of acrylic acid, dimethylacrylamide, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, methacrylic acid or hydroxyethyl methacrylate; when two monomers are used, the mass ratio of the two monomers is 1: 5-5: 1; the initiator is one or more than two of potassium persulfate, ammonium persulfate, azodiisobutyronitrile and ammonium ceric nitrate; the catalyst is one or more of sodium sulfite, N-dimethylcyclohexylamine, tetramethylethylenediamine and N-ethylmorpholine.
The invention provides a high-bonding-strength environment-friendly gel adhesive prepared based on supramolecular physical gel and a preparation method thereof. The preparation method is simple, and the supramolecular physical gel hydrogel can be obtained only by preparing the aqueous solution of the nano particles and the monomers, then adding the initiator and the catalyst, and carrying out static polymerization at normal temperature. The gel adhesive is formed based on multiple weak interaction hydrogen bonds among polymers, chain entanglement and physical adsorption between nano particles and the polymers, the forming process is simple and efficient, complex instruments and equipment and a large amount of manpower are not needed, an organic solvent is not needed to be added in the preparation process, no peculiar smell, no toxicity and environmental protection are realized, the used raw materials are common chemical raw materials, and the price is low. The gel adhesive can be applied to the adhesion of various materials such as optical glass, metal, wood, plastic and the like, has high adhesion strength, is convenient to use, and can be cured at normal temperature to realize adhesion only by uniformly coating the surface of a required adhesive material and pressing the adhesive surface. In addition, the adhesive has a shelf life of more than 24 months and is convenient to store. The gel adhesive prepared by the invention is expected to be applied in a wide range of fields.
Drawings
FIG. 1: the state photograph of the environment-friendly supramolecular physical gel adhesive with high bonding strength shows that the adhesive is in a transparent gel state, which corresponds to the embodiment 1;
FIG. 2: the state photograph of the small gel adhesive piece taken out of the tweezers shows that the adhesive has strong viscosity, which corresponds to example 1;
FIG. 3: a state photograph of the environment-friendly supramolecular physical gel adhesive with high bonding strength having strong bonding force on wood at normal temperature corresponds to example 1;
FIG. 4: the method is characterized in that a state photo of a 9mm thick plywood (2.6 meters long and 1.3 meters wide original board) which takes poplar sandwich skin as a raw material is prepared on a large scale by taking a high bonding strength environment-friendly supramolecular physical gel adhesive as a wood adhesive under the normal temperature condition, the plywood does not contain aldehyde, and the bonding strength reaches the strength requirement of national three types of plywood after being tested, and corresponds to example 2;
FIG. 5: the state photograph of two pieces of glass bonded by the high bonding strength environment-friendly supramolecular physical gel adhesive under the normal temperature condition corresponds to the embodiment 3;
FIG. 6: the high bonding strength environment-friendly supramolecular physical gel adhesive is applied to a tensile shear strength histogram of different substrates, corresponds to a wood block and glass from left to right in sequence, and when the high bonding strength environment-friendly supramolecular physical gel adhesive is used for bonding wood block materials, the bonding strength of the adhesive is as high as 5.1MPa, and corresponds to the embodiment 1; when the adhesive is used for bonding glass materials, the bonding strength of the adhesive is 4.3MPa corresponding to the embodiment 3;
Detailed Description
The following examples further illustrate the practice and results of the invention, but are not intended to limit the invention thereto
Example 1:
a. preparation of prepolymerization solution: 100mg of cellulose nanocrystals (particle size about 120nm) were dissolved in 15mL of deionized water, and added in a molar ratio of 1:1, stirring the dimethylacrylamide monomer and the acrylic acid monomer for 20 minutes until the monomers are completely dissolved to prepare a prepolymerization solution with the monomer concentration of 12 wt%;
b. preparation of supramolecular physical gel: b, dissolving an initiator azobisisobutyronitrile into deionized water, performing ultrasonic treatment for 10 minutes until the initiator azobisisobutyronitrile is completely dissolved into a solution with the concentration of 10mg/mL, and adding 1mL of the solution into 10mL of the prepolymerization solution obtained in the step a; finally, 30mg of N-ethylmorpholine was added as a catalyst. Stirring was stopped for 5 minutes. Standing for 20 hours to obtain the high bonding strength environment-friendly supramolecular physical gel adhesive.
Bonding of the samples: taking off a proper amount of small blocks from the prepared gel adhesive, placing the small blocks at one end of the wood chips, covering the other wood chip in parallel, wherein the bonding area is 25 mm/25 mm, applying pressure to the bonding part to enable the two wood blocks to be tightly contacted, and bonding firmly after the moisture in the gel adhesive is volatilized to dry.
The glued wood blocks were applied to lap tensile shear testing to test the bond strength of the gel adhesive. This example measured a tensile break stress of 3187N. The tensile shear strength (stress divided by bonding area) of the gel adhesive applied to the surface of the wood block is 5.1 MPa.
Example 2:
a. preparation of prepolymerization solution: dissolving 250mg of nano carbon dots (the particle size is about 50nm) in 20mL of deionized water, adding monomer acrylamide and methacrylic acid according to the molar ratio of 1:4, stirring for 20 minutes until the nano carbon dots are completely dissolved, and preparing a prepolymerization solution with the monomer concentration of 14 wt%.
b. Preparation of supramolecular physical gel: and (3) dissolving initiator ammonium ceric nitrate in deionized water, performing ultrasonic treatment for 10 minutes until the initiator ammonium ceric nitrate is completely dissolved to be a solution with the concentration of 7mg/mL, adding 2mL of the solution into 15mL of the prepolymerization solution obtained in the step (a), and finally adding 15mg of catalyst sodium persulfate. Stirring was stopped for 3 minutes. Standing for 10 hours to obtain the high bonding strength environment-friendly supramolecular physical gel adhesive.
Bonding of the samples: the prepared gel adhesive is respectively and uniformly coated on two surfaces of a plurality of poplar sandwich skins, then the poplar sandwich skins are orderly stacked together to form a composite board with a multilayer structure, a cold press is used for applying a certain pressure (10MPa) to the whole composite board to enable the poplar sandwich skins to be in close contact with each other, and after the moisture in the gel adhesive is volatilized, the multi-layer plywood with the thickness of 9mm can be firmly bonded.
The glued plywood is sent to a professional organization for testing, the requirements of the national standard GB/T9846-. The adhesive strength of the adhesive measured in the example is 1.7MPa, and the value shows that the common plywood prepared by using the gel adhesive completely meets the strength requirement (more than or equal to 0.7MPa) of three types of plywood in the national standard.
Example 3:
a. preparation of prepolymerization solution: 300mg of montmorillonite and cellulose nanocrystal (the mass ratio is 1:1, the particle size is about 30nm and 150nm respectively) are dissolved in 40mL of deionized water, hydroxyethyl methacrylate monomer is added, and the mixture is stirred for 20 minutes until the monomer is completely dissolved to prepare a prepolymerization solution with the monomer concentration of 8.5 wt%;
b. preparation of supramolecular physical gel: dissolving initiator ammonium persulfate in deionized water, performing ultrasonic treatment for 10 minutes until the initiator ammonium persulfate is completely dissolved into a solution with the concentration of 13mg/mL, and adding 3mL of the solution into 14mL of the prepolymerization solution obtained in the step a; finally, 18mg of N, N-dimethylcyclohexylamine as a catalyst was added. Stirring was stopped for 8 minutes. Standing for 15 hours to obtain the high bonding strength environment-friendly supramolecular physical gel adhesive.
Bonding of the samples: and respectively and uniformly coating the prepared gel adhesive on one end of the surface of the glass sheet, then pressing the other glass sheet on the area coated with the adhesive, and standing at room temperature until the adhesive is fixed.
The bonded glass sheets were subjected to tensile testing, and the tensile shear strength (stress divided by bonding area) of the gel adhesive applied to the glass surface in this example was calculated to be 4.3 MPa.
The examples show that the method for preparing the water-based adhesive of the invention is simple and convenient, and the used materials are safe and nontoxic, have good adhesion effect and wide application range, and have wide application prospect and commercial value.
Claims (5)
1. A preparation method of a high bonding strength environment-friendly supramolecular physical gel adhesive comprises the following steps:
1) preparation of prepolymerization solution: dissolving the nanoparticles in deionized water, and stirring for 10-50 minutes until the nanoparticles are completely dissolved, wherein the concentration is 5.0-20.0 mg/mL; adding a monomer into the solution, stirring the solution for 20 to 70 minutes until the monomer is completely dissolved, and preparing a prepolymerization solution with the monomer concentration of 7 to 15 wt%; the nano particles are one or more than two of carbon nano tubes, montmorillonite, cellulose nanocrystals or nano carbon dots, and the particle size is 10-200 nm; the monomer is one or two of acrylic acid, dimethyl acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, methacrylic acid or hydroxyethyl methacrylate;
2) preparation of supramolecular physical gel: adding an initiator into deionized water, and carrying out ultrasonic treatment for 10-30 minutes until the initiator is completely dissolved to obtain a solution with the concentration of 4-18 mg/mL; adding 1-7 mL of the solution into 10-17 mL of the prepolymerization solution obtained in the step 1), finally adding a catalyst with the mass ratio of the catalyst to the initiator being 1: 10-10: 1, stirring for 3-10 minutes, and standing at room temperature for 10-20 hours to obtain the high-bonding-strength environment-friendly supramolecular physical gel adhesive.
2. The method for preparing the environment-friendly supramolecular physical gel adhesive with high bonding strength as claimed in claim 1, characterized in that: when two monomers are used, the molar ratio between the two monomers is 1:5 to 5: 1.
3. The method for preparing the environment-friendly supramolecular physical gel adhesive with high bonding strength as claimed in claim 1, characterized in that: the initiator is one or more of potassium persulfate, ammonium persulfate, azodiisobutyronitrile and ammonium ceric nitrate.
4. The method for preparing the environment-friendly supramolecular physical gel adhesive with high bonding strength as claimed in claim 1, characterized in that: the catalyst is one or more of sodium sulfite, N-dimethylcyclohexylamine, tetramethylethylenediamine and N-ethylmorpholine.
5. The environment-friendly supramolecular physical gel adhesive with high bonding strength is characterized in that: is prepared by the method of any one of claims 1 to 4.
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| CN110423363B (en) * | 2019-09-17 | 2022-02-08 | 安徽农业大学 | Preparation method and application of high-strength ultrahigh-elasticity hydrogel |
| CN114763457B (en) * | 2021-01-15 | 2023-06-16 | 天津大学 | High-strength long-acting adhesive suitable for various severe environments and preparation method and application thereof |
| CN113601659B (en) * | 2021-06-29 | 2022-06-24 | 中国林业科学研究院木材工业研究所 | Flame-retardant glue-free fiber board based on carbon quantum dots and preparation method thereof |
| CN114652887A (en) * | 2022-03-17 | 2022-06-24 | 北京大学 | Strong-adhesion microgel dry powder capable of spontaneously forming sealing layer, preparation method and application thereof |
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| CN105462523A (en) * | 2016-01-05 | 2016-04-06 | 吉林大学 | Method for preparing high-adhesion water-borne adhesive based on polymer compound |
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