CN110144189B - Water-based flocking adhesive and preparation method thereof - Google Patents
Water-based flocking adhesive and preparation method thereof Download PDFInfo
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- CN110144189B CN110144189B CN201910393723.5A CN201910393723A CN110144189B CN 110144189 B CN110144189 B CN 110144189B CN 201910393723 A CN201910393723 A CN 201910393723A CN 110144189 B CN110144189 B CN 110144189B
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3893—Low-molecular-weight compounds having heteroatoms other than oxygen containing silicon
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Abstract
The invention relates to a water-based flocking adhesive which is characterized by being prepared from the following raw materials in parts by weight: 20-30 parts of water-soluble end acrylate group hyperbranched polyester, 5-10 parts of 3-chlorine-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine, 30-40 parts of end hydroxyl waterborne polyurethane, 1-5 parts of blocked isocyanate cross-linking agent, 1-3 parts of D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate), 0.5-1 part of fluorine-containing trihydroxysilane compound, 2-5 parts of emulsifier, 0.1-0.5 part of initiator and 50-60 parts of water. The invention also discloses a preparation method and a using method of the water-based flocking adhesive. The water-based flocking adhesive disclosed by the invention has the advantages of good water resistance, wear resistance and weather resistance, high bonding strength, excellent stability, water resistance, hand feeling, air permeability and moisture permeability, safety in use, greenness and environmental friendliness.
Description
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to a water-based flocking adhesive and a preparation method thereof.
Background
With the development of society and the improvement of living standard, the automobile industry develops rapidly, people have higher and higher requirements on sealing materials in the automobile industry, and the sealing materials with good development performance become hot spots of research in the current industry. The automobile flocking sealing strip is a sealing material which is common in the automobile field, mainly comprises a window side sealing strip (water cutting) and a window glass guide groove, has the functions of sealing outside wind and rain, preventing dust from entering, reducing noise, enabling glass to slide more easily and the like, and is flocking adhesive which is an essential reagent in the manufacturing process of the automobile flocking sealing strip, wherein the performance of the flocking sealing strip directly affects the sealing effect of the automobile flocking sealing strip. Therefore, it is imperative to develop a flocking adhesive having excellent properties.
The flocking glue can be roughly divided into organic solvent type glue and water-based glue according to different solvents used by the flocking glue, and due to the increasingly strict environmental protection policy and law and regulation of the country and the place, the water-based flocking glue becomes the mainstream trend of the current and future development of the flocking glue industry with the advantage of environmental protection, and can be more commonly used. At present, the more used water-based flocking adhesive is polyacrylate emulsion adhesive which has the advantages of low price, convenient preparation and use, aging resistance and good adhesive force system on various fibers, but has the defects of wear resistance, water resistance and flexibility, particularly, the crosslinking monomer of the acrylate emulsion flocking adhesive is mostly hydroxymethyl acrylamide and the crosslinking agent is mostly methylated hydroxymethyl melamine, the contained hydroxymethyl group can slowly release formaldehyde, the toxicity is higher, and the increasingly strict environmental protection requirement on textiles can not be met.
The water-based flocking adhesive with water-based polyurethane as a main component in the prior art is provided, the water-based flocking adhesive just avoids the defects of polyacrylate flocking adhesives, but still has the problems of poor water resistance and wear resistance, and is often inconvenient for industrial production in practical application. The water-based flocking adhesive on the market also generally has the defects of low bonding strength and poor stability, water resistance, hand feeling, air permeability and moisture permeability, and also has the defects of unsafe use, high baking temperature and the like of partial adhesives.
Therefore, the flocking adhesive which is excellent in comprehensive performance, safe and environment-friendly to use, meets market requirements, has wide market value and application prospect, and has very important significance for promoting the development of the water-based adhesive industry.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the water-based flocking adhesive and the preparation method thereof, the preparation method is simple, convenient and easy to operate, the preparation raw materials are environment-friendly and harmless, the preparation cost is low, and the preparation method is suitable for large-scale production; the prepared water-based flocking adhesive has the advantages of good water resistance, wear resistance and weather resistance, high bonding strength, excellent stability, water resistance, hand feeling, air permeability and moisture permeability, safety in use, greenness and environmental protection.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the water-based flocking adhesive is prepared from the following raw materials in parts by weight: 20-30 parts of water-soluble terminal acrylate hyperbranched polyester, 5-10 parts of 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine, 30-40 parts of terminal hydroxyl waterborne polyurethane, 1-5 parts of blocked isocyanate cross-linking agent, 1-3 parts of D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate) (CAS number: 61241-59-6), 0.5-1 part of fluorine-containing trihydroxysilane compound, 2-5 parts of emulsifier, 0.1-0.5 part of initiator and 50-60 parts of water.
Further, the emulsifier is at least one of sodium dodecyl sulfate, secondary alcohol fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether and alkylphenol ether sodium sulfosuccinate.
Further, the initiator is at least one of potassium persulfate, sodium persulfate, ammonium persulfate and azodiisopropyl imidazoline hydrochloride.
Further, the preparation method of the 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine comprises the following steps: dissolving 3-chloro-2-hydroxypropyl acrylate and hyperbranched polyethyleneimine in N, N-dimethylacetamide, stirring and reacting at 60-80 ℃ for 4-6 hours, then carrying out rotary evaporation to remove N, N-dimethylacetamide, washing the product with diethyl ether for 3-5 times, and then placing in a vacuum drying oven at 80-90 ℃ to dry to constant weight.
Preferably, the mass ratio of the 3-chloro-2-hydroxypropyl acrylate to the hyperbranched polyethyleneimine to the N, N-dimethylacetamide is 1:1 (8-12).
Further, the preparation method of the fluorine-containing trihydroxy silane compound comprises the following steps: mixing trifluoro-chloro-chrysanthemic acid and 3-aminopropyl trihydroxy silane, stirring and reacting at 60-80 ℃ for 3-5 hours, adding water and dichloromethane according to the mass ratio of 3:1, separating liquid, taking an organic phase, removing water by using anhydrous magnesium sulfate, filtering, taking a filtrate, and removing dichloromethane by rotary evaporation to obtain the fluorine-containing hydroxysilane compound.
Preferably, the mass ratio of the trifluoro-chloro-chrysanthemic acid to the 3-aminopropyl trihydroxy silane is 1.77: 1.
Further, the preparation method of the water-based flocking adhesive comprises the following steps:
s1, adding water and an emulsifier into an emulsifying kettle, wherein the adding amount of the water is 40-50% of the total amount, the adding amount of the emulsifier is 80-90% of the total amount, adding water-soluble terminal acrylate hyperbranched polyester, 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine and hydroxyl-terminated waterborne polyurethane while stirring, and uniformly stirring to obtain a mixture A;
s2, adding the residual amount of water and the residual amount of emulsifier into another emulsifying kettle, adding a closed isocyanate crosslinking agent, D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate), a fluorine-containing trihydroxysilane compound and an initiator while stirring, and uniformly stirring to obtain a mixture B;
and S3, mixing the mixture A prepared in the step S1 and the mixture B prepared in the step S2, and stirring uniformly to obtain the water-based flocking adhesive.
Further, the use method of the water-based flocking adhesive comprises the following steps: and (3) gluing the water-based flocking adhesive on the vegetation body at the temperature of 60-80 ℃, and curing.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the preparation method of the water-based flocking adhesive is simple, convenient and easy to operate, environment-friendly and harmless in preparation raw materials, low in preparation cost and suitable for large-scale production; the prepared water-based flocking adhesive has the advantages of good water resistance, wear resistance and weather resistance, high bonding strength, excellent stability, water resistance, hand feeling, air permeability and moisture permeability, safety in use, greenness and environmental protection. Monomers with unsaturated bonds, such as water-soluble terminal allyl acid hyperbranched polyester, 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine, D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate) and fluorine-containing trihydroxysilane compounds, are introduced, and are converged to form a three-dimensional network structure in a curing stage, so that the comprehensive performance of the adhesive is improved, and a fluorine-silicon structure is introduced through polymerization and curing, so that the comprehensive performance of the material can be further improved; the introduced fluorine-containing trihydroxy silane compound forms a hydrophobic group after being cured, so that the water resistance of the cured adhesive is improved; the hydroxyl-terminated waterborne polyurethane and quaternary ammonium salt structure is introduced, so that the adhesive strength can be obviously improved; the blocked isocyanate crosslinking agent is stable at normal temperature and does not react with other components in the adhesive chemically, and when the blocked isocyanate crosslinking agent is cured, the blocked isocyanate crosslinking agent is deblocked due to heating and then reacts with other substances with hydroxyl and amino to further improve the comprehensive performance of the adhesive.
Detailed Description
The invention relates to a water-based flocking adhesive which is prepared from the following raw materials in parts by weight: 20-30 parts of water-soluble terminal acrylate hyperbranched polyester, 5-10 parts of 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine, 30-40 parts of terminal hydroxyl waterborne polyurethane, 1-5 parts of blocked isocyanate cross-linking agent, 1-3 parts of D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate) (CAS number: 61241-59-6), 0.5-1 part of fluorine-containing trihydroxysilane compound, 2-5 parts of emulsifier, 0.1-0.5 part of initiator and 50-60 parts of water.
The emulsifier is at least one of sodium dodecyl sulfate, secondary alcohol fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether and alkylphenol ether sodium sulfosuccinate. The initiator is at least one of potassium persulfate, sodium persulfate, ammonium persulfate and azodiisopropyl imidazoline hydrochloride. The preparation method of the 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine comprises the following steps: dissolving 3-chloro-2-hydroxypropyl acrylate and hyperbranched polyethyleneimine in N, N-dimethylacetamide, stirring and reacting at 60-80 ℃ for 4-6 hours, then carrying out rotary evaporation to remove N, N-dimethylacetamide, washing the product with diethyl ether for 3-5 times, and then placing in a vacuum drying oven at 80-90 ℃ to dry to constant weight. The mass ratio of the 3-chloro-2-hydroxy propyl acrylate to the hyperbranched polyethyleneimine to the N, N-dimethylacetamide is 1:1 (8-12). The preparation method of the fluorine-containing trihydroxysilane compound comprises the following steps: mixing trifluoro-chloro-chrysanthemic acid and 3-aminopropyl trihydroxy silane, stirring and reacting at 60-80 ℃ for 3-5 hours, adding water and dichloromethane according to the mass ratio of 3:1, separating liquid, taking an organic phase, removing water by using anhydrous magnesium sulfate, filtering, taking a filtrate, and removing dichloromethane by rotary evaporation to obtain the fluorine-containing hydroxysilane compound. The mass ratio of the trifluoro-chloro-chrysanthemic acid to the 3-aminopropyl trihydroxy silane is 1.77: 1.
The preparation method of the water-based flocking adhesive comprises the following steps: s1, adding water and an emulsifier into an emulsifying kettle, wherein the adding amount of the water is 40-50% of the total amount, the adding amount of the emulsifier is 80-90% of the total amount, adding water-soluble terminal acrylate hyperbranched polyester, 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine and hydroxyl-terminated waterborne polyurethane while stirring, and uniformly stirring to obtain a mixture A; s2, adding the residual amount of water and the residual amount of emulsifier into another emulsifying kettle, adding a closed isocyanate crosslinking agent, D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate), a fluorine-containing trihydroxysilane compound and an initiator while stirring, and uniformly stirring to obtain a mixture B; and S3, mixing the mixture A prepared in the step S1 and the mixture B prepared in the step S2, and stirring uniformly to obtain the water-based flocking adhesive.
The application method of the water-based flocking adhesive comprises the following steps: and (3) gluing the water-based flocking adhesive on the vegetation body at the temperature of 60-80 ℃, and curing. The raw materials were all purchased commercially. The preparation method of the water-based flocking adhesive is simple, convenient and easy to operate, environment-friendly and harmless in preparation raw materials, low in preparation cost and suitable for large-scale production; the prepared water-based flocking adhesive has the advantages of good water resistance, wear resistance and weather resistance, high bonding strength, excellent stability, water resistance, hand feeling, air permeability and moisture permeability, safety in use, greenness and environmental protection. Monomers with unsaturated bonds, such as water-soluble terminal allyl acid hyperbranched polyester, 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine, D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate) and fluorine-containing trihydroxysilane compounds, are introduced, and are converged to form a three-dimensional network structure in a curing stage, so that the comprehensive performance of the adhesive is improved, and a fluorine-silicon structure is introduced through polymerization and curing, so that the comprehensive performance of the material can be further improved; the introduced fluorine-containing trihydroxy silane compound forms a hydrophobic group after being cured, so that the water resistance of the cured adhesive is improved; the hydroxyl-terminated waterborne polyurethane and quaternary ammonium salt structure is introduced, so that the adhesive strength can be obviously improved; the blocked isocyanate crosslinking agent is stable at normal temperature and does not react with other components in the adhesive chemically, and when the blocked isocyanate crosslinking agent is cured, the blocked isocyanate crosslinking agent is deblocked due to heating and then reacts with other substances with hydroxyl and amino to further improve the comprehensive performance of the adhesive.
The following detailed description of preferred embodiments of the invention will be made.
Example 1
Embodiment 1 provides a water-based flocking adhesive, which is prepared from the following raw materials in parts by weight: 20 parts of water-soluble end acrylate based hyperbranched polyester, 5 parts of 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine, 30 parts of hydroxyl-terminated waterborne polyurethane, 1 part of blocked isocyanate cross-linking agent, 1 part of D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate), 0.5 part of fluorine-containing trihydroxysilane compound, 2 parts of sodium dodecyl sulfate, 0.1 part of potassium persulfate and 50 parts of water.
The preparation method of the 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine comprises the following steps: dissolving 1kg of 3-chloro-2-hydroxypropyl acrylate and 1kg of hyperbranched polyethyleneimine in 8kg of N, N-dimethylacetamide, stirring and reacting at 60 ℃ for 4 hours, then carrying out rotary evaporation to remove the N, N-dimethylacetamide, washing the product with diethyl ether for 3 times, and then placing the product in a vacuum drying oven at 80 ℃ to dry the product to constant weight.
The preparation method of the fluorine-containing trihydroxysilane compound comprises the following steps: mixing 1.77kg of trifluoro-chloro-chrysanthemic acid and 1kg of 3-aminopropyl trihydroxysilane, stirring and reacting for 3 hours at 60 ℃, adding water and dichloromethane according to the mass ratio of 3:1, separating liquid, taking an organic phase, removing water by using anhydrous magnesium sulfate, filtering, taking a filtrate, and removing dichloromethane by rotary evaporation to obtain the fluorine-containing hydroxysilane compound.
The preparation method of the water-based flocking adhesive comprises the following steps:
s1, adding water and an emulsifier into an emulsifying kettle, wherein the adding amount of the water is 40% of the total amount, the adding amount of the emulsifier is 80% of the total amount, adding water-soluble terminal acrylate hyperbranched polyester, 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine and hydroxyl-terminated waterborne polyurethane while stirring, and stirring uniformly to obtain a mixture A;
s2, adding the residual amount of water and the residual amount of emulsifier into another emulsifying kettle, adding a closed isocyanate crosslinking agent, D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate), a fluorine-containing trihydroxysilane compound and an initiator while stirring, and uniformly stirring to obtain a mixture B;
and S3, mixing the mixture A prepared in the step S1 and the mixture B prepared in the step S2, and stirring uniformly to obtain the water-based flocking adhesive.
The application method of the water-based flocking adhesive comprises the following steps: and (3) gluing the water-based flocking adhesive on a 60-DEG C plant to be planted, and curing.
Example 2
Embodiment 2 provides a water-based flocking adhesive and a preparation method thereof, which are substantially the same as those in embodiment 1, except that the water-based flocking adhesive is prepared from the following raw materials in parts by weight: 23 parts of water-soluble end acrylate based hyperbranched polyester, 7 parts of 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine, 33 parts of end hydroxyl waterborne polyurethane, 2 parts of blocked isocyanate crosslinking agent, 1.5 parts of D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate), 0.7 part of fluorine-containing trihydroxysilane compound, 3 parts of secondary alcohol fatty alcohol polyoxyethylene ether, 0.2 part of sodium persulfate and 53 parts of water.
Example 3
Embodiment 3 provides a water-based flocking adhesive and a preparation method thereof, which are basically the same as those in embodiment 1, except that the water-based flocking adhesive is prepared from the following raw materials in parts by weight: 25 parts of water-soluble end acrylate based hyperbranched polyester, 7.5 parts of 3-chlorine-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine, 35 parts of end hydroxyl waterborne polyurethane, 3 parts of blocked isocyanate cross-linking agent, 2 parts of D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate), 0.7 part of fluorine-containing trihydroxysilane compound, 3.6 parts of castor oil polyoxyethylene ether, 0.3 part of initiator and 55 parts of ammonium persulfate.
Example 4
Embodiment 4 provides a water-based flocking adhesive and a preparation method thereof, which are substantially the same as those in embodiment 1, except that the water-based flocking adhesive is prepared from the following raw materials in parts by weight: 28 parts of water-soluble end acrylate hyperbranched polyester, 9 parts of 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine, 38 parts of hydroxyl-terminated waterborne polyurethane, 4 parts of blocked isocyanate crosslinking agent, 2.5 parts of D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate), 0.9 part of fluorine-containing trihydroxysilane compound, 4.5 parts of emulsifier, 0.45 part of initiator and 59 parts of water. The emulsifier is formed by mixing sodium dodecyl sulfate, secondary alcohol fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether and alkylphenol ether sodium sulfosuccinate according to the mass ratio of 1:1:3: 2. The initiator is formed by mixing potassium persulfate, sodium persulfate, ammonium persulfate and azodiisopropyl imidazoline hydrochloride according to the mass ratio of 1:3:2: 2.
Example 5
Example 5 provides a water-based flocking adhesive and a preparation method thereof, which are substantially the same as those in example 1, except that the water-based flocking adhesive is prepared from the following raw materials in parts by weight: 30 parts of water-soluble end acrylate hyperbranched polyester, 10 parts of 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine, 40 parts of hydroxyl-terminated waterborne polyurethane, 5 parts of blocked isocyanate cross-linking agent, 3 parts of D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate), 1 part of fluorine-containing trihydroxysilane compound, 5 parts of alkylphenol ether sulfosuccinic acid sodium salt, 0.5 part of azodiisopropyl imidazoline hydrochloride and 60 parts of water.
Comparative example 1
Comparative example 1 provides an aqueous flocking adhesive and a method for preparing the same, which are substantially identical to those of example 1 except that a water-soluble terminal acrylate-based hyperbranched polyester is not added to the formulation.
Comparative example 2
Comparative example 2 provides a water-based flocking adhesive and a preparation method thereof, which are substantially identical to those of example 1 except that 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine is not added in the formula.
Comparative example 3
Comparative example 3 provides a water-based flocking adhesive and a method for preparing the same, which are substantially identical to those of example 1 except that D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate) is not added to the formulation.
Comparative example 4
Comparative example 4 provides an aqueous flocking adhesive and a method for preparing the same, which are substantially identical to those of example 1 except that a fluorine-containing trihydroxysilane compound is not added to the formulation.
Comparative example 5
Comparative example 5 provides a commercially available aqueous polyurethane-based flocking adhesive.
In order to further illustrate the technical effects of the aqueous flocking adhesive in the embodiments of the present invention, the aqueous flocking adhesive in each of the above embodiments is coated on a plant to be treated at 60 ℃, after curing, the aqueous flocking adhesive is tested for washing fastness, dry grinding fastness, solvent resistance, flexibility and hand feeling, and the results are shown in table 1, wherein the washing fastness is tested according to GB/T8629-2001, home washing and drying procedure for textile testing, and the abrasion resistance is tested according to GB/T21196-2007, determination of abrasion resistance of textile by martindale method.
TABLE 1 Performance test Table based on the aqueous flocking adhesives in examples 1-5 and comparative examples 1-5
As can be seen from Table 1, the aqueous flocking adhesives in examples 1-5 have significantly better performance than the prior art (comparative example 5), and are more excellent in washing fastness, dry grinding fastness, solvent resistance, flexibility and hand feeling, which is a result of the synergistic effect of the components.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
1. The water-based flocking adhesive is characterized by being prepared from the following raw materials in parts by weight: 20-30 parts of water-soluble end acrylate group hyperbranched polyester, 5-10 parts of 3-chlorine-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine, 30-40 parts of end hydroxyl waterborne polyurethane, 1-5 parts of blocked isocyanate cross-linking agent, 1-3 parts of D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate), 0.5-1 part of fluorine-containing trihydroxysilane compound, 2-5 parts of emulsifier, 0.1-0.5 part of initiator and 50-60 parts of water.
2. The aqueous flocking glue of claim 1 wherein the emulsifier is at least one of sodium lauryl sulfate, secondary alcohol fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether, and sodium alkylphenol ether sulfosuccinate.
3. The water-based flocking glue of claim 1 wherein the initiator is at least one of potassium persulfate, sodium persulfate, ammonium persulfate, azodiisopropyl imidazoline hydrochloride.
4. The aqueous flocking glue of claim 1, wherein the preparation method of the 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine comprises the following steps: dissolving 3-chloro-2-hydroxypropyl acrylate and hyperbranched polyethyleneimine in N, N-dimethylacetamide, stirring and reacting at 60-80 ℃ for 4-6 hours, then carrying out rotary evaporation to remove N, N-dimethylacetamide, washing the product with diethyl ether for 3-5 times, and then placing in a vacuum drying oven at 80-90 ℃ to dry to constant weight.
5. The water-based flocking glue according to claim 4, wherein the mass ratio of the 3-chloro-2-hydroxypropyl acrylate, the hyperbranched polyethyleneimine and the N, N-dimethylacetamide is 1:1 (8-12).
6. The aqueous flocking glue of claim 1, wherein the preparation method of the fluorine-containing trihydroxysilane compound comprises the following steps: mixing trifluoro-chloro-chrysanthemic acid and 3-aminopropyl trihydroxy silane, stirring and reacting at 60-80 ℃ for 3-5 hours, adding water and dichloromethane according to the mass ratio of 3:1, separating liquid, taking an organic phase, removing water by using anhydrous magnesium sulfate, filtering, taking a filtrate, and removing dichloromethane by rotary evaporation to obtain the fluorine-containing hydroxysilane compound.
7. The water-based flocking glue according to claim 6, wherein the mass ratio of the trichloro-chrysanthemic acid to the 3-aminopropyl trihydroxy silane is 1.77: 1.
8. The aqueous flocking glue of any one of claims 1 to 7 wherein the preparation method of the aqueous flocking glue comprises the following steps:
s1, adding water and an emulsifier into an emulsifying kettle, wherein the adding amount of the water is 40-50% of the total amount, the adding amount of the emulsifier is 80-90% of the total amount, adding water-soluble terminal acrylate hyperbranched polyester, 3-chloro-2-hydroxypropyl acrylate ionized modified hyperbranched polyethyleneimine and hydroxyl-terminated waterborne polyurethane while stirring, and uniformly stirring to obtain a mixture A;
s2, adding the residual amount of water and the residual amount of emulsifier into another emulsifying kettle, adding a closed isocyanate crosslinking agent, D-mannitol 1, 6-bis (2-isocyano-3-methyl-2-butenoate), a fluorine-containing trihydroxysilane compound and an initiator while stirring, and uniformly stirring to obtain a mixture B;
and S3, mixing the mixture A prepared in the step S1 and the mixture B prepared in the step S2, and stirring uniformly to obtain the water-based flocking adhesive.
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| CN112079982B (en) * | 2020-09-21 | 2022-04-15 | 浙江华峰合成树脂有限公司 | Super-soft protein-imitated hydrolysis-resistant polyurethane resin and preparation method thereof |
| CN112500732A (en) * | 2020-12-22 | 2021-03-16 | 冯国旭 | Weather-resistant exterior wall putty powder and preparation method thereof |
| CN114525098B (en) * | 2022-03-03 | 2023-09-08 | 华威粘结材料（上海）股份有限公司 | Single-component water-based flocking adhesive, flocking piece and preparation method thereof |
| CN114539966B (en) * | 2022-04-24 | 2022-07-19 | 苏州市陆氏新材料有限公司 | Heating crosslinking polyurethane adhesive, polyurethane adhesive film and preparation method thereof |
| CN115895540A (en) * | 2022-12-20 | 2023-04-04 | 益丰新材料股份有限公司 | Adhesive composition and application thereof in preparation of recombined wood |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5821294A (en) * | 1996-08-30 | 1998-10-13 | National Starch And Chemical Investment Holding Corporation | Water-based laminating adhesives |
| DE102006011813A1 (en) * | 2006-03-15 | 2007-09-20 | Degussa Gmbh | Use of a hyperbranched polymer for surface modification of a solid matrix in the cured state |
| JP2011084625A (en) * | 2009-10-14 | 2011-04-28 | Aica Kogyo Co Ltd | Adhesive composition and laminate body |
| CN102030884B (en) * | 2010-10-26 | 2012-08-08 | 华南理工大学 | High-solid-content UV (Ultraviolet)-curing aqueous urethane acrylate dispersion liquid and preparation method thereof |
| CN107674629B (en) * | 2017-07-21 | 2020-12-22 | 华南理工大学 | One-component moisture-curing polyurethane furniture edge sealing adhesive and preparation method thereof |
| CN107695902B (en) * | 2017-10-18 | 2020-03-06 | 河北思瑞恩新材料科技有限公司 | Flocking material and preparation method thereof |
| CN107779073A (en) * | 2017-11-17 | 2018-03-09 | 广东华兹卜新材料科技有限公司 | A kind of hot water resistance woodcare paint |
| CN109439263B (en) * | 2018-12-03 | 2019-08-30 | 苏州市陆氏新材料有限公司 | A kind of preparation method of spary coating type water soluble flocking glue |
| CN109517567B (en) * | 2018-12-03 | 2021-02-12 | 苏州市陆氏新材料有限公司 | Preparation method of water-based flocking adhesive for automobile sealing strip |
| CN110317301B (en) * | 2019-06-24 | 2022-01-11 | 常熟巴德富科技有限公司 | Core-shell type polyurethane-acrylic emulsion and preparation method and application thereof |
-
2019
- 2019-05-13 CN CN202010197328.2A patent/CN111234758A/en not_active Withdrawn
- 2019-05-13 CN CN201910393723.5A patent/CN110144189B/en not_active Expired - Fee Related
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| CN110144189A (en) | 2019-08-20 |
| CN111234758A (en) | 2020-06-05 |
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