Preparation method and application of washing-resistant, temperature-change-resistant and fast-curing hot melt adhesive

By controlling the temperature in the reactor and adding appropriate amounts of paraffin, tackifying resin, antioxidant and polar wax, the percentages of tackifying resin 40%~70%, elastic polymer 18%~30%, paraffin 10 were prepared by controlling the temperature in the reactor and adding appropriate amounts of paraffin, tackifying resin, antioxidant and polar wax. %~25%, polar wax 1%~15% hot melt adhesive solves the problem of insufficient solidification of hot melt adhesive in high temperature environments, realizes the stable adhesion performance of hot melt tape in harsh environments, and improves the Waterproof performance of outdoor equipment.

CN119161837APending Publication Date: 2024-12-20FOSHAN BEILIXIN NEW MATERIAL TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202411422811.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-12
Publication Date
2024-12-20

AI Technical Summary

Technical Problem

The existing hot melt adhesive is difficult to completely solidify in high-temperature environments, resulting in the waterproof overlap tape being easily peeled off under the action of external forces, making it difficult to achieve continuous and stable waterproof overlap, affecting the waterproof performance of outdoor equipment.

Method used

A hot melt adhesive preparation method that is resistant to water washing, temperature change and rapid curing is adopted, including adding paraffin, tackifying resin, and antioxidant to the preheated reactor, stirring and vacuuming at high temperature, and then adding elasticity Polymer polymers and polar waxes, control temperature and viscosity to ensure uniform mixing and stability of materials, and finally obtain the percentage of compositions of 40%~70%, elastic polymers 18%~30%, paraffin 10 %~25%, polar wax 1%~15%, antioxidant 0.1%~1.0%.

Benefits of technology

The rapid curing and efficient adhesion of hot melt adhesive is achieved. The protective adhesion of hot melt adhesive tape at the joints of outdoor equipment can maintain stable and good adhesion performance after low temperature, high temperature and water washing treatment, improving the waterproofing of outdoor equipment, Wind resistance and durability.

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Abstract

The invention discloses a preparation method and application of a washing-resistant, temperature-change-resistant and rapidly-cured hot melt adhesive, and belongs to the technical field of hot melt adhesives, the preparation method comprises the following steps: S1, adding paraffin, tackifying resin and an antioxidant into a preheated reaction kettle, stirring, and continuously heating in the stirring process; s2, after all the materials in the reaction kettle are heated to be molten, adding an elastic high-molecular polymer, continuously stirring, keeping constant-temperature heating, and vacuumizing the reaction kettle; s3, after all the materials in the reaction kettle are heated to be molten, polar wax and tackifying resin are added and continuously stirred, constant-temperature heating is kept, and the reaction kettle is vacuumized; s4, heating all the materials until the materials are molten, and uniformly stirring to obtain a hot melt adhesive; the hot melt adhesive is applied to manufacturing of the hot melt adhesive tape, and the hot melt adhesive tape is applied to protective adhesion of joints of outdoor equipment. The hot melt adhesive tape provided by the invention can improve the waterproof and windproof performance and durability of outdoor equipment.
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Description

Technical Field

[0001] The invention relates to the technical field of hot melt adhesives, and in particular to a preparation method and application of a hot melt adhesive that is resistant to water washing, temperature change and rapid curing. Background Art

[0002] Outdoor equipment such as waterproof clothing, tents, protective covers for weapons or engineering equipment usually require good waterproof and windproof properties. They are usually made of waterproof fabrics, and waterproof tapes are needed at the seams of the waterproof fabrics for waterproof bonding. The surface of the waterproof fabric is usually coated with a coating that prevents moisture from penetrating and causes moisture to roll off in the form of water droplets. These coatings reduce the adhesion of sticky materials on the surface of the waterproof fabric, and waterproof tapes usually use sticky materials such as hot melt adhesives to achieve waterproof bonding. In addition, outdoor equipment needs to be frequently used in harsh environments such as strong winds, heavy rains, low temperatures, and high temperatures. High requirements are placed on the low-temperature or high-temperature bonding effect and washability of the waterproof tape. It is necessary to ensure that the waterproof tape maintains stable and good adhesion in harsh environments and during long-term use. If the waterproof tape has insufficient adhesion on the surface of the waterproof fabric, it is easy to debond during use or cleaning, causing moisture to penetrate inward from the seams of the outdoor equipment, affecting the waterproof performance of the outdoor equipment.

[0003] Based on the above situation, a Chinese patent with announcement number CN113956825A discloses a hot melt adhesive and a waterproof overlapping tape, which include the following components in percentage: SIS elastomer 20-40%, SBS 2-10%, hydrogenated C5 resin 10-30%, hydrogenated C9 resin 10-30%, rosin resin 5-10%, cyclohexane oil 10-20%, antioxidant 0.5-1%; hydrogenated C5 resin is compatible with rubber segment I / B segment in SIS / SBS ​​elastomer, and hydrogenated C9 resin is compatible with rubber segment S segment in SIS / SBS ​​elastomer; the preparation method includes the following steps: step S1, stirring each component in a stirring kettle, step S2, after stirring in step S1, waiting until it is transparent and free of particles to obtain a hot melt adhesive; the hot melt adhesive is coated on the HDPE coil layer as a hot melt adhesive layer by a high-temperature glue coating device to obtain a waterproof overlapping tape.

[0004] The above-mentioned waterproof overlapping tape is adhered to the application part and compacted to achieve waterproof overlapping after tearing off the surface release film. It can be seen that the waterproof overlapping tape has certain adhesion properties in a room temperature environment. Although its surface is coated with hot melt adhesive, it is foreseeable that the waterproof overlapping tape can have better adhesion properties through hot pressing for waterproof overlapping. However, since hot melt adhesives have adhesion properties in a room temperature environment, they are difficult to completely cure in a high temperature or even room temperature environment, which affects the adhesion properties of the waterproof overlapping tape, causing the waterproof overlapping tape to be easily peeled off under the action of external force, and it is difficult to achieve continuous and stable waterproof overlapping. Therefore, the above-mentioned hot melt adhesives and waterproof overlapping tapes still have room for improvement. Summary of the invention

[0005] In view of the technical defects existing in the background technology, the present invention proposes a method for preparing a hot melt adhesive that is resistant to water washing, temperature change and fast curing and its application, which solves the above technical problems and meets the actual needs. The specific technical solution is as follows: A method for preparing a hot melt adhesive that is resistant to water washing, temperature change and rapid curing, comprising the following steps: S1. Add paraffin wax, tackifying resin and antioxidant into the preheated reactor and stir, and continue heating to 130-150°C during stirring; S2. After all materials in the reactor are heated to melt, add the elastic polymer and continue stirring, keep the temperature of the materials at 130-150°C and evacuate the reactor; S3. After all materials in the reactor are heated to melt, add polar wax and tackifying resin and continue stirring, keep the material temperature at 110-120°C and evacuate the reactor; S4, after all materials are heated to melt and stirred evenly, hot melt adhesive is obtained; The hot melt adhesive comprises the following components by mass percentage: 40% to 70% tackifying resin, 18% to 30% elastic high molecular polymer, 10% to 25% paraffin wax, 1% to 15% polar wax, and 0.1% to 1.0% antioxidant.

[0006] As a further technical solution of the present invention, in step S1 and step S3, the ratio of the added amount of the tackifying resin is 1:(1~2).

[0007] As a further technical solution of the present invention, the tackifying resin is selected from hydrogenated petroleum resin, light-colored rosin resin, or a mixture of the two.

[0008] As a further technical solution of the present invention, the polar wax is selected from polar copolymer wax, oxidized polyethylene wax, and polar montan wax.

[0009] As a further technical solution of the present invention, the elastic high molecular polymer is selected from one of styrene-isoprene-styrene triblock copolymer and styrene-butadiene-styrene triblock copolymer or a mixture of two thereof.

[0010] As a further technical solution of the present invention, the antioxidant is selected from one of the antioxidant (168) and the antioxidant (1010), or a mixture of the two.

[0011] As a further technical solution of the present invention, in steps S2 and S3, the vacuum degree of the reactor during evacuation is -0.08 MPa to -0.1 MPa.

[0012] An application of hot melt adhesive, wherein the hot melt adhesive is used to make hot melt adhesive tape, and the hot melt adhesive tape is used for protective adhesion at seam positions of outdoor equipment.

[0013] As a further technical solution of the present invention, the hot melt tape is prepared by the following method: the hot melt adhesive is heated until it is molten and then evenly coated on the surface of a carrier sheet, and after the hot melt adhesive is solidified, it is cut and rolled to obtain a hot melt tape composed of the hot melt adhesive and the carrier sheet.

[0014] As a further technical solution of the present invention, the following application method of the hot melt tape is included: covering the side of the hot melt tape coated with hot melt adhesive on the seam position of the substrate of the outdoor equipment that needs to be bonded, heating and pressing the hot melt adhesive with a hot press to melt the hot melt adhesive, and completing the bonding of the substrate seam position after the hot melt adhesive is re-solidified.

[0015] The beneficial effects of the present invention are: The hot melt adhesive of the present invention has the advantages of fast curing speed, water washing resistance, low temperature resistance and high temperature resistance. The hot melt adhesive can be efficiently coated on the surface of a carrier sheet to produce a hot melt tape through rapid curing, and the hot melt adhesive will not stick to the back of the hot melt tape, thereby improving the production efficiency of the hot melt tape. In addition, the hot melt tape is used for protective adhesion at the seam positions of outdoor equipment. The positions protected by the hot melt tape still maintain stable and good adhesion properties after water washing, low temperature and high temperature treatments, and can well cope with the harsh use environment of the outdoor equipment, thereby improving the waterproof and windproof properties and durability of the outdoor equipment. DETAILED DESCRIPTION

[0016] The implementation mode of the present invention is described below in conjunction with relevant embodiments. The implementation mode of the present invention is not limited to the following embodiments, and the present invention relates to relevant necessary components in the technical field, which should be regarded as the known technology in the technical field and can be known and mastered by the technical personnel in the technical field.

[0017] A method for preparing a hot melt adhesive that is resistant to water washing, temperature change and rapid curing, comprising the following steps: S1. Add paraffin wax, tackifying resin and antioxidant into the preheated reactor and stir, and continue heating to 130-150°C during stirring; S2. After all materials in the reactor are heated to melt, add the elastic polymer and continue stirring, keep the temperature of the materials at 130-150°C and evacuate the reactor to a vacuum degree of -0.08MPa--0.1MPa; S3. After all materials in the reactor are heated to melt, add polar wax and tackifying resin and continue stirring, keep the material temperature at 110-120°C and evacuate the reactor to a vacuum degree of -0.08MPa--0.1MPa; S4, after all materials are heated to melt and stirred evenly, hot melt adhesive is obtained; The hot melt adhesive includes the following components in percentage by mass: 40% to 70% tackifying resin, 18% to 30% elastic high molecular polymer, 10% to 25% paraffin wax, 1% to 15% polar wax, and 0.1% to 1.0% antioxidant.

[0018] In the process of preparing the hot melt adhesive of the present invention, batch mixing is performed according to the characteristics of the raw materials, which is beneficial to improving the stability and quality of the hot melt adhesive; in step S1, the reactor is preferably preheated to 100°C. By preheating the reactor, the materials are quickly preheated to a certain temperature after entering the reactor, which is beneficial to the efficient heating of the materials to melt in the subsequent heating process, and the efficiency of heating the materials to melt is improved. Among them, paraffin wax and tackifying resin are low molecular polymers, and the viscosity is low after being heated to melt. Since the viscosity of the materials is low and easy to mix evenly at this time, the stirring speed can be set within a lower range, and the rotation speed is preferably 30r / min. Step S1 is to first put paraffin wax and tackifying resin into the reactor to form a basic melt with low viscosity, which is beneficial to reduce the overall viscosity of the materials in the next step of melting the elastic polymer, reduce the resistance of the stirring motor, and make the elastic polymer more evenly mixed after melting. In addition, the addition of antioxidants can reduce the oxidation reaction of the materials, chemical bond breaking and other phenomena during the entire high-temperature heating reaction process, thereby ensuring the stability of the materials in the reactor.

[0019] In the above steps, paraffin, tackifying resin and antioxidant have been completely heated to a molten state in the reactor to form a basic melt. In step S2, the material melting effect is optimal when the mass ratio of the basic melt to the elastic high molecular polymer is 1.7:1. During the mixing, heating and stirring process, the shearing effect of the stirring paddle on the elastic high molecular polymer will not be affected by the low viscosity, nor will the current of the stirring motor be too high due to the high viscosity. At this time, the stirring speed is increased to 50r / min, or the stirring speed is increased according to the maximum limited current of the motor in the stirring equipment, and the mixing effect of the material is improved by increasing the stirring speed; during the heating and stirring process, the material temperature needs to be maintained at 130~150℃. If the temperature is too high, oxidation reaction or chemical bond breaking is likely to occur during the melting process of the elastic high molecular polymer. If the temperature is too low, it is not conducive to the transformation of the elastic high molecular polymer to a molten state. Improper temperature control will affect the quality of the hot melt adhesive product. In addition, vacuuming can cooperate with antioxidants to reduce oxidation reactions, chemical bond breaking and other phenomena, thereby ensuring the stability of the material in the reactor.

[0020] In step S3, since the polar wax has poor stability at high temperature, the polar wax is mixed with the material at the end. At the same time, part of the tackifying resin is added to the reactor together with the polar wax, so that the material in the reactor can be reduced to a more suitable temperature and viscosity, which is conducive to the uniform mixing of the polar wax and other materials. During the mixing and stirring process, the stirring speed is maintained at 50r / min or higher to ensure that the raw materials are efficiently mixed and uniformly mixed, and the temperature in the reactor is maintained at 110-120°C to avoid excessive temperature and cooperate with the antioxidant through vacuuming to jointly reduce the oxidation reaction of the polar wax, the breakage of chemical bonds and the like, ensure the stability of the material in the reactor and avoid the appearance of bubbles in the finished product.

[0021] In step S4, all materials are added to the reactor in sequence and heated and stirred to obtain a hot melt adhesive. Among the materials constituting the hot melt adhesive, the tackifying resin mainly plays a role in increasing the viscosity of the hot melt adhesive, so that the hot melt adhesive can better adhere to the surface of the substrate when it is molten. The tackifying resin can also improve the high temperature resistance and cohesion of the hot melt adhesive, so that it can maintain stable and good adhesion performance in a high temperature environment; the elastic polymer in the hot melt adhesive mainly plays a bonding role, so that the hot melt adhesive maintains stable adhesion performance in environments with different temperatures. The elastic polymer can also make the cured hot melt adhesive softer and more conformable, and at the same time improve the high temperature resistance and cohesion of the hot melt adhesive; paraffin wax has a great effect on the hot melt adhesive. The main function is to reduce viscosity and quickly solidify, so that the hot melt adhesive will not have initial tack after solidification. Paraffin wax can also improve the thermal stability of the hot melt adhesive, so that it can maintain good adhesion in a high temperature environment and is not prone to deformation or failure. Polar wax can adjust the initial tack of the hot melt adhesive. By cooperating with paraffin wax, the hot melt adhesive can be quickly solidified and no longer have initial tack after solidification, so that the hot melt tape does not need to be isolated with release paper during the winding process. The antioxidant is selected from one of the antioxidants (168) and antioxidants (1010) or a mixture of the two. The antioxidant mainly plays a role in reducing the oxidation of materials in the reactor during high-temperature stirring and use at room temperature.

[0022] As one of the preferred embodiments of the present invention, in step S1 and step S3, the ratio of the added amount of the tackifier resin is 1:(1~2); the tackifier resin of the present invention is divided into two parts and added to the reactor in steps S1 and S3 respectively, wherein the tackifier resin is added in step S1 to form a basic melt with low viscosity with paraffin wax, which is beneficial to the subsequent elastic high molecular polymer being added to the reactor and can be quickly mixed evenly, thereby improving the processing efficiency of the hot melt adhesive; the tackifier resin is added in step S3 to reduce the viscosity and temperature of the melt system in the reactor, so that the polar wax can be efficiently mixed with other materials, thereby avoiding oxidation reactions, chemical bond breakage and the like of the polar wax, and improving the quality of the hot melt adhesive product.

[0023] As one of the preferred embodiments of the present invention, the tackifying resin is selected from hydrogenated petroleum resin, light-colored rosin resin, or a mixture of the two; hydrogenated petroleum resin has good weather resistance, adhesion, water resistance and other properties, which can make the hot melt adhesive maintain stable properties such as waterproofness, adhesion, durability, etc. during long-term use. The hydrogenated petroleum resin also has good compatibility and can be easily mixed with other materials that make up the hot melt adhesive to ensure the uniformity and stability of the hot melt adhesive; the light-colored rosin resin has good hot melt and good adhesion. The light-colored rosin resin can melt quickly during heating and tightly combine with the surface of the adherend to provide strong adhesion. The light-colored rosin resin also has good viscosity adjustment ability, which can improve the flexibility of the hot melt adhesive processing process by adjusting the viscosity of the melt in the reactor, thereby improving the processing efficiency of the hot melt adhesive.

[0024] As one of the preferred embodiments of the present invention, the polar wax is selected from one of polar copolymer wax, oxidized polyethylene wax and polar montan wax; the polar copolymer wax has good compatibility due to the presence of its polar groups, and can be well dispersed in the hot melt adhesive system, which helps to improve the uniformity and stability of the hot melt adhesive. The polar copolymer wax also has the function of improving the wettability of the hot melt adhesive and adjusting the fluidity of the hot melt adhesive. The adhesion effect of the hot melt adhesive is enhanced by improving the wettability of the hot melt adhesive, and the adhesion effect of the hot melt adhesive is improved by adjusting the fluidity of the hot melt adhesive to make the molten hot melt adhesive more easily penetrate on the surface of the substrate; the polar group of the oxidized polyethylene wax can improve its compatibility with other materials, thereby improving the wettability and dispersibility of the hot melt adhesive, which helps to improve the adhesion effect of the hot melt adhesive. The oxidized polyethylene wax can also prevent the hot melt adhesive from agglomerating and becoming sticky on the surface during storage, so that the solidified hot melt adhesive no longer has initial viscosity, so that the hot melt adhesive tape does not need to be isolated with release paper during the winding process.

[0025] As one of the preferred embodiments of the present invention, the elastic high molecular polymer is selected from styrene-isoprene-styrene triblock copolymer, styrene-butadiene-styrene triblock copolymer, or a mixture of the two; The styrene-isoprene-styrene triblock copolymer has a soft rubber segment in the middle and hard plastic segments on both sides. This structure gives it good elasticity and bonding strength, which can make the hot melt adhesive have excellent adhesion and flexibility. The styrene-isoprene-styrene triblock copolymer can also increase the curing speed of the hot melt adhesive and keep its performance stable in a low-temperature environment; the styrene-butadiene-styrene triblock copolymer has excellent tensile strength and surface friction coefficient, which can make the hot melt adhesive have higher strength and wear resistance. The styrene-butadiene-styrene triblock copolymer can also improve the processing and molding performance of the hot melt adhesive and keep its performance stable in a low-temperature environment.

[0026] Furthermore, the elastic macromolecular polymer preferably adopts a copolymer with a high styrene content, which can improve the strength, heat resistance and weather resistance of the hot melt adhesive.

[0027] The invention discloses an application of hot melt adhesive. The hot melt adhesive is used to make hot melt adhesive tape. The hot melt adhesive tape is made by the following method: the hot melt adhesive is heated to be molten and then evenly coated on the surface of a carrier sheet. After the hot melt adhesive is solidified, it is cut and rolled to obtain a hot melt adhesive tape composed of the hot melt adhesive and the carrier sheet.

[0028] After the hot melt adhesive of the present invention is heated to a molten state, it is evenly coated on the surface of a carrier sheet by a knife coating machine, the heating temperature is 160-170°C, the carrier sheet can be adaptively adjusted according to the material of the bonding substrate as needed, and the hot melt adhesive is solidified on the surface of the carrier sheet by slitting and winding to obtain a hot melt adhesive tape. During the winding process, the hot melt adhesive will not adhere to the back of the carrier sheet, so there is no need to cover the surface of the hot melt adhesive with release paper for isolation; in addition, after the hot melt adhesive is coated on the surface of the carrier sheet, the side coated with the hot melt adhesive can be folded in half to observe whether they are mutually adhered, thereby judging the anti-anti-sticking effect of the hot melt adhesive. After the hot melt adhesive of the present invention is coated on the surface of the carrier sheet, rapid solidification can be achieved, and the coating speed of the hot melt adhesive can reach 12-15 m / min, which can improve the production efficiency of the hot melt adhesive tape.

[0029] Furthermore, the hot melt tape is used for the protective adhesion of the seam position of outdoor equipment, including the following application method of the hot melt tape: covering the side of the hot melt tape coated with hot melt adhesive on the seam position of the substrate of the outdoor equipment to be adhered, heating and pressing the hot melt adhesive by a hot press to melt the hot melt adhesive, and completing the adhesion of the substrate seam position after the hot melt adhesive is re-solidified; the hot melt tape of the present invention is mainly used for the protective adhesion of the seam position of outdoor equipment such as waterproof clothing and tents. These waterproof equipment are more commonly made of polyurethane waterproof fabrics. The hot melt tape Polyurethane waterproof fabric can be used as a carrier sheet, and the hot melt tape is used to bond the seams of two pieces of polyurethane waterproof fabric through hot air seam sealing machine. The heating temperature is 430°C, the hot pressing speed is 12m / min, and the hot pressing pressure is 2MPa. The two pieces of polyurethane waterproof fabric can be bonded and the bonding position has a good waterproof effect. The polyurethane waterproof fabric and the polyurethane waterproof fabric bonded with the hot melt tape are subjected to a hydrostatic pressure test. The hydrostatic pressure of the two tests can reach 8000mmH2O.

[0030] The present invention is further described below by way of examples and comparative examples.

[0031] Example 1

[0032] S1. Add 17.5% paraffin wax, 20% hydrogenated petroleum resin, 0.3% antioxidant (168), and 0.2% antioxidant (1010) by mass into a reactor preheated to 100°C, stir at a speed of 30 r / min, and continue heating to 130-150°C during stirring; S2. After all the materials in the reactor are heated to melt, 8% of styrene-isoprene-styrene triblock copolymer and 14% of styrene-butadiene-styrene triblock copolymer are added into the reactor in percentage by mass, and stirred continuously at a speed of 50 r / min, while maintaining the temperature of the materials at 130-150° C. and evacuating the reactor to a vacuum degree of -0.08 MPa; S3. After all the materials in the reactor are heated to melt, add 2.5% of polar copolymer wax, 17.5% of hydrogenated petroleum resin, and 20% of light-colored rosin resin in percentage by mass into the reactor and stir continuously at a speed of 50r / min. Keep the material temperature at 110-120°C and evacuate the reactor to a vacuum degree of -0.08MPa. S4, after all materials are heated to melt and stirred evenly, hot melt adhesive is obtained; S5. After the hot melt adhesive is heated to a molten state, it is evenly coated on the surface of the polyurethane waterproof fabric by a scraper coating machine. After the hot melt adhesive is solidified, it is cut and rolled to obtain a hot melt tape.

[0033] Example 2

[0034] S1. Add 17.5% paraffin wax, 20% hydrogenated petroleum resin, 0.3% antioxidant (168), and 0.2% antioxidant (1010) by mass into a reactor preheated to 100°C, stir at a speed of 30 r / min, and continue heating to 130-150°C during stirring; S2. After all the materials in the reactor are heated to melt, 8% of styrene-isoprene-styrene triblock copolymer and 14% of styrene-butadiene-styrene triblock copolymer are added into the reactor in percentage by mass, and stirred continuously at a speed of 50 r / min, while maintaining the temperature of the materials at 130-150° C. and evacuating the reactor to a vacuum degree of -0.08 MPa; S3. After all the materials in the reactor are heated to melt, add 5% of polar copolymer wax, 15% of hydrogenated petroleum resin, and 20% of light-colored rosin resin in percentage by mass into the reactor and stir continuously at a speed of 50r / min. Keep the material temperature at 110-120°C and evacuate the reactor to a vacuum degree of -0.08MPa. S4, after all materials are heated to melt and stirred evenly, hot melt adhesive is obtained; S5. After the hot melt adhesive is heated to a molten state, it is evenly coated on the surface of the polyurethane waterproof fabric by a scraper coating machine. After the hot melt adhesive is solidified, it is cut and rolled to obtain a hot melt tape.

[0035] Example 3

[0036] S1. Add 17.5% paraffin wax, 20% hydrogenated petroleum resin, 0.3% antioxidant (168), and 0.2% antioxidant (1010) by mass into a reactor preheated to 100°C, stir at a speed of 30 r / min, and continue heating to 130-150°C during stirring; S2. After all the materials in the reactor are heated to melt, 8% of styrene-isoprene-styrene triblock copolymer and 14% of styrene-butadiene-styrene triblock copolymer are added into the reactor in percentage by mass, and stirred continuously at a speed of 50 r / min, while maintaining the temperature of the materials at 130-150° C. and evacuating the reactor to a vacuum degree of -0.08 MPa; S3. After all the materials in the reactor are heated to melt, add 10% oxidized polyethylene wax, 12.5% ​​hydrogenated petroleum resin, and 17.5% light-colored rosin resin by mass percentage into the reactor and stir continuously at a speed of 50r / min, keep the material temperature at 110-120°C, and evacuate the reactor to a vacuum degree of -0.08MPa; S4, after all materials are heated to melt and stirred evenly, hot melt adhesive is obtained; S5. After the hot melt adhesive is heated to a molten state, it is evenly coated on the surface of the polyurethane waterproof fabric by a scraper coating machine. After the hot melt adhesive is solidified, it is cut and rolled to obtain a hot melt tape.

[0037] Comparative Example 1 S1. Add 17.5% paraffin wax, 20% hydrogenated petroleum resin, 5% polar copolymer wax, 0.3% antioxidant (168), and 0.2% antioxidant (1010) by mass into a reactor preheated to 100°C, stir at a speed of 30 r / min, and continue heating to 130-150°C during stirring; S2. After all the materials in the reactor are heated to melt, 8% of styrene-isoprene-styrene triblock copolymer and 14% of styrene-butadiene-styrene triblock copolymer are added into the reactor in percentage by mass, and stirred continuously at a speed of 50 r / min, while maintaining the temperature of the materials at 130-150° C. and evacuating the reactor to a vacuum degree of -0.08 MPa; S3. After all materials in the reactor are heated to melt, add 15% by mass of hydrogenated petroleum resin and 20% of light-colored rosin resin into the reactor and stir continuously at a speed of 50 r / min. Keep the material temperature at 110-120°C and evacuate the reactor to a vacuum degree of -0.08 MPa. S4, after all materials are heated to melt and stirred evenly, hot melt adhesive is obtained; S5. After the hot melt adhesive is heated to a molten state, it is evenly coated on the surface of the polyurethane waterproof fabric by a scraper coating machine. After the hot melt adhesive is solidified, it is cut and rolled to obtain a hot melt tape.

[0038] Comparative Example 2 S1. Add 17.5% paraffin wax, 20% hydrogenated petroleum resin, 0.3% antioxidant (168), and 0.2% antioxidant (1010) by mass into a reactor preheated to 100°C, stir at a speed of 30 r / min, and continue heating to 130-150°C during stirring; S2. After all the materials in the reactor are heated to melt, 8% of styrene-isoprene-styrene triblock copolymer and 14% of styrene-butadiene-styrene triblock copolymer are added into the reactor in percentage by mass, and stirred continuously at a speed of 50 r / min, while maintaining the temperature of the materials at 130-150° C. and evacuating the reactor to a vacuum degree of -0.08 MPa; S3. After all materials in the reactor are heated to melt, add 20% by mass of hydrogenated petroleum resin and 20% of light-colored rosin resin into the reactor and stir continuously at a speed of 50 r / min. Keep the material temperature at 110-120°C and evacuate the reactor to a vacuum degree of -0.08 MPa. S4, after all materials are heated to melt and stirred evenly, hot melt adhesive is obtained; S5. After the hot melt adhesive is heated to a molten state, it is evenly coated on the surface of the polyurethane waterproof fabric by a scraper coating machine. After the hot melt adhesive is solidified, it is cut and rolled to obtain a hot melt tape.

[0039] Comparative Example 3 S1. Add 43.5% by mass of hydrogenated petroleum resin, 0.3% of antioxidant (168), and 0.2% of antioxidant (1010) into a reactor preheated to 100°C, stir at a speed of 30 r / min, and continue heating to 130-150°C during stirring; S2. After all the materials in the reactor are heated to melt, 10% of styrene-isoprene-styrene triblock copolymer and 26% of styrene-butadiene-styrene triblock copolymer are added into the reactor in percentage by mass, and stirred continuously at a speed of 50 r / min, while maintaining the temperature of the materials at 130-150° C. and evacuating the reactor to a vacuum degree of -0.08 MPa; S3. After all materials in the reactor are heated to melt, add 20% of light-colored rosin resin by mass percentage into the reactor and stir continuously at a speed of 50r / min, keep the material temperature at 110-120°C and evacuate the reactor to a vacuum degree of -0.08MPa; S4, after all materials are heated to melt and stirred evenly, hot melt adhesive is obtained; S5. After the hot melt adhesive is heated to a molten state, it is evenly coated on the surface of the polyurethane waterproof fabric by a scraper coating machine. After the hot melt adhesive is solidified, it is cut and rolled to obtain a hot melt tape.

[0040] In all the above embodiments and comparative examples, after the hot melt adhesive is coated on the surface of the polyurethane waterproof fabric, the side coated with the hot melt adhesive is folded in half to test the anti-sticking effect of the hot melt adhesive tape; several hot melt adhesive tapes obtained from all the above embodiments and comparative examples are used to hot-press and bond the seams of two pieces of polyurethane waterproof fabric for 10 seconds through a hot air seam sealing machine to obtain a test fabric. After the test fabric is cooled, it is placed at room temperature for 24 hours and the following tests are performed: 1. Test at room temperature. Peel off the hot melt tape from the surface of the test fabric. Observe the degree of damage to the test fabric caused by the adhesion between the hot melt tape and the test fabric during the peeling process, and record the peeling force during the peeling process. 2. Low temperature test: After placing the hot melt tape at a constant temperature of 0℃ for 24 hours, peel the hot melt tape from the surface of the test fabric, observe the degree of damage to the test fabric caused by the adhesion between the hot melt tape and the test fabric during the peeling process, and record the peeling force during the peeling process; 3. High temperature test: After placing the hot melt tape at a constant temperature of 60°C for 24 hours, peel the hot melt tape from the surface of the test fabric, observe the degree of damage to the test fabric caused by the adhesion between the hot melt tape and the test fabric during the peeling process, and record the peeling force during the peeling process; 4. Washing test: wash the hot melt tape in clean water at 40°C and dry it. Wash it 5 times and each time for 30 minutes. Then peel the hot melt tape from the surface of the test fabric. Observe the degree of damage to the test fabric caused by the adhesion between the hot melt tape and the test fabric during the peeling process, and record the peeling force during the peeling process.

[0041] The results of the above anti-sticking effect test, normal temperature test, low temperature test, high temperature test, and water washing test are recorded, and the recorded results are shown in Table 1 below:

[0042] Table 1 It should be noted that, in the description of the anti-anti-sticking effect in Table 1, "good" means that the hot-melt adhesive on the surface of the hot-melt tape does not adhere to each other after being folded in half, "general" means that the hot-melt adhesive on the surface of the hot-melt tape adheres to each other to a certain extent after being folded in half, and "poor" means that the hot-melt adhesive on the surface of the hot-melt tape adheres to each other seriously and is difficult to separate after being folded in half; in the description of the degree of damage to the test fabric in Table 1, "complete damage" means that the polyurethane waterproof fabric is completely destroyed during the peeling process of the hot-melt tape, and the polyurethane waterproof fabric is still completely and firmly adhered to the surface of the hot-melt tape after peeling, "partial damage" means that the polyurethane waterproof fabric is partially destroyed during the peeling process of the hot-melt tape, and the polyurethane waterproof fabric is partially firmly adhered to the surface of the hot-melt tape after peeling, and "no damage" means that the hot-melt tape can be completely peeled off, and the polyurethane waterproof fabric is not adhered to the surface of the hot-melt tape after peeling.

[0043] According to the data in Table 1, it can be seen that the hot-melt adhesive tapes of Examples 1 to 3 are prepared based on the technical solution of the present invention. These hot-melt adhesive tapes all show good anti-anti-sticking effect, that is, the hot-melt adhesive can be quickly solidified after coating, and these hot-melt adhesive tapes show good adhesion performance in normal temperature, low temperature, high temperature environment and after multiple washings. After the hot-melt adhesive tape is applied to the protective adhesion of the seam position of outdoor equipment, the outdoor equipment can cope with the harsh outdoor environment well; in addition, in Comparative Example 1, the polar wax is mixed in step S1, and the obtained hot-melt adhesive tape has low temperature resistance and high temperature resistance. , and water washing resistance are poor. This is because the polar wax is mixed into the melt system too early, and the high temperature causes part of the polar wax to be oxidized or the structure to be destroyed. In Comparative Example 2, no polar wax is added, and the performance of the obtained hot melt tape is similar to that of Comparative Example 1, and the anti-sticking effect is worse, which means that the polar wax has a significant effect on the anti-sticking effect, low-temperature resistance, high-temperature resistance, and water washing resistance of the hot melt adhesive. In Comparative Example 3, no paraffin wax and polar wax are added, and the anti-sticking effect and adhesion performance of the obtained hot melt tape are further deteriorated, and the hot melt tape is difficult to be used for protective adhesion at the seams of outdoor equipment.

[0044] The peeling force record results of the hot melt tape during the above test are shown in Table 2 below:

[0045] Table 2 It should be noted that the peeling force data of the hot melt tape in Table 2 are based on the above-mentioned four tests of normal temperature test, low temperature test, high temperature test and water washing test. It is known that Examples 1 to 3 completely destroyed the polyurethane waterproof fabric during the peeling test, so the peeling force data is only the force generated when the hot melt tape destroys the polyurethane waterproof fabric. It can be expected that if a material with higher strength is used as the carrier sheet of the hot melt tape and the substrate for bonding, the peeling force data obtained by the test will be higher; in addition, the peeling force of Examples 1 to 3 after the low temperature test, high temperature test and water washing test all showed a slight decrease. This is because the polyurethane waterproof fabric shows a decrease in strength in low temperature and high temperature environments and after multiple water washings, thereby reducing the peeling force of the hot melt tape.

[0046] The above is only a preferred embodiment of the present invention. It should be pointed out that ordinary technicians in this technical field can make several improvements and modifications without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing a hot melt adhesive that is resistant to water washing, temperature changes and rapid curing, characterized in that: The following steps are involved: S1. Add paraffin wax, tackifying resin and antioxidant into the preheated reactor and stir, and continue heating to 130-150°C during stirring; S2. After all materials in the reactor are heated to melt, add the elastic polymer and continue stirring, keep the temperature of the materials at 130-150°C and evacuate the reactor; S3. After all materials in the reactor are heated to melt, add polar wax and tackifying resin and continue stirring, keep the material temperature at 110-120°C and evacuate the reactor; S4, after all materials are heated to melt and stirred evenly, hot melt adhesive is obtained; The hot melt adhesive comprises the following components by mass percentage: 40% to 70% tackifying resin, 18% to 30% elastic high molecular polymer, 10% to 25% paraffin wax, 1% to 15% polar wax, and 0.1% to 1.0% antioxidant.

2. The method for preparing a hot melt adhesive that is resistant to water washing, temperature change and fast curing according to claim 1, characterized in that: In step S1 and step S3, the ratio of the added amount of the tackifying resin is 1:(1~2).

3. The method for preparing a hot melt adhesive that is resistant to water washing, temperature change and fast curing according to claim 1, characterized in that: The tackifying resin is selected from hydrogenated petroleum resin, light-colored rosin resin, or a mixture of the two.

4. The method for preparing a hot melt adhesive that is resistant to water washing, temperature change and fast curing according to claim 1, characterized in that: The polar wax is selected from polar copolymer wax, oxidized polyethylene wax and polar montan wax.

5. The method for preparing a hot melt adhesive that is resistant to water washing, temperature change and fast curing according to claim 1, characterized in that: The elastic high molecular polymer is selected from styrene-isoprene-styrene triblock copolymer, styrene-butadiene-styrene triblock copolymer, or a mixture of the two.

6. The method for preparing a hot melt adhesive that is resistant to water washing, temperature change and fast curing according to claim 1, characterized in that: The antioxidant is selected from one of antioxidant (168) and antioxidant (1010) or a mixture of the two.

7. The method for preparing a hot melt adhesive that is resistant to water washing, temperature change and fast curing according to claim 1, characterized in that: In steps S2 and S3, the vacuum degree of the reactor during evacuation is -0.08 MPa to -0.1 MPa.

8. An application of the hot melt adhesive according to any one of claims 1 to 7, characterized in that: The hot melt adhesive is used to make hot melt tape, and the hot melt tape is used for protective adhesion at the seam positions of outdoor equipment.

9. The use of the hot melt adhesive according to claim 8, characterized in that: The hot melt adhesive tape is prepared by the following method: the hot melt adhesive is heated to be molten and then evenly coated on the surface of a carrier sheet, and after the hot melt adhesive is solidified, it is cut and rolled to obtain a hot melt adhesive tape composed of the hot melt adhesive and the carrier sheet.

10. The use of the hot melt adhesive according to claim 9, characterized in that: The hot melt tape includes the following application method: covering the hot melt tape with one side coated with hot melt adhesive on the seam position of the substrate of the outdoor equipment to be bonded, heating and pressing the hot melt adhesive with a hot press to melt the hot melt adhesive, and completing the bonding of the substrate seam position after the hot melt adhesive is re-solidified.

Citation Information

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