CN111394045A - Single-component polyurethane adhesive for plastic sports floor compounding and preparation method thereof - Google Patents
Single-component polyurethane adhesive for plastic sports floor compounding 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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
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- C09J175/08—Polyurethanes from polyethers
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/4205—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups
- C08G18/4208—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups
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- C08G18/40—High-molecular-weight compounds
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- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/06—Polyurethanes from polyesters
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Abstract
The invention discloses a preparation method of a single-component polyurethane adhesive for compounding plastic sports floors, which is characterized in that polyol ester and diisocyanate are used as basic raw materials, and an antioxidant, a catalyst, a leveling agent and other auxiliaries are matched, so that a moisture reaction type polyurethane adhesive with the solid content of 100% is obtained through high-temperature polymerization reaction. The adhesive is a single-component moisture-reactive polyurethane adhesive which is cured without using a cross-linking agent, is applied to compounding of a fiber reinforced layer and a TPE/EVA/PVC foaming buffer layer of a plastic sports floor, and has the advantages of simple process, higher bonding strength and good application prospect. The solid content of the adhesive is 100%, the adhesive does not contain a solvent, the solvent is not used in the process, a drying tunnel is not needed to be arranged during application, the cost is reduced, and the problems of safety and environmental protection do not exist.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a single-component polyurethane adhesive for compounding a plastic sports floor and a preparation method thereof.
Background
The plastic sports floor comprises a rubber floor, a PVC floor and a TPU floor, is a novel light floor decoration material which is popular at present, and is produced by taking synthetic rubber, PVC, TPU and copolymer resin thereof as main raw materials through a coating process or a calendering extrusion process. The floor has wide market application prospect, and is particularly widely applied to various sports fields and commercial occasions.
The economy develops rapidly, people have higher and higher requirements on the field level of fitness sports, and the market demand of high-grade and professional indoor sports fields is increased. At present, the TPU or PVC floor is the best material for paving the indoor playground, and the selection is not only based on the good impact absorbability, shock absorption, elasticity, pollution resistance, bacteria resistance and the like of the TPU/PVC floor, but also is suitable for indoor use because of absolute safety, no volatile odor, real environmental protection and durability.
The plastic sports floor material is precise in structure and mainly comprises a TPU/PVC wear-resistant layer, a fiber reinforced layer and a TPE/EVA/PVC foaming buffer layer, and an adhesive is required to be used for adhesion between the fiber reinforced layer and the TPE/EVA/PVC foaming buffer layer. In the past, the adhesive for plastic sports floor sold on the market is solvent type, and the solvent is dried when in use, and a curing agent is needed for curing and adhering. The solvent has the properties of irritation, flammability, explosiveness and the like, so that the solvent can cause harm or potential harm to the environment, safety and sanitation, and the solvent residue problem is easy to occur after the solvent-based adhesive is used for the sports floor and is processed, so that the problem of bad smell is caused, and the sports quality is influenced. The subsequent market successively appears solvent-free adhesives, which are divided into two components and one component. The double-component adhesive has the advantages of short service time due to the fact that the double-component adhesive is prepared when in use, low initial adhesion and inconvenient operation, and the market occupation ratio is low. Meanwhile, the single-component adhesive is simple to prepare without the need of preparing the adhesive, but the reactive type or the non-reactive type generally needs to be processed at a high temperature of more than 130 ℃, so that the temperature-sensitive material cannot be processed, and the development of the single-component adhesive is limited. Therefore, a substitute preparation process is urgently needed for the application field of the adhesive for plastic sports floor composite, and the problems of sports floor composite processing are solved.
Chinese patent CN110172325A discloses a solvent-free bi-component polyurethane adhesive suitable for composite floors, which comprises a component A and a component B, wherein the component A is a polyisocyanate raw material, and the component B is oligomeric polyol, a cross-linking/chain-extending agent, a filler, a thixotropic agent and a catalyst. The invention is a solvent-free adhesive, has no solvent volatilization problem, solves many problems generated by solvent-based adhesives, however A, B. The two components have the problem of time use and inconvenient operation after mixing when in use.
Chinese patent CN110343502A discloses a solvent-free polyurethane adhesive for rubber floors and a preparation method thereof, wherein the adhesive comprises A, B two components which are mixed according to a ratio when in use. Compared with a solvent-based adhesive, the adhesive has no solvent volatilization problem, avoids harm to personnel health caused by an organic solvent in the gluing process, and avoids pollution of the organic solvent to the environment. But instead. The problem of glue preparation is inconvenient to operate and the problem of use time after glue preparation is solved, and the problem is different from the problem that a single-component adhesive does not need to be prepared and does not have use time.
Chinese patent CN105778824A discloses an adhesive for sheet material, which is also A, B bi-component, and has the above processing problems.
Chinese patent CN109098392A discloses a novel rubber sports floor and a preparation method thereof, wherein the rubber sports floor comprises a rubber wear-resistant layer and a PVC composite layer, and the two layers are bonded by using an interfacial agent (adhesive) to obtain the novel rubber sports floor. The adhesive for floor compounding is a single-component moisture-curing polyurethane PUR hot melt adhesive, when the adhesive is used, the polyurethane PUR is heated to 150 ℃ and then is changed from solid to liquid, coating processing can be carried out, energy is wasted due to high-temperature melting, and the temperature-sensitive material cannot be partially processed, so that the quality of a finished product is easily influenced.
Disclosure of Invention
The invention provides a single-component polyurethane adhesive for compounding plastic sports floors and a preparation method thereof, and solves the technical problems of difficult processing, safety and environmental protection of the adhesive.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation method of a single-component polyurethane adhesive for compounding plastic sports floors comprises the following steps:
s1, taking the polyol ester and the antioxidant according to the corresponding weight based on the total weight of the polyurethane adhesive, and putting the taken polyol ester and the antioxidant into a polymerization stirring reaction kettle;
s2, heating and melting materials in the polymerization stirring reaction kettle, stirring and mixing uniformly, vacuumizing to enable the vacuum degree in the reaction kettle to be below 50torr when the temperature of the materials reaches 110-120 ℃, then dehydrating, filling nitrogen to return to normal pressure after the reaction kettle is continuously in a negative pressure state for 1-3 hours, detecting the moisture value contained in the materials, ending the dehydration if the moisture value is lower than 300ppm (mg/kg), and returning to the negative pressure state to continue the dehydration if the moisture value is higher than 300ppm (mg/kg);
s3, after dehydration is finished, returning the reaction kettle to normal pressure, reducing the temperature to 60-70 ℃, introducing nitrogen to maintain the micro-positive pressure of the reaction kettle, taking diisocyanate with corresponding weight based on the total weight of the polyol ester in the step S1, putting the taken diisocyanate into a polymerization stirring reaction kettle, heating the reaction kettle, maintaining the reaction temperature at 100-110 ℃, and allowing the reaction time to be not less than 1 hour;
s4, detecting the weight percentage content NCO% of the isocyanate group every 20-30min in the reaction process of the step S3;
and S5, when the NCO% is lower than the theoretical value, adding a certain amount of catalyst and flatting agent into the reaction kettle, uniformly stirring, carrying out negative pressure defoaming and continuous reaction, and reacting until no bubble exists in the reaction kettle to obtain a viscous liquid product.
Further, the polyol ester is any one of or a mixture of at least two of polyethylene glycol butanediol adipate, neopentyl glycol phthalate, neopentyl glycol isophthalate, polypropylene oxide glycol and trimethylolpropane dipropylene glycol adipate. The function of adapting to the connection of various substrates is achieved by selecting and matching one or more polyol esters according to the product performance and the characteristics of the connected substrates.
Further, the antioxidant is a hindered phenol antioxidant; the leveling agent is acrylate copolymer polymer. Has the functions of no reaction with isocyanate group and ensuring longer pot life and storage life of the product.
Further, the polyol ester accounts for 65-74.5 wt% of the total weight of the polyurethane adhesive, the antioxidant accounts for 0.1-0.3 wt% of the total weight of the polyurethane adhesive, and the diisocyanate accounts for 25-34.5 wt% of the total weight of the polyurethane adhesive.
Further, in the step S5, 0.02 to 0.1 wt% of a catalyst and 0.10 to 0.30 wt% of a leveling agent are added to the reaction kettle based on the total weight of the polyurethane adhesive.
In step S3, the diisocyanate is diphenylmethane diisocyanate (MDI), and an excess amount of the diisocyanate (MDI) is added in an amount of 1.7 to 2.0 times the total weight of the polyol ester.
Further, the catalyst is a mixture of an amine catalyst and a tin catalyst. The catalyst has the effects of promoting the rapid reaction of isocyanate groups and hydroxyl groups and the crosslinking reaction of the processed isocyanate groups and water vapor, and the simultaneous use of the two catalysts is beneficial to promoting the curing and curing speed of the adhesive.
A single-component polyurethane adhesive for compounding plastic sports floors comprises the following components in percentage by weight: 65-74.5 wt% of polyol ester, 25-34.5 wt% of diisocyanate, 0.1-0.3 wt% of antioxidant, 0.02-0.1 wt% of catalyst and 0.10-0.30 wt% of flatting agent, wherein the sum of the weight percentages of the components is 100%.
Further, the polyurethane adhesive is a polyurethane prepolymer with 100% of solid content, which is prepared by taking polyol ester and diisocyanate as basic raw materials, matching with an antioxidant, a catalyst and a leveling agent and carrying out high-temperature polymerization reaction.
Further, the polyol ester is any one or a mixture of at least two of polyethylene glycol butanediol adipate, neopentyl glycol phthalate, neopentyl glycol isophthalate, polypropylene oxide glycol and trimethylolpropane dipropylene glycol adipate; the catalyst is a mixture of amine catalyst and tin catalyst.
The invention achieves the following beneficial effects:
(1) the adhesive disclosed by the invention has the advantages that the solid content is 100%, no solvent is contained, the production process is free of solvent taste, and the adhesive is safe and environment-friendly. The adhesive disclosed by the invention is processed without drying, and is high in speed, wide in application range of base materials and low in cost.
(2) The adhesive disclosed by the invention is single-component, does not need to be used in a glue preparation manner, is convenient to use, and solves the problem of short service time of a double-component adhesive.
(3) The adhesive contains strongly polar and chemically active urethane groups (NHCOO) and isocyanate groups (NCO), can generate hydrogen bonds with an adhered material, and generates a high-molecular polymer with high polymerization force by reacting with moisture existing in air or adhered to the surface of the adhered material and extending a chain after initial adhesion is formed, so that the adhesion force, the heat resistance and the like are obviously improved.
The adhesive takes NCO end group prepolymer as a basic raw material, and is matched with additives such as antioxidant, accelerant, flatting agent and the like which do not react with isocyanate groups, so that the product has longer pot life and storage period. The adhesive disclosed by the invention has good elasticity and excellent chemical resistance at low temperature, the heating temperature of the adhesive is 80-110 ℃, and the low-temperature operation overcomes the defects that the commercially available single-component adhesive is difficult to process and is operated at high temperature.
Detailed Description
The invention is further described below. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
A preparation method of a single-component polyurethane adhesive for compounding plastic sports floors comprises the following steps:
s1, taking the polyol ester and the antioxidant according to the corresponding weight based on the total weight of the polyurethane adhesive, and putting the taken polyol ester and the antioxidant into a polymerization stirring reaction kettle;
s2, heating and melting materials in the polymerization stirring reaction kettle, stirring and mixing uniformly, vacuumizing to enable the vacuum degree in the reaction kettle to be below 50torr when the temperature of the materials reaches 110-120 ℃, then dehydrating, filling nitrogen to return to normal pressure after the reaction kettle is continuously in a negative pressure state for 1-3 hours, detecting the moisture value contained in the materials, ending the dehydration if the moisture value is lower than 300ppm (mg/kg), and returning to the negative pressure state to continue the dehydration if the moisture value is higher than 300ppm (mg/kg);
s3, after dehydration is finished, returning the reaction kettle to normal pressure, reducing the temperature to 60-70 ℃, introducing nitrogen to maintain the micro-positive pressure of the reaction kettle, taking diisocyanate with corresponding weight based on the total weight of the polyol ester in the step S1, putting the taken diisocyanate into a polymerization stirring reaction kettle, heating the reaction kettle, maintaining the reaction temperature at 100-110 ℃, and allowing the reaction time to be not less than 1 hour;
s4, detecting the weight percentage content NCO% of the isocyanate group every 20-30min in the reaction process of the step S3;
and S5, when the NCO% is lower than the theoretical value, adding a certain amount of catalyst and flatting agent into the reaction kettle, uniformly stirring, carrying out negative pressure defoaming and continuous reaction, and reacting until no bubble exists in the reaction kettle to obtain a viscous liquid product.
In the actual production process, the prepared adhesive product is colorless to yellow sticky liquid in appearance, the prepared adhesive product is measured and packaged after being filtered, and the finished product package needs to be sealed by inert gas. The adhesive disclosed by the invention is used without adhesive preparation, the problem of unstable quality of finished products caused by adhesive preparation can be reduced, the process is simple, the process is simplified, the production efficiency is high, and the production cost is reduced.
In the step S2, the moisture content of the material is measured by a Karl-Fischer moisture meter.
The formula for the theoretical value of NCO% is: (diisocyanate NCO addition weight-theoretical weight of polyol ester consumed NCO)/total weight of reactor contents. The actual NCO% is determined by di-n-butylamine titration, and the specific process is referred to the detection standard ISO 14896.
The polyol ester is any one or a mixture of at least two of polyethylene glycol butanediol adipate, neopentyl glycol phthalate, neopentyl glycol isophthalate, polypropylene oxide glycol (PPG) and trimethylolpropane dipropylene glycol adipate. The weight percentage of the polyol ester is 65-74.5 wt% based on the total weight of the polyurethane adhesive. The polyol ester is selected and matched with one or more polyol esters according to the product performance and the characteristics of the bonded substrate so as to adapt to the bonding of various substrates. Specifically, the molecular weight of the polyethylene glycol butanediol adipate is 2000, the molecular weight of the neopentyl glycol isophthalate is 1000, the molecular weight of the neopentyl glycol isophthalate is 2200, and the molecular weight of the trimethylolpropane dipropylene glycol adipate is 700, and the functionality is 2.6; the molecular weight of the polyoxypropylene glycol (PPG) is 1000, the purity is required to be more than 99.5%, and the water content is required to be less than 300 ppm.
The polyol ester can be prepared by self or purchased from the market, and the molecular weight and the acid value AV meet the requirements. The molecular weight is determined by the acetic anhydride-pyridine method, and the detection standard is established according to ASTM D6432. The acid number AV is determined by KOH titration and the standard of detection is established according to ASTM D4662.
In step S3, the diisocyanate is diphenylmethane diisocyanate (MDI), and an excess amount of the diisocyanate (MDI) is added in an amount of 1.7 to 2.0 times the total weight of the polyol ester. The molar ratio of the isocyanate group in the diisocyanate to the hydroxyl group in the polyol ester is 1.7-2.0: 1; the content of the diisocyanate is 25 to 35 wt% based on the total weight of the polyurethane adhesive, that is, the amount of the diisocyanate added is 25 to 34.5 wt% of the total weight of the polyurethane adhesive.
The antioxidant is a hindered phenol antioxidant, and is added in an amount of 0.1-0.3 wt% based on the total weight of the polyurethane adhesive, wherein the antioxidant is any one or a mixture of at least two of β (pentaerythritol 3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (CHINOX1010), β (octadecyl 3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (CHINOX 1076), and N, N' -bis [ β (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] -1, 6-hexanediamine (CHINOX 1098), and the antioxidant is further preferably CHINOX 1010.
The leveling agent is an acrylate copolymer polymer, preferably MODAF L OW resin, and is added in an amount of 0.02-0.1 wt% based on the total weight of the polyurethane adhesive, so that the leveling agent promotes the formation of a flat and uniform coating film in the film forming process of the adhesive, the surface tension of the adhesive can be effectively reduced, the leveling property and uniformity of the adhesive are improved, and the adhesive force is increased.
The catalyst is a mixture of an amine catalyst and a tin catalyst, and preferably the amine catalyst dimorpholinodiethylether and the tin catalyst are used simultaneously. The two catalysts are used simultaneously, so that the effects of promoting the rapid reaction of isocyanate groups and hydroxyl groups and the crosslinking reaction of the processed isocyanate groups and water vapor are achieved, and the curing and curing speed of the adhesive is promoted.
A single-component polyurethane adhesive for compounding plastic sports floors comprises the following components in percentage by weight: 65-74.5 wt% of polyol ester, 25-34.5 wt% of diisocyanate, 0.1-0.3 wt% of antioxidant, 0.02-0.1 wt% of catalyst and 0.10-0.30 wt% of flatting agent.
The polyurethane adhesive is prepared from polyol ester and diisocyanate serving as basic raw materials, an antioxidant, a catalyst and a flatting agent through high-temperature polymerization reaction, and a polyurethane prepolymer with the solid content of 100 percent is prepared. The solid content is 100%, no solvent is contained, the production process has no solvent taste, and the method is safe and environment-friendly.
The performance test standards used in the present invention are:
1. the method for measuring the physical properties of the film comprises coating adhesive on release paper to obtain film, aging at room temperature of 23 deg.C and relative humidity of 50% for 96hr, testing the cut pieces of the film with an electronic tensile tester at a tensile rate of 200mm/min, wherein the unit is (Kg/cm), the modulus is 100%, the tensile strength is TS (tensile strength), and the elongation is E L (elongation)2) Reference is made to the standard ASTM D-412.
2. Softening point, melting point: softening point: using an oven method to cut the adhesive film into pieces, weighing corresponding weights according to a film thickness and a weight conversion table (45 grams per square centimeter load), clamping the weights below the test piece, fixing the test piece above the oven, starting heating, wherein the heating rate is 2 ℃/min, and recording the temperature of the test piece beginning to extend and break, namely the softening point and the melting point of the test piece.
Example 1
The reaction vessel was charged with polyoxypropylene glycol, polyethylene glycol butylene adipate, and trimethylolpropane dipropylene glycol adipate, and further charged with an antioxidant.
Heating and melting the raw materials in the polymerization reaction kettle, stirring and mixing uniformly, slowly heating to ensure that the material temperature reaches 110-120 ℃, vacuumizing to start dehydration to be less than 300ppm, and finishing dehydration.
Returning to normal pressure in the reaction kettle after dehydration is finished, reducing the temperature to 60-70 ℃, introducing nitrogen to maintain the micro-positive pressure of the reaction kettle, calculating the equivalent of the required consumed diisocyanate (MDI) according to the molecular weight of the polyol ester, adding excessive diisocyanate with the amount of 1.7-2.0 times of the equivalent of the polyol ester, heating the reaction kettle, maintaining the reaction temperature at 100-110 ℃, detecting the weight percentage content NCO of isocyanate groups at intervals of 20-30min, adding a catalyst and a leveling agent into the reaction kettle when the NCO% reaches a theoretical value, uniformly stirring, starting negative pressure defoaming, and continuously reacting until no bubble reaction is finished in the reaction kettle, thereby obtaining a viscous liquid with a colorless to yellow product appearance, wherein the equivalent ratio of the isocyanate groups to the hydroxyl groups is 1.76:1, the theoretical NCO% is 3.77%, the diisocyanate is diphenylmethane diisocyanate (MDI), the antioxidant is a hindered phenol antioxidant CHINOX1010, and the amine catalyst is amine catalyst (such as amine dimorpholine diethyl ether DMDEE) and a tin catalyst (such as TMG 129) and the basic weight ratio of acrylate copolymer (MODOW) is as shown in the following formula:
table 1 example 1 basic formulation of the product
The performance tests are shown in table 4.
The suggested processing method for applying the single-component polyurethane adhesive for compounding the plastic sports floor to compounding the sports floor is as follows:
step 1, glue melting: a pressure disc type melt adhesive machine is adopted, and the melt adhesive temperature is set to be 80-110 ℃.
Step 2, gluing and compounding: a two-roller gluing compound machine is adopted, after solid glue is heated and melted in a glue melting machine, a gluing process is performed by roller coating, so that the glue is uniformly coated on a TPE (thermoplastic elastomer)/EVA (ethylene vinyl acetate copolymer)/PVC (polyvinyl chloride) foaming buffer layer of the plastic sports floor, the temperature of a gluing roller is set to be 80-110 ℃, and the gluing amount is controlled to be 35-50 g/m through a two-roller gap and a differential speed2And (4) compounding the fiber reinforced layer, wherein the gluing amount is adjusted according to the flatness of the bonding surface.
And 3, standing the mixture after compounding and curing the mixture at room temperature.
Example 2
This example is the same as the process of example 1, with an equivalent ratio of isocyanate groups to hydroxyl groups of 1.9:1, a theoretical NCO% of 5.37%, and the basic formulation of the product of this example is as follows (by weight):
table 2 example 2 basic product formulation
| Formulation of | Weight (Kg) | Content (WT%) |
| Polyoxypropylene diol | 700 | 41.90 |
| Polyneopentyl glycol phthalate | 300 | 17.96 |
| Polytrimethylolpropane dipropylene glycol adipate | 100 | 5.99 |
| Diphenylmethane diisocyanate (MDI) | 563.2 | 33.71 |
| Antioxidant agent | 3.3 | 0.20 |
| Amine catalysts | 0.5 | 0.03 |
| Tin catalyst | 0.5 | 0.03 |
| Leveling agent | 3.3 | 0.20 |
The performance tests are shown in table 4.
Example 3
This example is the same as the example 1, the equivalent ratio of isocyanate group to hydroxyl group in the formulation is 1.86:1, the theoretical NCO% is 4.06%, the basic formulation of this example is as follows (weight ratio):
table 3 example 3 basic product formulation
| Formulation of | Weight (Kg) | Content (WT%) |
| Polyoxypropylene diol | 300 | 29.36 |
| Polyisophthalic acid neopentyl glycol adipate | 400 | 39.15 |
| Polytrimethylolpropane dipropylene glycol adipate | 50 | 4.89 |
| Diphenylmethane diisocyanate (MDI) | 267.2 | 26.15 |
| Antioxidant agent | 2.0 | 0.20 |
| Amine catalysts | 0.3 | 0.03 |
| Tin catalyst | 0.3 | 0.03 |
| Leveling agent | 2.0 | 0.20 |
The performance tests are shown in table 4.
TABLE 4 Performance test Table for one-component polyurethane adhesives prepared in examples 1 to 3
| Examples | 100％M | TS | EL | Softening point | Melting Point |
| kgf/cm2 | kgf/cm2 | ％ | ℃ | ℃ | |
| Example 1 | 38.67 | 313.33 | 621.55 | 155 | 184 |
| Example 2 | 57.78 | 377.78 | 455.10 | 160 | 193 |
| Example 3 | 45.05 | 349.55 | 477.05 | 160 | 189 |
Table 4 shows the statistics of the analysis data of the physical properties of the products obtained in examples 1 to 3. As can be seen from Table 4, the tensile strength after aging reached 300kgf/cm2The softening point ranges are above 140 ℃, which shows that the product has excellent physical adhesive strength and good heat resistance.
In conclusion, the solid content of the adhesive product is 100%, the adhesive product is different from solvent-based and solvent-free two-component adhesives commonly used in the market at present, the problems of safety and environmental protection of the solvent-based adhesive are solved, the adhesive preparation operation is not needed during use, the problem of unstable quality of finished products caused by adhesive preparation can be reduced, the process is simple, the production efficiency is high, the production cost is reduced, the adhesive product is suitable for composite processing of plastic sports floors, and the application prospect is good.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a single-component polyurethane adhesive for compounding plastic sports floors is characterized by comprising the following steps:
s1, taking the polyol ester and the antioxidant according to the corresponding weight based on the total weight of the polyurethane adhesive, and putting the taken polyol ester and the antioxidant into a polymerization stirring reaction kettle;
s2, heating and melting materials in the polymerization stirring reaction kettle, stirring and mixing uniformly, vacuumizing to enable the vacuum degree in the reaction kettle to be below 50torr when the temperature of the materials reaches 110-120 ℃, then dehydrating, filling nitrogen to return to normal pressure after the reaction kettle is continuously in a negative pressure state for 1-3 hours, detecting the moisture value contained in the materials, ending the dehydration if the moisture value is lower than 300ppm (mg/kg), and returning to the negative pressure state to continue the dehydration if the moisture value is higher than 300ppm (mg/kg);
s3, after dehydration is finished, returning the reaction kettle to normal pressure, reducing the temperature to 60-70 ℃, introducing nitrogen to maintain the micro-positive pressure of the reaction kettle, taking diisocyanate with corresponding weight based on the total weight of the polyol ester in the step S1, putting the taken diisocyanate into a polymerization stirring reaction kettle, heating the reaction kettle, maintaining the reaction temperature at 100-110 ℃, and allowing the reaction time to be not less than 1 hour;
s4, detecting the weight percentage content NCO% of the isocyanate group every 20-30min in the reaction process of the step S3;
and S5, when the NCO% is lower than the theoretical value, adding a certain amount of catalyst and flatting agent into the reaction kettle, uniformly stirring, carrying out negative pressure defoaming and continuous reaction, and reacting until no bubble exists in the reaction kettle to obtain a viscous liquid product.
2. The method for preparing the one-component polyurethane adhesive for plastic sports floor composition as claimed in claim 1, wherein the polyol ester is any one or a mixture of at least two of polybutylene glycol adipate, neopentyl glycol phthalate, neopentyl glycol isophthalate, polyoxypropylene glycol, and trimethylolpropane dipropylene glycol adipate.
3. The method for preparing the one-component polyurethane adhesive for plastic sports floor composition as claimed in claim 1, wherein the antioxidant is hindered phenol antioxidant; the leveling agent is acrylate copolymer polymer.
4. The method as claimed in claim 1, wherein the polyol ester is 65-74.5 wt% of the total weight of the polyurethane adhesive, the antioxidant is 0.1-0.3 wt% of the total weight of the polyurethane adhesive, and the diisocyanate is 25-34.5 wt% of the total weight of the polyurethane adhesive.
5. The method as claimed in claim 1, wherein the step S5 comprises adding 0.02-0.1 wt% of catalyst and 0.10-0.30 wt% of leveling agent into the reaction kettle, based on the total weight of the polyurethane adhesive.
6. The method as claimed in claim 1, wherein in the step S3, the diisocyanate is diphenylmethane diisocyanate (MDI), and the excess diisocyanate (MDI) is added in an amount of 1.7 to 2.0 times the total weight of the polyol ester.
7. The method as claimed in claim 1, wherein the catalyst is a mixture of amine catalyst and tin catalyst.
8. The single-component polyurethane adhesive for compounding the plastic sports floor is characterized by comprising the following components in percentage by weight: 65-74.5 wt% of polyol ester, 25-34.5 wt% of diisocyanate, 0.1-0.3 wt% of antioxidant, 0.02-0.1 wt% of catalyst and 0.10-0.30 wt% of flatting agent.
9. The single-component polyurethane adhesive for compounding the plastic sports floor as claimed in claim 8, wherein the polyurethane adhesive is a polyurethane prepolymer with a solid content of 100% prepared by high temperature polymerization reaction of polyol ester and diisocyanate as basic raw materials, and an antioxidant, a catalyst and a leveling agent.
10. The one-component polyurethane adhesive for plastic sports floor composition as claimed in claim 8, wherein the polyol ester is any one or a mixture of at least two of polyethylene glycol butylene adipate, neopentyl glycol phthalate, neopentyl glycol isophthalate, polyoxypropylene glycol, and trimethylolpropane dipropylene glycol adipate; the catalyst is a mixture of amine catalyst and tin catalyst.
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| CN109370504A (en) * | 2018-10-09 | 2019-02-22 | 高鼎精细化工(昆山)有限公司 | A kind of photovoltaic component back plate is compound to use one-component solvent-free polyurethane adhesive and preparation method |
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| CN113878943B (en) * | 2021-09-30 | 2023-09-01 | 东莞佰得新材料科技有限公司 | Soft and hard composite material production process, obtained material, application and production line |
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