CN115044336A - Quick-drying adhesive - Google Patents
Quick-drying adhesive Download PDFInfo
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- CN115044336A CN115044336A CN202210739542.5A CN202210739542A CN115044336A CN 115044336 A CN115044336 A CN 115044336A CN 202210739542 A CN202210739542 A CN 202210739542A CN 115044336 A CN115044336 A CN 115044336A
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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
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4202—Two or more polyesters of different physical or chemical nature
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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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
- C09J11/04—Non-macromolecular additives inorganic
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a quick-drying adhesive, which comprises a silicon modified polyether adhesive, wherein the silicon modified polyether adhesive is prepared from the following raw materials in percentage by weight: 8-10% of novel alkyl phenolic tackifying resin, 32-35% of high chlorinated polyethylene, 20-23% of macromolecular thermoplastic polyester resin, 0.05-0.1% of water removing agent and antioxidant: 0-0.2% and white carbon black: 1.5-2% and the balance of MS prepolymer; the novel alkyl phenolic tackifying resin is silane coupling agent modified alkyl phenolic resin; the molecular weight of the macromolecular thermoplastic polyester resin is 8-10 ten thousand. The adhesive has the advantages of short surface drying time, high curing speed, good flexibility and good construction performance.
Description
Technical Field
The application relates to the field of adhesives, in particular to a quick-drying adhesive.
Background
At present, the commonly used adhesives in the industries of building adhesives, structural adhesives, sealant and the like comprise silicone adhesive, polyurethane adhesive, silicon modified polyether adhesive and the like, and the adhesives are single-component or double-component adhesives, and the comprehensive performance of the adhesives is optimal with the silicon modified polyether adhesive. The silicon modified polyether adhesive comprises the following main raw materials: the adhesive has the advantages of extremely low surface energy, high permeability, good weather resistance and durability, environmental protection, and can be used for adhering almost all decorative base materials.
However, the existing silicon modified polyether adhesive has the problems of long surface drying time and low curing speed, and the initial adhesion is poor.
Disclosure of Invention
In order to solve the problem that the initial adhesion is poor due to the slow curing speed of the silicon modified polyether adhesive in the related art, the application provides a quick-drying adhesive.
The quick-drying adhesive provided by the application adopts the following technical scheme:
a quick-drying adhesive comprises a silicon modified polyether adhesive, wherein the silicon modified polyether adhesive is prepared from the following raw materials in percentage by weight:
novel alkyl phenolic tackifying resins: 8 to 10 percent of
Highly chlorinated polyethylene: 32 to 35 percent
Macromolecular thermoplastic polyester resin: 20 to 23 percent of
Water removal agent: 0.05 to 0.1 percent
Antioxidant: 0 to 0.2 percent
White carbon black: 1.5 to 2 percent
MS prepolymer: balance of
The novel alkyl phenolic tackifying resin is silane coupling agent modified alkyl phenolic resin;
the molecular weight of the macromolecular thermoplastic polyester resin is 8-10 ten thousand.
By adopting the technical scheme, the novel alkyl phenolic tackifying resin and the macromolecular thermoplastic polyester resin with the molecular weight of 8-10 ten thousand are added on the basis of the MS prepolymer, so that on one hand, the surface drying time and the curing speed of the silicon modified polyether adhesive can be accelerated, no air bubbles are generated, and the initial adhesive property of the silicon modified polyether adhesive is favorably improved; on the other hand, the surface drying time of the silicon modified polyether adhesive is within 20-30min, and the silicon modified polyether adhesive has the advantage of good construction performance. Secondly, the high chlorinated polyethylene can enhance the wettability and the adhesive force of the adhesive to the base material with wax feeling on the surface or the PET base material with smooth surface, and can improve the bonding fastness of the adhesive to the base material. The adhesive has good quick-drying property and strong initial adhesion, and is particularly suitable for being used as building adhesive.
Optionally, the novel alkyl phenolic tackifying resin comprises raw materials of alkyl phenolic resin, ethyl acetate, absolute ethyl alcohol and a silane coupling agent; wherein the mass of the alkyl phenolic resin is 28-32% of that of ethyl acetate, the mass of the absolute ethyl alcohol is 8-12% of that of the alkyl phenolic resin, and the mass of the silane coupling agent is 4-6% of that of the alkyl phenolic resin.
By adopting the technical scheme, the novel alkyl phenolic tackifying resin prepared from the raw materials according to the proportion has good compatibility with the MS prepolymer, and the probability of layering after long-term storage is low.
Optionally, the preparation method of the novel alkyl phenolic tackifying resin comprises the following steps:
adding alkyl phenolic resin into ethyl acetate, stirring for dissolving, adding absolute ethyl alcohol and a silane coupling agent, stirring for reacting for 7.5-8.5h, then heating to 75-85 ℃, vacuumizing for recovering ethyl acetate and absolute ethyl alcohol, heating to 100 ℃, and vacuumizing for removing moisture to obtain the novel alkyl phenolic tackifying resin.
By adopting the technical scheme, when the novel alkyl phenolic tackifying resin is prepared according to the method, the novel alkyl phenolic tackifying resin and the MS prepolymer are kept stable and do not mutually cause reaction when being mixed, the compatibility of the novel alkyl phenolic tackifying resin and the MS prepolymer is further improved, and the silicon modified polyether adhesive can not be layered after being placed for a long time.
Optionally, the macromolecular thermoplastic polyester resin comprises the following raw materials in parts by weight:
diisocyanate
Polyester polyols
Low molecular weight diols
Wherein the molar ratio of isocyanic acid radical in the diisocyanate to the total amount of hydroxyl in the polyester polyol and the low molecular diol is 0.90-0.95;
the polyester polyol comprises 4000 molecular weight polyester polyol and 6000 molecular weight polyester polyol, and the weight ratio of the 4000 molecular weight polyester polyol to the 6000 molecular weight polyester polyol is (6-7): (3-4).
Preferably, the diisocyanate is 4' 4-diphenylmethane diisocyanate.
By adopting the technical scheme, when the polyester polyol is the 4000-molecular-weight polyester polyol, the flexibility of the silicon modified polyether adhesive is insufficient, the brittleness is enhanced, and the resistance to temperature and humidity deformation is poor; and when the polyester polyol is 6000 molecular weight polyester polyol, the silicon modified polyether adhesive is too soft, and the tearing strength is low. In this application, polyester polyol adopts the composition of 4000 molecular weight polyester polyol and 6000 molecular weight polyester polyol two kinds, is favorable to obtaining the better silicon modified polyether adhesive of pliability also better simultaneously of initial viscous property, and when this silicon modified polyether adhesive is applied to the ceramic tile bonding, is favorable to reducing the safety risk.
Preferably, the low molecular diol is 2-butyl-2-ethyl-1, 3-propanediol.
The 2-butyl-2-ethyl-1, 3-propylene glycol is branched low molecular glycol, and compared with other low molecular glycols, when the 2-butyl-2-ethyl-1, 3-propylene glycol is adopted, the silicon modified polyether adhesive has stronger adhesive force to a base material with wax feeling on the surface or a PET base material with smooth surface, and the hydrolysis resistance and the weather resistance of the silicon modified polyether adhesive are better.
Optionally, the preparation method of the macromolecular thermoplastic polyester resin comprises the following steps:
melting polyester polyol at the temperature of 105-115 ℃, vacuumizing to remove moisture, then cooling to 65-75 ℃, adding a first part of diisocyanate, stirring to react for 1.4-1.6h, then adding low-molecular diol, continuing to stir to react for 1.8-2.2h, then supplementing a second part of diisocyanate, continuing to react for 0.8-1.2h, then slowly heating to the temperature of 105-115 ℃, and continuing to react for 2-3h to obtain macromolecular thermoplastic polyester resin with the molecular weight of 8-10 ten thousand;
wherein the weight ratio of the first part of diisocyanate to the second part of diisocyanate is 11 (10-12).
By adopting the technical scheme, the diisocyanate is added in two steps, so that the reaction time is favorably shortened, and the side reaction can be reduced.
Optionally, adding a second portion of diisocyanate, continuing to react for 0.8-1.2h, and then increasing the temperature to 105-115 ℃ at a temperature increase rate of 1-1.2 ℃/min.
By adopting the technical scheme, the excessively fast heating rate influences the flexibility and the surface drying time of the silicon modified polyether adhesive, and the reason is that the excessively fast heating rate can influence the molecular weight distribution of the macromolecular thermoplastic polyester resin, even molecular self-cohesion byproducts can occur, and the acquisition of a linear chain structure with consistent molecular weight is not facilitated, so that the flexibility and the surface drying time of the silicon modified polyether adhesive can be influenced.
Optionally, the preparation method of the silicon-modified polyether adhesive comprises the following steps:
s1, heating the macromolecular thermoplastic polyester resin to 125-135 ℃;
s2, heating the novel alkyl phenolic tackifying resin to 125-135 ℃, adding high chlorinated polyethylene and macromolecular thermoplastic resin with the temperature range of 125-135 ℃, and uniformly stirring to obtain a premix;
s3, adding a water removing agent, an antioxidant and white carbon black into the MS prepolymer, heating to 115-125 ℃, stirring for reaction for 2-3h, transferring to the premix, then filling nitrogen to replace air in the reactor, cooling to about 60 ℃, filtering, extruding and packaging to obtain the quick-drying silicon modified polyether adhesive.
By adopting the technical scheme, the novel alkyl phenolic tackifying resin and the macromolecular thermoplastic polyester resin are heated to 125-phase 135 ℃ and then mixed with the high chlorinated polyethylene, so that the improvement of the dispersion performance of each component of the silicon modified polyether adhesive is facilitated, and the uniform quick-drying silicon modified polyether adhesive is obtained; in addition, a water removing agent capable of reacting with water is added into the silicon modified polyether adhesive, so that the storage time of the silicon modified polyether adhesive is prolonged; the antioxidant is added into the silicon modified polyether adhesive, so that the heat resistance and the weather resistance of the silicon modified polyether adhesive are improved; the white carbon black is added into the silicon modified polyether adhesive, so that the mechanical property and the wear resistance of the silicon modified polyether adhesive are improved.
Preferably, the water removal agent is triethyl orthoformate.
By adopting the technical scheme, the triethyl orthoformate has very high reaction activity with water and high water removal efficiency.
Optionally, the quick-drying adhesive further comprises a drier, and the drier is prepared from the following raw materials in percentage by weight:
metal organic compound: 1 percent of
Amine compounds: 1 to 3 percent of
Dichloromethane: 35 to 40 percent of
Solvent: and (4) the balance.
By adopting the technical scheme, the volatilization rate of the dichloromethane is high, and in the spraying process, the surrounding air can be cooled, water vapor is condensed, the surface humidity of the base material is obviously increased, and the OH reacted with NCO is favorably provided; in addition, the compounding of the metal organic compound and the amine compound can strengthen the catalytic action on the reaction of NCO and OH, and is favorable for accelerating the curing speed of the silicon modified polyether adhesive in the environment with the temperature lower than 10 ℃ and the humidity lower than 40 percent, thereby improving the service performance of the silicon modified polyether adhesive in a low-temperature drying environment.
The drier is in a spray form, when the drier is matched with the silicon modified polyether adhesive for use, before glue application, a layer of drier is uniformly sprayed on a substrate, then glue application is performed on one substrate, after glue application is completed, another substrate is attached, the substrate is fixed in 10-15s after pressure is applied, and finally the substrate is placed still and cured.
Optionally, the metal organic compound comprises a bismuth organic compound and a zinc organic compound, wherein the bismuth organic compound is any one or a combination of bismuth isooctanoate and bismuth neodecanoate; the zinc organic compound is selected from one or a combination of more of zinc neodecanoate and zinc isooctanoate; the amine compound is one or a combination of more of dimorpholinylethyl ether, ethanolamine and triethylamine.
Preferably, the bismuth-containing organic compound is bismuth isooctanoate, the zinc-containing organic compound is zinc neodecanoate, and the weight ratio of the bismuth isooctanoate to the zinc neodecanoate is (2-3): and (3-2), the amine compound is dimorpholinylethyl ether.
By adopting the technical scheme, the bismuth isooctanoate, the zinc neodecanoate and the dimorpholinylethyl ether have strong catalytic action on the reaction of NCO and OH according to the proportion in the application, and the surface drying time of the silicon modified polyether adhesive in a low-temperature drying environment can be controlled within 20-30min, so that the drying speed of the silicon modified polyether adhesive is accelerated, and meanwhile, the silicon modified polyether adhesive is ensured to have enough open time in the low-temperature drying environment.
Optionally, the solvent includes any one or more of ethyl acetate, methyl acetate and acetone.
In summary, the quick-drying adhesive has at least the following beneficial effects:
1. on the one hand, the surface drying time and the curing speed of the silicon modified polyether adhesive can be accelerated, no air bubbles are generated, and the initial adhesive property of the silicon modified polyether adhesive is favorably improved; on the other hand, the surface drying time of the silicon modified polyether adhesive is within 20-30min, and the workability is good;
2. when the low molecular diol is 2-butyl-2-ethyl-1, 3-propylene glycol, the silicon modified polyether adhesive has stronger adhesive force to a base material with wax feeling on the surface or a PET base material with smooth surface, and has better hydrolysis resistance and weather resistance;
3. when the drier is prepared for use, the silicon modified polyether adhesive can be used under a low-temperature drying condition.
Detailed Description
The present application will be described in further detail below with reference to preparation examples, examples and comparative examples.
Preparation of novel alkyl phenol-formaldehyde tackifying resin
The amounts of the components of the novel alkyl phenol-formaldehyde tackifying resin used in preparation examples 1-2 are respectively given in Table 1 below.
TABLE 1 amounts of components of the novel alkyl phenol-formaldehyde tackifying resins of preparation examples 1-2
| Raw materials | Preparation example 1 | Preparation example 2 |
| Ethyl acetate/kg | 100 | 100 |
| Silane coupling agent KH560/kg | 1.12 | 1.92 |
| Alkylphenol formaldehyde resin/kg | 28 | 32 |
| Absolute ethyl alcohol/kg | 2.24 | 3.84 |
The preparation of the novel alkylphenol tackifying resins of preparation examples 1-2 was as follows:
adding alkylphenol-formaldehyde resin into ethyl acetate, stirring for dissolving, adding absolute ethyl alcohol and a silane coupling agent, stirring for reacting for 8 hours, then heating to 80 ℃, vacuumizing for recycling ethyl acetate and absolute ethyl alcohol, heating to 100 ℃, vacuumizing for removing moisture, and obtaining the novel alkylphenol-formaldehyde tackifying resin.
Preparation of macromolecular thermoplastic polyester resin
The amounts of the respective components of the macromolecular thermoplastic polyester resin used in preparation examples 1 to 6 are shown in Table 2 below.
TABLE 2 amounts of components of macromolecular thermoplastic polyester resins in preparation examples 1 to 6
In this preparation example, the hydroxyl value of the 4000 molecular weight polyester polyol was 28KOHmg/g, and the hydroxyl value of the 6000 molecular weight polyester polyol was 18.5 KOHmg/g. In addition, the molar ratio of isocyanate group to hydroxyl group in preparation examples 1 and 3 to 6 was 0.95, and the molar ratio of isocyanate group to hydroxyl group in preparation example 2 was 0.90.
The preparation method of the macromolecular thermoplastic polyester resin in preparation examples 1 to 6 comprises the following steps:
melting polyester polyol at 110 ℃, vacuumizing to remove moisture, then cooling to 70 ℃, adding a first part of 4 '4-diphenylmethane diisocyanate according to the proportion in table 2, stirring to react for 1.5h, then adding 2-butyl-2-ethyl-1, 3-propanediol or propanediol, continuing to stir to react for 2h, then additionally adding a second part of 4' 4-diphenylmethane diisocyanate, continuing to react for 1h, then heating to 110 ℃ at a slow heating rate, and continuing to react for 2.5h to obtain the macromolecular thermoplastic polyester resin. Wherein the temperature rise rate after the addition of the second portion of 4', 4-diphenylmethane diisocyanate in preparation examples 1-2 and 5-6 was limited to 1 ℃/min, the temperature rise rate in preparation example 3 was limited to 1.2 ℃/min, and the temperature rise rate in preparation example 4 was limited to 4 ℃/min.
Example of preparation of siccative
The amounts of the respective components of the siccative used in preparation examples 1 to 4 are shown in Table 3 below.
TABLE 3 weight percentages of the components of the siccative in preparations 1-4
| Raw materials | Drier 1 | Drier 2 | Drier 3 | Catalyst 4 |
| Bismuth Isooctanoate | 0.4％ | 0.4％ | 0.6％ | 1％ |
| Zinc neodecanoate | 0.6％ | 0.6％ | 0.4％ | 0 |
| Dimorpholinylethyl ether | 1％ | 1％ | 3％ | 1％ |
| Methylene dichloride | 0 | 35％ | 40％ | 35％ |
| Ethyl acetate | 98％ | 63％ | 56％ | 63％ |
The preparation of the siccative of preparation examples 1 to 4 was as follows:
in a blending kettle, adding ethyl acetate and dichloromethane according to the formula in the table 3, adding bismuth isooctanoate, zinc neodecanoate and dimorpholinyl ethyl ether under low-speed stirring at 50rpm, stirring uniformly, and subpackaging to obtain the drier.
Examples
The weight percentages of the components of the quick-drying adhesives of examples 1-11 are given in Table 4 below.
TABLE 4 weight percents of the components of the quick-drying adhesives of examples 1-11
Example 1
A quick-drying adhesive only comprises a silicon modified polyether adhesive, and the preparation method of the silicon modified polyether adhesive comprises the following steps: heating the novel alkyl phenolic tackifying resin to 130 ℃, adding high chlorinated polyethylene and macromolecular thermoplastic resin with the temperature range of 130 ℃, and uniformly stirring to obtain a premix;
and adding a water removing agent, an antioxidant and white carbon black into the MS prepolymer, heating to 120 ℃, stirring for reaction for 2.5 hours, transferring to the premix, then filling nitrogen to replace air in the reactor, cooling to about 60 ℃, filtering, extruding and packaging to obtain the silicon modified polyether adhesive.
The MS prepolymer of the embodiment is purchased from the Japanese Brillouin chemical industry, and the high chlorinated polyethylene is HCPE-L grade.
Example 2
A quick-drying adhesive, which is different from the adhesive of example 1 in that: the preparation examples of the novel alkyl phenolic tackifying resin and the macromolecular thermoplastic polyester resin are different from the weight ratio, and the weight ratio of the high chlorinated polyethylene is different.
Example 3
A quick-drying adhesive, which is different from the adhesive of example 1 in that:
macromolecular thermoplastic polyester resin the macromolecular thermoplastic polyester resin obtained in preparation example 3 was used.
Example 4
A quick-drying adhesive, which is different from the adhesive of example 1 in that:
macromolecular thermoplastic polyester resin the macromolecular thermoplastic polyester resin obtained in preparation example 4 was used.
Example 5
A quick-drying adhesive, which is different from the adhesive of example 1 in that:
macromolecular thermoplastic polyester resin the macromolecular thermoplastic polyester resin obtained in preparation example 5 was used.
Example 6
A quick-drying adhesive, which is different from the adhesive of example 1 in that:
macromolecular thermoplastic polyester resin the macromolecular thermoplastic polyester resin obtained in preparation example 6 was used.
Example 7
A quick-drying adhesive, which is different from the adhesive of example 1 in that:
0.2 wt% of antioxidant 1010 was also added.
Example 8
A quick-drying adhesive, which is different from example 7 in that:
the quick-drying adhesive also included the drier prepared in preparation example 1.
Example 9
A quick-drying adhesive, which is different from example 7 in that:
the quick-drying adhesive also included the drier prepared in preparation example 2.
Example 10
A quick-drying adhesive, which is different from example 7 in that:
the quick-drying adhesive further included the drier prepared in preparation example 3.
Example 11
A quick-drying adhesive, which is different from example 7 in that:
the quick-drying adhesive further included the drier prepared in preparation example 4.
Comparative example
Comparative example 1
An adhesive, differing from example 1 in that:
the novel alkylphenol aldehyde tackifying resin prepared in preparation example 1 is replaced by the same amount of the macromolecular thermoplastic polyester resin prepared in preparation example 1.
Comparative example 2
An adhesive, differing from example 1 in that:
the macromolecular thermoplastic polyester resin prepared in preparation example 1 was replaced by the same amount of the novel alkyl phenol formaldehyde tackifying resin prepared in preparation example 1.
Comparative example 3
An adhesive is prepared by the following steps:
sequentially putting 110kg of MS polymer, 50kg of polyoxypropylene glycol with the average relative molecular mass of 5000, 100kg of nano calcium carbonate, 35kg of white carbon black, 0.52kg of antioxidant 1010 and 0.52kg of UV327 into a planetary stirrer barrel, carrying out high-speed dispersion stirring, carrying out vacuum to-0.095 MPa at the temperature of 110 ℃ for dehydration for 2.5h, cooling to 35 ℃, then sequentially adding 3.5kg of silane coupling agent KH550 and 0.71kg of catalyst dibutyltin dilaurate, vacuumizing, uniformly stirring, discharging and packaging to obtain the adhesive.
Performance test data
Viscosity: with reference to astm d 1084, test rotational speed: 10 rpm;
surface drying time: dry-to-touch time, test conditions: 50% RH at 23 ℃ or 30% RH at-10 ℃;
curing speed: and (3) testing conditions are as follows: 50% RH at 23 ℃ or 30% RH at-10 ℃;
tensile strength: reference ISO 137;
shear strength: reference ISO 137;
elongation percentage: reference ISO 137;
sag resistance: with reference to GB/T13477.6, test temperature: 70 ℃;
shore hardness: see ISO 868.
TABLE 5 Performance data for the adhesives of examples 1-7 and comparative examples 1-3
Wherein, the conditions of the surface drying time and the curing speed test are 23 ℃ and 50% RH.
As can be seen from example 1 and comparative example 1 in combination with table 5, when the same amount of the macromolecular thermoplastic polyester resin was used in place of the novel alkyl phenol formaldehyde tackifying resin, the elongation of the silicon-modified polyether adhesive was improved, but the surface drying time of the silicon-modified polyether adhesive was prolonged, the curing speed was reduced, and the sagging resistance of the silicon-modified polyether adhesive was also reduced, which was not favorable for the construction of tile bonding.
From example 1 and comparative example 2 in combination with table 5, it is clear that when the macromolecular thermoplastic polyester resin is replaced with an equivalent amount of a novel alkyl tackifying resin, the surface drying time of the silicon-modified polyether adhesive is prolonged, the curing speed is reduced, the elongation and sag resistance are also reduced, and the construction for bonding tiles is also not facilitated.
According to the examples 1 to 7 and the comparative example 3 and the combination of the table 5, compared with the existing silicon modified polyether adhesive, the silicon modified polyether adhesive has the advantages of faster surface drying time, higher elongation, good sag resistance, better construction performance for the bonding of ceramic tiles and contribution to improving the initial adhesive performance of the ceramic tiles.
According to the examples 1, 3 and 4 and the combination of Table 5, it can be seen that the temperature rise rate is controlled to be 1-1.2 ℃/min, which is more favorable for improving the elongation and curing speed of the silicon modified polyether adhesive, that is, when the temperature rise rate is controlled to be 1-1.2 ℃/min, the flexibility of the silicon modified polyether adhesive is better, and the silicon modified polyether adhesive has high drying speed, no bubbles and good initial adhesion performance.
From example 1 and example 6 in combination with table 5, it is seen that the surface dry time of the silicon-modified polyether adhesive is prolonged and the elongation is reduced when 4', 4' -diphenylmethane diisocyanate is added in one step. That is, the curing speed of the silicon modified polyether adhesive is easily influenced by adding 4', 4-diphenylmethane diisocyanate in one step; in addition, the elongation of the silicon modified polyether adhesive is reduced, which shows that the flexibility of the silicon modified polyether adhesive is reduced, and the resistance of the silicon modified polyether adhesive to temperature and humidity deformation is poor.
TABLE 6 Performance data for quick-drying adhesives of examples 7-11
| Item | Example 7 | Example 8 | Example 9 | Example 10 | Example 11 |
| Time to surface dry (min) | 68 | 59 | 26 | 23 | 42 |
| Curing speed (mm/24h) | 1.5 | 1.8 | 4.4 | 4.5 | 3.0 |
Wherein, the test conditions of the surface drying time and the curing speed are-10 ℃ x 30% RH, and the same amount of corresponding drier is uniformly sprayed on the silicon modified polyether adhesive in the examples 8-11.
According to the data in the table 6 in combination with the examples 7 and 8-11, it can be seen that the addition of the drier is beneficial to improving the surface drying time and curing speed of the silicon modified polyether adhesive under the low-temperature drying condition.
As can be seen from example 8 and example 9 in combination with table 6, the addition of methylene chloride advantageously accelerates the cure rate of the silicon-modified polyether adhesive.
According to the data in the table 6 in the embodiment 8 and the embodiment 11, the surface drying time of the silicon modified polyether adhesive under the low-temperature drying condition is within 20-30min when the metal organic compound is selected from bismuth isooctanoate and zinc neodecanoate, and the amine compound is selected from dimorpholinylethyl ether.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A quick-drying adhesive is characterized in that: the adhesive comprises a silicon modified polyether adhesive, wherein the silicon modified polyether adhesive is prepared from the following raw materials in percentage by weight:
novel alkyl phenolic tackifying resins: 8 to 10 percent of
Highly chlorinated polyethylene: 32-35 percent
Macromolecular thermoplastic polyester resin: 20 to 23 percent of
Water removal agent: 0.05 to 0.1 percent
Antioxidant: 0 to 0.2 percent
White carbon black: 1.5 to 2 percent
MS prepolymer: balance of
The novel alkyl phenolic tackifying resin is silane coupling agent modified alkyl phenolic resin;
the molecular weight of the macromolecular thermoplastic polyester resin is 8-10 ten thousand.
2. A quick-drying adhesive according to claim 1, wherein: the novel alkyl phenolic tackifying resin comprises raw materials of alkyl phenolic resin, ethyl acetate, absolute ethyl alcohol and a silane coupling agent; wherein the mass of the alkyl phenolic resin is 28-32% of that of ethyl acetate, the mass of the absolute ethyl alcohol is 8-12% of that of the alkyl phenolic resin, and the mass of the silane coupling agent is 4-6% of that of the alkyl phenolic resin.
3. A quick-drying adhesive according to claim 2, wherein the novel alkyl phenol formaldehyde tackifying resin is prepared by the following method:
adding alkyl phenolic resin into ethyl acetate, stirring for dissolving, adding absolute ethyl alcohol and a silane coupling agent, stirring for reacting for 7.5-8.5h, then heating to 75-85 ℃, vacuumizing for recovering ethyl acetate and absolute ethyl alcohol, heating to 100 ℃, and vacuumizing for removing moisture to obtain the novel alkyl phenolic tackifying resin.
4. A quick-drying adhesive according to claim 1, wherein: the macromolecular thermoplastic polyester resin comprises the following raw materials:
diisocyanate
Polyester polyols
Low molecular weight diols
Wherein the molar ratio of isocyanic acid radical in the diisocyanate to the total amount of hydroxyl in the polyester polyol and the low molecular diol is 0.90-0.95;
the polyester polyol comprises 4000 molecular weight polyester polyol and 6000 molecular weight polyester polyol, and the weight ratio of the 4000 molecular weight polyester polyol to the 6000 molecular weight polyester polyol is (6-7): (3-4).
5. A quick-drying adhesive according to claim 4, wherein said macromolecular thermoplastic polyester resin is prepared by the following steps:
melting polyester polyol at the temperature of 105-;
wherein the weight ratio of the first part of diisocyanate to the second part of diisocyanate is 11 (10-12).
6. A quick-drying adhesive as claimed in claim 5, wherein the second part of diisocyanate is added, and after the reaction is continued for 0.8-1.2h, the temperature is raised to 105-115 ℃ at a temperature raising rate of 1-1.2 ℃/min.
7. The quick-drying adhesive according to claim 1, wherein the preparation method of the silicon-modified polyether adhesive comprises the following steps:
heating the novel alkyl phenolic tackifying resin to the temperature of 125-135 ℃, adding high chlorinated polyethylene and macromolecular thermoplastic resin with the temperature range of 125-135 ℃, and uniformly stirring to obtain a premix;
adding a water removing agent, an antioxidant and white carbon black into the MS prepolymer, heating to 115-125 ℃, stirring for reaction for 2-3h, transferring to a premix, then filling nitrogen to replace air in a reactor, cooling to about 60 ℃, filtering, extruding and packaging to obtain the silicon modified polyether adhesive.
8. A quick-drying adhesive according to any one of claims 1 to 7, wherein: the quick-drying adhesive also comprises a drier which is prepared from the following raw materials in percentage by weight:
metal organic compound: 1-1.2%
Amine compounds: 1 to 3 percent of
Dichloromethane: 35 to 40 percent of
Solvent: and (4) the balance.
9. A quick-drying adhesive according to claim 8, wherein: the metal organic compound comprises a bismuth organic compound and a zinc organic compound, the bismuth organic compound is bismuth isooctanoate, the zinc organic compound is zinc neodecanoate, and the weight ratio of the bismuth isooctanoate to the zinc neodecanoate is (2-3): and (3-2), the amine compound is dimorpholinylethyl ether.
10. A quick-drying adhesive according to claim 8, wherein: the solvent comprises one or more of ethyl acetate, methyl acetate and acetone.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024154691A1 (en) * | 2023-01-16 | 2024-07-25 | Ｍｃｐｐイノベーション合同会社 | Polyolefin composition, silane crosslinkable molded body, silane crosslinked molded body and use of same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106554732A (en) * | 2015-09-29 | 2017-04-05 | 什邡市美的家木业有限责任公司 | A kind of preparation method of adhesion agent for artificial board |
| CN107177340A (en) * | 2017-06-21 | 2017-09-19 | 三友（天津）高分子技术有限公司 | Transparent single component silane modified polyether seal glue of waterproof mould-proof-type and preparation method thereof |
| CN110172111A (en) * | 2019-05-09 | 2019-08-27 | 山东高信化学股份有限公司 | A kind of preparation method of the low temperature resistant high chlorinated polyethylene resin of glue |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106554732A (en) * | 2015-09-29 | 2017-04-05 | 什邡市美的家木业有限责任公司 | A kind of preparation method of adhesion agent for artificial board |
| CN107177340A (en) * | 2017-06-21 | 2017-09-19 | 三友（天津）高分子技术有限公司 | Transparent single component silane modified polyether seal glue of waterproof mould-proof-type and preparation method thereof |
| CN110172111A (en) * | 2019-05-09 | 2019-08-27 | 山东高信化学股份有限公司 | A kind of preparation method of the low temperature resistant high chlorinated polyethylene resin of glue |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024154691A1 (en) * | 2023-01-16 | 2024-07-25 | Ｍｃｐｐイノベーション合同会社 | Polyolefin composition, silane crosslinkable molded body, silane crosslinked molded body and use of same |
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