CN115477905A - Polyolefin hot melt adhesive with quick surface drying and preparation method thereof - Google Patents
Polyolefin hot melt adhesive with quick surface drying and preparation method thereof Download PDFInfo
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- CN115477905A CN115477905A CN202211248743.1A CN202211248743A CN115477905A CN 115477905 A CN115477905 A CN 115477905A CN 202211248743 A CN202211248743 A CN 202211248743A CN 115477905 A CN115477905 A CN 115477905A
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- hot melt
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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
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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
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention provides a polyolefin hot melt adhesive with quick surface drying, which comprises the following raw materials in parts by weight: 30-60 parts of polyolefin; 5-20 parts of a crystallization auxiliary agent; 20-50 parts of tackifying resin; 1-15 parts of a viscosity regulator; 0.1-1 part of antioxidant. The invention also provides a preparation method of the polyolefin hot melt adhesive with quick surface drying. A crystallization auxiliary agent is added into the raw material of the polyolefin hot melt adhesive to accelerate the surface drying speed; meanwhile, a large amount of low-viscosity wax is avoided, and the mechanical strength and flexibility of the hot melt adhesive are prevented from being influenced.
Description
Technical Field
The invention relates to the technical field of glue, in particular to a polyolefin hot melt adhesive with quick surface drying and a preparation method thereof.
Background
A hot melt adhesive is a 100% solids thermoplastic polymer that does not require a solvent. The hot melt adhesive melts and rapidly solidifies during cooling, resulting in excellent mechanical strength. Compared with other adhesives, the hot melt adhesive has the advantages of no solvent, convenient synthesis, short curing time, wide bonding range, convenient storage and transportation and no environmental pollution, conforms to the leading direction of green chemistry, and belongs to an environment-friendly chemical product. The product is solid, so the product is convenient to package, transport and store, and has no solvent, pollution and toxicity; and the advantages of simple production process, high added value, high bonding strength, high speed and the like. With the development of the petrochemical industry, various thermoplastic materials such as ethylene-vinyl acetate copolymer (EVA), polyamide (PA), polyolefin, etc. are used as base materials for hot melt adhesives, and have been widely used in the fields of wood, footwear, clothing, automobiles, packaging, etc.
The fast operation is a great characteristic of the hot melt adhesive. The operation time of the hot melt adhesive is about 15 seconds generally, and along with the wide application of modern production lines, the requirement on the operation time of the hot melt adhesive is shorter and shorter, and the requirement on the operation time of the hot melt adhesive reaches about 5 seconds if packaging and pipe pasting, book binding and loudspeaker box manufacturing are carried out. It is desirable that hot melt adhesives wet the substrate quickly and sufficiently, while having a fast cure rate and providing a certain bond strength. In general, the use of low viscosity waxes, such as Fischer-Tropsch waxes, polyolefin waxes, paraffin waxes, microcrystalline waxes, and the like, in hot melt adhesive formulations can significantly increase the rate of cure, but can have some effect on the adhesive properties of the hot melt adhesive material and can result in poor flexibility.
Disclosure of Invention
In order to achieve the above object, the present invention is achieved by the following technical solutions.
The invention provides a polyolefin hot melt adhesive with quick surface drying, which comprises the following raw materials in parts by weight:
preferably, the polyolefin is selected from at least one of polyethylene, polypropylene, polybutylene, ethylene-vinyl acetate copolymer, ethylene-acrylic acid copolymer, amorphous polyalphaolefin.
Preferably, the crystallization aid comprises the following raw materials in parts by weight:
4.9-18 parts of high-crystallinity polyolefin;
0.1-2 parts of nucleating agent.
Preferably, the highly crystalline polyolefin is selected from at least one of linear low density polyethylene, high density polyethylene, isotactic polypropylene, and isotactic polybutylene.
Preferably, the nucleating agent is selected from at least one of sorbitol derivatives, organic carboxylic acids, metal salts of organic carboxylic acids, organic phosphates, talc, calcium carbonate, mica.
Preferably, the tackifying resin is selected from at least one of rosin, rosin derivatives, terpene resins, petroleum resins, thermoplastic phenolic resins, low molecular weight polystyrene.
Preferably, the viscosity modifier is selected from at least one of naphthenic mineral oil, hydrogenated polybutadiene, paraffin wax, microcrystalline wax, fischer-Tropsch wax, polyethylene wax, oxidized polyethylene wax, polypropylene wax, and saso wax.
Preferably, the antioxidant is at least one selected from antioxidant B215, antioxidant 1010, antioxidant 168, antioxidant 1076 and antioxidant 3114.
It is a second object of the present invention to provide a process for preparing the fast tack-free polyolefin hot melt adhesive as described above, comprising the steps of:
s1, heating the inside of a reaction container to a temperature of over 100 ℃;
s2, adding polyolefin, a crystallization auxiliary agent, tackifying resin, a viscosity regulator and an antioxidant into the reaction container according to the measurement, vacuumizing, stirring and reacting to obtain the polyolefin hot melt adhesive.
Preferably, the reaction temperature is from 180 ℃ to 220 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a polyolefin hot melt adhesive with quick surface drying, wherein a crystallization auxiliary agent is added into the raw material of the polyolefin hot melt adhesive to accelerate the surface drying speed; meanwhile, a large amount of low-viscosity wax is avoided, and the high-viscosity polyurethane elastomer has high mechanical strength and flexibility.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood and to be implemented according to the content of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings. The detailed description of the present invention is given in detail by the following examples and the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention and do not constitute a limitation of the invention. In the drawings:
FIG. 1 is a flow chart of the steps of the preparation method of the present invention.
Detailed Description
The foregoing and other objects, features, aspects and advantages of the present invention will become more apparent from the following detailed description of the present invention when taken in conjunction with the accompanying drawings, which will enable those skilled in the art to practice the present invention with reference to the accompanying specification. In the drawings, the shape and size may be exaggerated for clarity, and the same reference numerals will be used throughout the drawings to designate the same or similar components. In the following description, terms such as center, thickness, height, length, front, back, rear, left, right, top, bottom, upper, lower, and the like are used based on the orientation or positional relationship shown in the drawings. In particular, "height" corresponds to the dimension from top to bottom, "width" corresponds to the dimension from left to right, and "depth" corresponds to the dimension from front to back. These relative terms are for convenience of description and generally are not intended to require a particular orientation. Terms concerning attachments, coupling and the like (e.g., "connected" and "attached") refer to a relationship wherein structures are secured or attached, either directly or indirectly, to one another through intervening structures, as well as both movable or rigid attachments or relationships, unless expressly described otherwise.
The present invention will be further described with reference to the accompanying drawings and the detailed description, and it should be noted that any combination of the embodiments or technical features described below can be used to form a new embodiment without conflict.
The invention provides a polyolefin hot melt adhesive with quick surface drying, which comprises the following raw materials in parts by weight:
in the embodiment, a crystallization auxiliary agent is added into the raw material of the polyolefin hot melt adhesive to accelerate the surface drying speed; meanwhile, the scheme that the curing rate is accelerated by adding low-viscosity wax in the traditional hot melt adhesive formula is replaced, so that a large amount of low-viscosity wax is avoided, and the mechanical strength and flexibility of the hot melt adhesive are prevented from being influenced. Namely, the technical scheme of adding the crystallization auxiliary agent is adopted, so that the surface drying speed of the hot melt adhesive can be accelerated, and meanwhile, the hot melt adhesive can have higher mechanical strength and flexibility.
In one embodiment, the polyolefin is selected from at least one of Polyethylene (PE), polypropylene (PP), polybutylene (PB), ethylene Vinyl Acetate (EVA), ethylene Acrylic Acid (EAA), amorphous Polyalphaolefin (APAO). Specifically, polyolefins are used as matrix resins to provide the necessary adhesive strength and cohesion for polyolefin hot melt adhesive systems.
In one embodiment, the crystallization aid comprises the following raw materials in parts by weight:
4.9-18 parts of high-crystallinity polyolefin;
0.1-2 parts of nucleating agent.
Further, the highly crystalline polyolefin is at least one selected from the group consisting of Linear Low Density Polyethylene (LLDPE), high Density Polyethylene (HDPE), isotactic polypropylene (iPP), and Isotactic Polybutylene (iPB). Specifically, the high-crystallinity polyolefin has higher molecular chain regularity, compact arrangement, higher crystallinity, stronger crystallization ability after melting and cooling, higher crystallization rate and shorter surface drying time. The highly crystalline polyolefin is preferably isotactic polypropylene (iPP) 。
Further, the nucleating agent is selected from at least one of sorbitol derivatives, organic carboxylic acids, organic carboxylic acid metal salts, organic phosphates, talc, calcium carbonate and mica. Specifically, the addition of the nucleating agent can significantly improve the crystallization peak temperature of the high-crystallinity polyolefin, accelerate the crystallization rate, shorten the crystallization time and further shorten the surface drying time. The nucleating agent is preferably a sorbitol derivative.
Further, the highly crystalline polyolefin is preferably 8 to 12 parts, and the nucleating agent is preferably 0.2 to 0.8 part.
In one embodiment, the tackifying resin is selected from at least one of rosin, rosin derivatives, terpene resins, petroleum resins, phenolic thermoplastic resins, low molecular weight polystyrene. Specifically, the tackifier resin can have good compatibility with the above polyolefin base resin, and can improve wetting property and initial tack property. Further, the terpene resin includes a modified terpene resin. Further, the petroleum resin includes hydrogenated petroleum resin.
In one embodiment, the viscosity modifier is selected from at least one of a naphthenic mineral oil, a hydrogenated polybutadiene, a paraffin wax, a microcrystalline wax, a fischer-tropsch wax, a polyethylene wax, an oxidized polyethylene wax, a polypropylene wax, and a saso wax. Specifically, the viscosity regulator is used for reducing the viscosity of the prepared polyolefin hot melt adhesive and reducing the softening point, thereby improving the low temperature resistance of the polyolefin hot melt adhesive.
In one embodiment, the antioxidant is selected from at least one of antioxidant B215, antioxidant 1010, antioxidant 168, antioxidant 1076, and antioxidant 3114. Specifically, the antioxidant is used for improving the thermal stability of the polyolefin hot melt adhesive, preventing the physical properties of the polyolefin hot melt adhesive from aging, and reducing the color change of the polyolefin hot melt adhesive.
The invention also provides a preparation method of the rapid surface-drying polyolefin hot melt adhesive, which comprises the following steps as shown in figure 1:
s1, heating the inside of a reaction container to a temperature of over 100 ℃;
s2, adding polyolefin, a crystallization assistant, tackifying resin, a viscosity regulator and an antioxidant into a reaction container according to a certain amount, vacuumizing, stirring and reacting to obtain the polyolefin hot melt adhesive.
The preparation method is simple and has mild process conditions.
Further, the reaction temperature is greater than 130 ℃. Preferably, the reaction temperature is from 180 ℃ to 220 ℃. The reaction temperature may be heated in place in step S1 or in place in step S2.
Further, step S2 further comprises the steps of: and obtaining clear liquid after the reaction is finished, and filtering to obtain the polyolefin hot melt adhesive.
The method of the present invention is illustrated below by means of specific examples, which are to be understood as being illustrative of the basic principles, main features and advantages of the present invention, and the present invention is not limited in scope by the following examples; the implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not noted are generally those in routine experiments.
In the following examples and comparative examples, the polyolefin is available from Dow under the trade designation Affinity GA 1900. Tackifying resins are available under the trademark Wingtack 98 from Cray Valley; the viscosity modifier was sold under the brand name A-C1660, available from Honeywell corporation. Antioxidant designations 1010 and 168 available from Tianjin Lianlong; the weight ratio of antioxidant 1010 to antioxidant 168 was 1.
Example 1
The preparation of the rapid surface-drying polyolefin hot melt adhesive comprises the following steps:
(1) Heating the mixture in a reaction kettle to 120 ℃;
(2) Adding 50 parts by weight of polyolefin, 4.9 parts by weight of high-crystallinity polyolefin, 0.1 part by weight of nucleating agent, 40 parts by weight of tackifying resin, 10 parts by weight of viscosity modifier and 0.5 part by weight of antioxidant into a reaction kettle, vacuumizing to-0.9 MPa, stirring, reacting at the temperature of 180 ℃ for 4 hours to completely react to form clear liquid, and filtering to obtain the polyolefin hot melt adhesive;
wherein, the first and the second end of the pipe are connected with each other,
the high crystalline polyolefin is linear low density polyethylene with the trade name of M500026 and is purchased from Sabic;
the nucleating agent is Talc powder, and is available from Nippon Talc company under the designation SG-2000.
Example 2
The preparation of the rapid surface-drying polyolefin hot melt adhesive comprises the following steps:
(1) Heating the mixture in a reaction kettle to 130 ℃;
(2) Adding 40 parts by weight of polyolefin, 15 parts by weight of high-crystallinity polyolefin, 1 part by weight of nucleating agent, 40 parts by weight of tackifying resin, 10 parts by weight of viscosity modifier and 0.5 part by weight of antioxidant into a reaction kettle, vacuumizing to-0.9 MPa, stirring, reacting at 190 ℃ for 4 hours to completely react to form clear liquid, and filtering to obtain the polyolefin hot melt adhesive;
wherein the highly crystalline polyolefin is high density polyethylene sold under the trademark Alathon H4250 available from Lyondell Basell company;
the nucleating agent is organic phosphate and is available from Adeka company, and the mark of the nucleating agent is NA-21.
Example 3
The preparation of the rapid surface-drying polyolefin hot melt adhesive comprises the following steps:
(1) Heating the mixture in a reaction kettle to 140 ℃;
(2) Adding 45 parts by weight of polyolefin, 10 parts by weight of high-crystallinity polyolefin, 0.5 part by weight of nucleating agent, 40 parts by weight of tackifying resin, 10 parts by weight of viscosity modifier and 0.5 part by weight of antioxidant into a reaction kettle, vacuumizing to-0.9 MPa, stirring, reacting at 200 ℃ for 4 hours to completely react to form clear liquid, and filtering to obtain the polyolefin hot melt adhesive;
wherein the high-crystallinity polyolefin is isotactic polypropylene with the trade name of PP7945E1 and is purchased from Exxon Mobil company;
the nucleating agent is sorbitol derivative, and the mark is Millad 3940, and is purchased from Milliken company.
Example 4
The preparation of the rapid surface-drying polyolefin hot melt adhesive comprises the following steps:
(1) Heating the mixture in a reaction kettle to 150 ℃;
(2) Adding 35 parts by weight of polyolefin, 18 parts by weight of high-crystallinity polyolefin, 2 parts by weight of nucleating agent, 40 parts by weight of tackifying resin, 10 parts by weight of viscosity modifier and 0.5 part by weight of antioxidant into a reaction kettle, vacuumizing to-0.9 MPa, stirring, reacting at the temperature of 210 ℃ for 4 hours to completely react to form clear liquid, and filtering to obtain the polyolefin hot melt adhesive;
wherein the high crystalline polyolefin is isotactic polybutene and has a trademark of Koattro PB M1500M, available from Lyondell Basell company;
the nucleating agent is organic carboxylate with the mark of SG-2000, and is purchased from Nippon Talc company.
Comparative example 1
The preparation method of the hot melt adhesive comprises the following steps:
(1) Heating the mixture in a reaction kettle to 120 ℃;
(2) Adding 45 parts by weight of polyolefin, 10 parts by weight of polyethylene wax (Epolene N-14, available from Westlake, inc.), 40 parts by weight of tackifying resin, 10 parts by weight of viscosity modifier and 0.5 part by weight of antioxidant into a reaction kettle, vacuumizing to-0.9 MPa, stirring, reacting at 180 ℃ for 4 hours to completely form clear liquid, and filtering to obtain the hot melt adhesive.
Comparative example 2
The preparation method of the hot melt adhesive comprises the following steps:
(1) Heating the mixture in a reaction kettle to 120 ℃;
(2) Adding 50 parts by weight of polyolefin, 40 parts by weight of tackifying resin, 10 parts by weight of viscosity modifier and 0.5 part by weight of antioxidant into a reaction kettle, vacuumizing to-0.9 MPa, stirring, reacting at the temperature of 180 ℃ for 4 hours to completely react to form clear liquid, and filtering to obtain the hot melt adhesive.
The hot melt adhesives obtained in examples 1 to 4 and comparative examples 1 and 2 were subjected to a performance test.
Wherein the softening point test method is according to GB/T15332.
Melt viscosity was measured according to HG/T3660-1999.
180 DEG peel strength was tested according to GB/T2790.
The surface dry time test method comprises the following steps: 8g of hot melt adhesive is placed in an aluminum foil cup, melted at 165 ℃ for 30 minutes, taken out after complete melting is confirmed, and the surface is touched with the tip of a toothpick at 23 ℃ without wire drawing and is regarded as surface dry.
The light transmittance test method is GB/T1038-2000.
The tensile strength and elongation at break test methods are in accordance with GB/T528-2009.
The test results are shown in table one.
Watch 1
As can be seen from Table I, in examples 1 to 4, the highly crystalline polyolefin and the nucleating agent were added, in comparative example 1, the polyethylene wax was used to adjust the tack free time of the hot melt adhesive, and in comparative example 2, the crystallization aid and the polyethylene wax were not used. The results show that examples 1 to 4 can achieve the same level of tack-free time as comparative example 1 while the tensile strength and light transmittance are significantly improved relative to comparative example 1. The results show that the addition of the crystallization auxiliary agent in the polyolefin hot melt adhesive raw material can enhance the tensile strength and improve the light transmittance.
In the crystallization processes of examples 1 to 4, the spherulite size is reduced, and the number of crystal nuclei and microcrystals is increased, so that the crystallinity is improved, and the tensile strength of the hot melt adhesive is improved. The surface drying time, the tensile strength and the light transmittance of the embodiment 3 are obviously superior to those of the embodiments 1 to 3, and the sorbitol derivative has a similar crystal structure with isotactic polypropylene, so that the system has good compatibility, is easy to disperse and has more efficient action.
Further, the contents of the highly crystalline polyolefin and the nucleating agent should be in appropriate ranges, that is, the content of the crystallization aid should be in appropriate ranges. Too much crystallization aid content can reduce the high-temperature wettability of the glue, thereby reducing the peeling strength; the content of the crystallization aid is too low, so that the crystallization rate of the whole material is not easy to accelerate, and the surface drying time is not favorably shortened.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; one of ordinary skill in the art can readily practice the present invention as illustrated and described herein with reference to the accompanying drawings; however, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the scope of the invention as defined by the appended claims; meanwhile, any equivalent changes, modifications and evolutions made to the above embodiments according to the substantial technology of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. The polyolefin hot melt adhesive capable of being quickly dried on the surface is characterized by comprising the following raw materials in parts by weight:
2. the fast open polyolefin hot melt adhesive of claim 1 wherein said polyolefin is selected from at least one of polyethylene, polypropylene, polybutylene, ethylene-vinyl acetate copolymer, ethylene-acrylic acid copolymer, amorphous polyalphaolefin.
3. The rapid surface-drying polyolefin hot melt adhesive according to claim 1, wherein the crystallization aid comprises the following raw materials in parts by weight:
4.9-18 parts of high-crystallinity polyolefin;
0.1-2 parts of nucleating agent.
4. The fast open-dry polyolefin hot melt adhesive according to claim 3, wherein said high crystalline polyolefin is selected from at least one of linear low density polyethylene, high density polyethylene, isotactic polypropylene, isotactic polybutylene.
5. The fast-tack polyolefin hot melt adhesive of claim 3, wherein the nucleating agent is selected from at least one of sorbitol derivatives, organic carboxylic acids, metal salts of organic carboxylic acids, organic phosphates, talc, calcium carbonate, mica.
6. The fast open-dry polyolefin hot melt adhesive of claim 1, wherein said tackifying resin is selected from at least one of rosin, rosin derivatives, terpene resins, petroleum resins, phenolic resins, low molecular weight polystyrene.
7. The fast open-top polyolefin hot melt adhesive of claim 1, wherein said viscosity modifier is selected from at least one of the group consisting of naphthenic mineral oil, hydrogenated polybutadiene, paraffin wax, microcrystalline wax, fischer-tropsch wax, polyethylene wax, oxidized polyethylene wax, polypropylene wax, and saso wax.
8. The fast tack-free polyolefin hot melt adhesive of claim 1, wherein the antioxidant is at least one selected from the group consisting of antioxidant B215, antioxidant 1010, antioxidant 168, antioxidant 1076, and antioxidant 3114.
9. The method for preparing the quick surface-drying polyolefin hot melt adhesive according to claim 1, which is characterized by comprising the following steps:
s1, heating the inside of a reaction container to a temperature of over 100 ℃;
s2, adding polyolefin, a crystallization auxiliary agent, tackifying resin, a viscosity regulator and an antioxidant into the reaction container according to the measurement, vacuumizing, stirring and reacting to obtain the polyolefin hot melt adhesive.
10. The process of claim 9, wherein the reaction temperature is from 180 ℃ to 220 ℃.
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2022
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| US20120318354A1 (en) * | 2010-12-29 | 2012-12-20 | E. I. Du Pont De Nemours And Company | Photovoltaic module with chlorosulfonated polyolefin layer |
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