CN110540818B - Non-reactive polyolefin hot melt adhesive, preparation method and application thereof - Google Patents
Non-reactive polyolefin hot melt adhesive, preparation method and application thereof Download PDFInfo
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- CN110540818B CN110540818B CN201910880954.9A CN201910880954A CN110540818B CN 110540818 B CN110540818 B CN 110540818B CN 201910880954 A CN201910880954 A CN 201910880954A CN 110540818 B CN110540818 B CN 110540818B
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/10—Homopolymers or copolymers of propene
- C09J123/12—Polypropene
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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
- C09J157/00—Adhesives based on unspecified polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09J157/02—Copolymers of mineral oil hydrocarbons
Abstract
The invention provides a preparation method and application of a non-reactive polyolefin hot melt adhesive with high softening point, low viscosity and good alkali resistance. The main raw materials comprise: 25-40 parts by weight of a polypropylene homopolymer; 10-25 parts by weight of an amorphous polyolefin resin; 30-50 parts by weight of tackifying resin; 5-10 parts of a viscosity regulator; 0.5-1 part by weight of heat-resistant stabilizer. The non-reactive polyolefin hot melt adhesive prepared by the invention is suitable for fixing the isolation paper in the alkaline battery, has lower viscosity which meets the requirement of a filling process, has good bonding performance on low-polarity base materials, and can still keep good bonding strength after alkali liquor treatment.
Description
Technical Field
The invention belongs to the technical field of hot melt adhesives, and particularly relates to a non-reactive polyolefin hot melt adhesive, and a preparation method and application thereof.
Background
In order to separate the positive electrode and the negative electrode in the alkaline battery, the separation paper needs to be fixed on the base, the separation paper is generally prepared by modifying PE, PP or fibers, belongs to a base material with lower polarity, and is in a weak alkaline solution environment, so that the adhesive for fixing and bonding is required to have the characteristics of good bonding effect and alkaline corrosion resistance, and simultaneously, the low dielectric constant is required to be met so as to reduce the energy loss in the battery.
The traditional alkaline battery is sealed by asphalt cement and epoxy cement, but the two have the defects of poor low-temperature flexibility, embrittlement at low temperature, adhesion peeling and the like, so that the leakage of the battery is caused, and the leakage is further replaced by solvent type polyethylene sealant. However, with the environmental protection requirement being more and more important, solvent-based products are gradually eliminated, and new sealants need to be found.
The polyolefin hot melt adhesive is the best choice, is an environment-friendly adhesive, has a good bonding effect on a base material with low polarity, and has good acid and alkali resistance and low dielectric constant. However, the viscosity of the existing non-reactive polyolefin adhesive is high and is not matched with the pouring process of the alkaline battery isolation paper.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a non-reactive hot melt adhesive with high softening point, low viscosity and good flowability, and a preparation method and an application thereof.
The invention provides a non-reactive polyolefin hot melt adhesive, which comprises the following components:
preferably, the softening point of the polypropylene homopolymer is 150-155 ℃, and the melt viscosity at 190 ℃ is 1000-4000 mPa & s.
Preferably, the amorphous polyolefin resin is amorphous polyolefin resin APAO.
Preferably, the softening point of the tackifying resin is 120 to 130 ℃.
Preferably, the tackifying resin is selected from hydrogenated C5 petroleum resins and/or hydrogenated C9 petroleum resins.
Preferably, the viscosity modifier is selected from a fischer-tropsch wax and/or a PE wax.
Preferably, the heat stabilizer is selected from the group consisting of tris [ 2.4-di-tert-butylphenyl ] phosphite) and/or tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] pentaerythritol ester.
The invention also provides a preparation method of the non-reactive polyolefin hot melt adhesive, which comprises the following steps:
heating and stirring a polypropylene homopolymer, amorphous polyolefin resin, tackifying resin, a viscosity regulator and a heat-resistant stabilizer until the polypropylene homopolymer, the amorphous polyolefin resin, the tackifying resin, the viscosity regulator and the heat-resistant stabilizer are dissolved, vacuumizing and continuously stirring, granulating and discharging after no bubbles exist in appearance, and thus obtaining the non-reactive polyolefin hot melt adhesive.
Preferably, the heating temperature is 170-190 ℃; vacuumizing until the vacuum degree is more than or equal to 0.09 MPa; the rotating speed of the continuous stirring is 40-45 r/min.
The invention also provides an application of the non-reactive polyolefin hot melt adhesive in an alkaline battery.
The invention provides a non-reactive polyolefin hot melt adhesive, which comprises the following components: 25-40 parts by weight of a polypropylene homopolymer; 10-25 parts by weight of an amorphous polyolefin resin; 30-40 parts by weight of tackifying resin; 5-10 parts of a viscosity regulator; 0.5-1 part by weight of heat-resistant stabilizer. Compared with the prior art, the preparation method takes the polypropylene homopolymer and the amorphous polyolefin resin as main raw materials, and simultaneously adds the tackifying resin, the viscosity regulator and the heat-resistant stabilizer, so that the obtained non-reactive polyolefin hot melt adhesive has the characteristics of high softening point and low viscosity, has good flowability, can self-level, meets the filling process, and has higher bonding strength to the release paper and good alkali resistance.
Experiments show that the positioning time of the non-reactive polyolefin hot melt adhesive provided by the invention is within 2min, the final strength can be achieved within 2h, the bonding strength is basically unchanged after alkali liquor treatment, and poor bonding results such as upwarp and peeling are not generated.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a non-reactive polyolefin hot melt adhesive, which comprises the following components:
the present invention is not particularly limited in terms of the source of all raw materials, and may be commercially available.
Wherein the content of the polypropylene homopolymer is preferably 25-35 parts by weight; in some embodiments provided herein, the polypropylene homopolymer is preferably present in an amount of 25 parts by weight; in some embodiments provided herein, the polypropylene homopolymer is preferably present in an amount of 30 parts by weight; in some embodiments provided herein, the polypropylene homopolymer is preferably present in an amount of 35 parts by weight; the softening point of the polypropylene homopolymer is preferably 150-155 ℃, and more preferably 155 ℃; the melt viscosity of the polypropylene homopolymer at 190 ℃ is preferably 1000-4000 mPas, more preferably 1500-3500 mPas, still more preferably 2000-3000 mPas, still more preferably 2200-2500 mPas, and most preferably 2300 mPas.
The content of the amorphous polyolefin resin is preferably 15 to 25 parts by weight, and more preferably 20 to 25 parts by weight; in some embodiments provided herein, the amorphous polyolefin resin is preferably present in an amount of 25 parts by weight; in some embodiments provided herein, the amorphous polyolefin resin is preferably present in an amount of 22 parts by weight; in other embodiments provided herein, the amorphous polyolefin resin is preferably present in an amount of 20 parts by weight; the softening point of the amorphous polyolefin resin is preferably 120 ℃ to 130 ℃; the amorphous polyolefin resin is preferably a homopolymer of ethylene and propylene, more preferably APAO. APAO is an ethylene propylene copolymer with high softening point, low viscosity and low hardness, and the softening point of the ethylene propylene copolymer is preferably 120-130 ℃, and more preferably 125-130 ℃; the ethylene mole percentage content in the APAO is preferably 60-80%, more preferably 70-80%, still more preferably 75-80%, and most preferably 80%; the penetration of the APAO is preferably 80-100 dmm, more preferably 90-100 dmm, and still more preferably 100 dmm.
The content of the tackifying resin is preferably 35-50 parts by weight, and more preferably 35-45 parts by weight; in some embodiments provided herein, the tackifying resin is preferably present in an amount of 40 parts by weight; in some embodiments provided herein, the tackifying resin is preferably present in an amount of 35 parts by weight; in other embodiments provided herein, the tackifying resin is preferably present in an amount of 45 parts by weight; the softening point of the tackifying resin is preferably 120-130 ℃, and more preferably 125-130 ℃; the tackifying resin is preferably a hydrogenated C5 petroleum resin and/or a hydrogenated C9 petroleum resin.
The content of the viscosity modifier is preferably 5-8 parts by weight, and more preferably 5 parts by weight; the softening point of the viscosity regulator is preferably 90-110 ℃; the viscosity modifier is preferably a fischer-tropsch wax and/or a PE wax.
The content of the heat-resistant stabilizer is preferably 0.8-1 part by weight, and more preferably 1 part by weight; the heat stabilizer is preferably (tris [ 2.4-di-tert-butylphenyl ] phosphite) and/or (tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] pentaerythritol ester).
The invention takes the polypropylene homopolymer and the amorphous polyolefin resin as main raw materials, and simultaneously adds the tackifying resin, the viscosity regulator and the heat-resistant stabilizer, so that the obtained non-reactive polyolefin hot melt adhesive has the characteristics of high softening point, low viscosity and good flowability, can self-level, meets the filling process, and has higher bonding strength to the release paper and good alkali resistance.
The invention also provides a preparation method of the non-reactive polyolefin hot melt adhesive, which comprises the following steps: heating and stirring a polypropylene homopolymer, amorphous polyolefin resin, tackifying resin, a viscosity regulator and a heat-resistant stabilizer until the polypropylene homopolymer, the amorphous polyolefin resin, the tackifying resin, the viscosity regulator and the heat-resistant stabilizer are dissolved, vacuumizing and continuously stirring, and cooling to obtain the non-reactive polyolefin hot melt adhesive.
In the invention, preferably, the polypropylene homopolymer, the amorphous polyolefin resin, the tackifying resin, the viscosity regulator and the heat-resistant stabilizer are added and stirred sequentially after being heated; the heating temperature is preferably 170-190 ℃, more preferably 175-185 ℃, and further preferably 180 ℃; the low-viscosity raw materials are added firstly, so that the diluent can play a role in stirring, and the subsequent added raw materials are dissolved.
Stirring until the mixture is dissolved, vacuumizing and continuously stirring; the vacuumizing is preferably carried out until the vacuum degree is more than or equal to 0.09 MPa; the rotation speed of the continuous stirring is preferably 40-45 r/min; the continuous stirring time is preferably 0.5-1.5 h, and more preferably 1 h.
Continuously stirring until no bubbles exist in the appearance, granulating and discharging to obtain a non-reactive polyolefin hot melt adhesive; the shape of the non-reactive polyolefin hot melt adhesive is granular.
The invention also provides the application of the non-reactive polyolefin hot melt adhesive in alkaline batteries, and the application is preferably used for fixing the alkaline battery separator paper.
In order to further illustrate the present invention, the following will describe in detail a non-reactive polyolefin hot melt adhesive, its preparation method and application.
The reagents used in the following examples are all commercially available.
Example 1
Setting the temperature of a stirring kettle to be 180 ℃, adding 30 parts by mass of polypropylene homopolymer (softening point of 155 ℃, and melt viscosity of 2300MPa & s at 190 ℃), 25 parts by mass of polyolefin resin APAO (ethylene-propylene copolymer, ethylene content of 80%, softening point of 125 ℃, needle penetration of 100dmm), 40 parts by mass of hydrogenated C9 petroleum resin (softening point of 125 ℃), 5 parts by mass of Fischer-Tropsch wax (softening point of 90-100 ℃) and 1 part by mass of antioxidant (1010), stirring and dissolving completely, then starting vacuum, wherein the vacuum degree is more than 0.09MPa, the rotating speed is 40-45r/min, stirring for 1h until no obvious bubbles appear, granulating and discharging to obtain the non-reactive polyolefin hot melt adhesive.
Example 2
Setting the temperature of a stirring kettle to be 180 ℃, adding 30 parts by mass of polypropylene homopolymer (softening point of 155 ℃, and melt viscosity of 2300MPa & s at 190 ℃), 22 parts by mass of polyolefin resin APAO (ethylene-propylene copolymer, ethylene content of 80%, softening point of 125 ℃, needle penetration of 100dmm), 40 parts by mass of hydrogenated C5 petroleum resin (softening point of 125 ℃), 8 parts by mass of Fischer-Tropsch wax (softening point of 90-100 ℃) and 1 part by mass of antioxidant (1010), stirring and dissolving completely, then starting vacuum, wherein the vacuum degree is more than 0.09MPa, the rotating speed is 40-45r/min, stirring for 1h until no obvious bubbles appear, granulating and discharging to obtain the non-reactive polyolefin hot melt adhesive.
Example 3
Setting the temperature of a stirring kettle to be 180 ℃, adding 30 parts by mass of polypropylene homopolymer (softening point of 155 ℃, and melt viscosity of 2300MPa & s at 190 ℃), 20 parts by mass of polyolefin resin APAO (ethylene-propylene copolymer, ethylene content of 80%, softening point of 125 ℃, needle penetration of 100dmm), 40 parts by mass of hydrogenated C5 petroleum resin (softening point of 125 ℃), 10 parts by mass of PE wax (softening point of 100-110 ℃) and 1 part by mass of antioxidant (1010), stirring and dissolving completely, then starting vacuum, wherein the vacuum degree is more than 0.09MPa, the rotating speed is 40-45r/min, stirring for 1h until no obvious bubbles appear, granulating and discharging to obtain the non-reactive polyolefin hot melt adhesive.
Example 4
Setting the temperature of a stirring kettle to be 180 ℃, adding 25 parts by mass of polypropylene homopolymer (softening point of 155 ℃, and melt viscosity of 2300MPa & s at 190 ℃), 25 parts by mass of polyolefin resin APAO (ethylene-propylene copolymer, ethylene content of 80%, softening point of 125 ℃, needle penetration of 100dmm), 45 parts by mass of hydrogenated C9 petroleum resin (softening point of 130 ℃), 5 parts by mass of Fischer-Tropsch wax and 1 part by mass of antioxidant (1010), stirring and dissolving completely, starting vacuum, wherein the vacuum degree is more than 0.09MPa, rotating speed is 40-45r/min, stirring for 1h until no obvious bubbles appear, granulating and discharging to obtain the non-reactive polyolefin hot melt adhesive.
Example 5
Setting the temperature of a stirring kettle to be 180 ℃, adding 35 parts by mass of polypropylene homopolymer (softening point of 155 ℃, and melt viscosity of 2300MPa & s at 190 ℃), 25 parts by mass of polyolefin resin APAO (ethylene-propylene copolymer, ethylene content of 80%, softening point of 125 ℃, needle penetration of 100dmm), 35 parts by mass of hydrogenated C5 petroleum resin (softening point of 125 ℃), 5 parts by mass of Fischer-Tropsch wax and 1 part by mass of antioxidant (1010), stirring and dissolving completely, starting vacuum, wherein the vacuum degree is more than 0.09MPa, rotating speed is 40-45r/min, stirring for 1h until no obvious bubbles appear, granulating and discharging to obtain the non-reactive polyolefin hot melt adhesive.
The properties of the non-reactive polyolefin hot melt adhesives obtained in examples 1 to 5 were measured, and the results are shown in Table 1.
TABLE 1 test results of the non-reactive polyolefin Hot melt adhesive Properties
And (4) conclusion: as can be seen from examples 1 to 3, increasing the amount of wax added and decreasing the amount of APAO added reduced the 180 ℃ melt viscosity of the hot melt adhesive, but the adhesion to the substrate decreased, the amount of addition reached 10 parts by mass, and the adhesive tape lifted up and dropped off after being dipped in alkali solution, and was considered to be an unacceptable product. As can be seen from examples 4 to 5, the amount of the polypropylene homopolymer has a large influence on the overall softening point, and the softening point is remarkably lowered when the amount is less than 30 parts by mass, while the viscosity is greatly increased when the amount is more than 30 parts by mass.
Claims (4)
1. A non-reactive polyolefin hot melt adhesive, which is characterized by comprising:
the softening point of the polypropylene homopolymer is 150-155 ℃, and the melt viscosity at 190 ℃ is 1000-4000 mPa & s;
the amorphous polyolefin resin is amorphous polyolefin resin APAO;
the ethylene mole percentage content in the APAO is 60-80%;
the penetration of the APAO is 80-100 dmm;
the softening point of the tackifying resin is 120-130 ℃;
the tackifying resin is selected from hydrogenated C5 petroleum resin and/or hydrogenated C9 petroleum resin;
the viscosity modifier is selected from Fischer-Tropsch wax and/or PE wax;
the heat-resistant stabilizer is selected from (tri [ 2.4-di-tert-butylphenyl ] phosphite) and/or (tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester).
2. The preparation method of the non-reactive polyolefin hot melt adhesive of claim 1, which is characterized by comprising the following steps:
heating and stirring a polypropylene homopolymer, amorphous polyolefin resin, tackifying resin, a viscosity regulator and a heat-resistant stabilizer until the polypropylene homopolymer, the amorphous polyolefin resin, the tackifying resin, the viscosity regulator and the heat-resistant stabilizer are dissolved, vacuumizing and continuously stirring, granulating and discharging after no bubbles exist in appearance, and thus obtaining the non-reactive polyolefin hot melt adhesive.
3. The method of claim 2, wherein the heating temperature is 170 ℃ to 190 ℃; vacuumizing until the vacuum degree is more than or equal to 0.09 MPa; the rotating speed of the continuous stirring is 40-45 r/min.
4. The use of the non-reactive polyolefin hot melt adhesive of claim 1 or the non-reactive polyolefin hot melt adhesive prepared according to any one of claims 2 to 3 in an alkaline battery.
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CN112679819A (en) * | 2020-12-24 | 2021-04-20 | 松川工业材料(无锡)有限公司 | Modified APAO resin and preparation method thereof |
CN114716947B (en) * | 2021-08-03 | 2023-09-05 | 无锡市万力粘合材料股份有限公司 | Polyolefin hot melt adhesive for CPL coating and preparation method thereof |
CN114774029A (en) * | 2022-05-05 | 2022-07-22 | 黄山市信德成胶业有限公司 | Polyolefin APAO hot melt adhesive |
CN115247039B (en) * | 2022-05-13 | 2023-10-31 | 上海路嘉胶粘剂有限公司 | Quick-drying cigarette hot melt adhesive with good weather resistance and preparation process thereof |
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