CN111019582B - Reactive polyurethane hot melt adhesive for household appliance sealing and preparation method thereof - Google Patents
Reactive polyurethane hot melt adhesive for household appliance sealing and preparation method thereof Download PDFInfo
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- CN111019582B CN111019582B CN201911214797.4A CN201911214797A CN111019582B CN 111019582 B CN111019582 B CN 111019582B CN 201911214797 A CN201911214797 A CN 201911214797A CN 111019582 B CN111019582 B CN 111019582B
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
-
- 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
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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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
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
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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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/329—Phosphorus containing acids
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a reactive polyurethane hot melt adhesive for sealing household appliances, which is characterized by comprising the following components in parts by weight: polyester polyol: 20-60 parts; polyether polyol: 5-25 parts; thermoplastic resin: 0-15 parts; tackifying resin: 0-15 parts; an adhesion promoter: 0-5 parts; antioxidant: 0-2 parts of a solvent; ultraviolet absorber: 0-2 parts of a solvent; a stabilizer: 0-0.5 parts; diisocyanate: 10-40 parts; catalyst: 0-1 part; silane coupling agent: 0-5 parts; the polyester polyol is one or more of crystalline polyester polyol and amorphous polyester polyol. The invention also discloses a preparation method of the composition. The hot melt adhesive provided by the invention effectively improves the assembly efficiency of sealing of the existing household appliance parts, and simultaneously solves the problem of bonding of the reactive polyurethane hot melt adhesive to galvanized iron and coating aluminum.
Description
Technical Field
The invention belongs to the technical field of polyurethane sealant synthesis, and particularly relates to a reactive polyurethane hot melt adhesive for household appliance sealing and a preparation method thereof.
Background
The reactive polyurethane hot melt adhesive is prepared by mixing an isocyanate group-terminated prepolymer synthesized by polyester or polyether polyol and diisocyanate with additives such as thermoplastic resin which does not react with isocyanate groups, tackifying resin, an antioxidant, an accelerator, a catalyst and the like. The reactive polyurethane adhesive is solid at normal temperature, and when the reactive polyurethane adhesive is used, the adhesive is heated, melted and glued on the surface of a material and substances such as air, moisture on the surface of an adherend or substances such as active hydrogen contained in the adherend, and reacts with the materials to form urea bonds to be partially crosslinked and cured. Therefore, the reactive polyurethane hot melt adhesive has the characteristics of high initial viscosity, high positioning speed and the like of the hot melt adhesive, and also has the characteristics of heat resistance, water resistance, chemical resistance, creep resistance and the like of the reactive adhesive, so that the reactive polyurethane hot melt adhesive is widely applied to the industries of automobile industry, shoe industry, textile industry, wood industry, electronic industry, white household appliances, book binding and the like.
For a long time, silicone adhesive has been used for sealing household electrical appliances. The silicone adhesive has good bonding effect, excellent flexibility, high and low temperature properties and weather resistance, but has poor initial adhesion and slow positioning speed. After parts are sealed, the parts are usually required to be placed for several hours to move, after the parts of the household appliance are sealed, the parts are cured at normal temperature for 24 hours, and then the next assembly process can be carried out, so that a large place is occupied, and the delivery time is prolonged, therefore, the development of a sealant which can be assembled in a short time is a difficult point in the sealing application of the household appliance, for example, the modulus of a two-component solvent-free reaction type polyurethane hot melt adhesive is required to reach 1300Mpa after the two-component solvent-free reaction type polyurethane hot melt adhesive is mixed for 24 hours in the CN108659775A publication.
According to the requirements of the assembly and the use environment of the household appliance motor, the adhesive for the household appliance motor is required to be positioned and solidified in a short time, the reliability of batch production after the motor is sealed is ensured, the process operation requirements of short-time online assembly and the like after the motor is sealed and bonded can be met, and the environment requirements of long-time vibration, shock cooling and sudden heating are met. Therefore, the sealant which is fast in positioning and curing, good in flexibility, aging resistance and water resistance is developed, and the urgent requirement of the fast sealing process of the household appliance motor is met.
However, the reactive polyurethane hot melt adhesive has the rapid positioning and curing performance of the hot melt adhesive, the production efficiency can be greatly improved in industrial production, and meanwhile, due to the characteristic of moisture crosslinking and curing, the reactive polyurethane hot melt adhesive has higher maximum bonding strength to metal, plastic, glass and the like and has excellent heat resistance, durability, chemical resistance and water resistance. Therefore, the reactive polyurethane hot melt adhesive is widely applied to the household appliance industry.
However, the reactive polyurethane hot melt adhesive has not been applied as a metal piece sealing product, so that the efficiency of sealing and assembling household appliance parts is low before a design, and meanwhile, the reactive polyurethane hot melt adhesive is very necessary for solving the problem of bonding of the reactive polyurethane hot melt adhesive to galvanized iron and coating aluminum.
Disclosure of Invention
In order to overcome the defects of the invention, the invention provides a reactive polyurethane hot melt adhesive for sealing household appliances.
The second purpose of the invention is to provide a preparation method of the reactive polyurethane hot melt adhesive for sealing household appliances.
In order to realize one of the purposes of the invention, the adopted technical scheme is as follows:
the reactive polyurethane hot melt adhesive for sealing the household appliances comprises the following components in parts by weight:
the polyester polyol is one or more of crystalline polyester polyol and amorphous polyester polyol.
The amount of the crystalline polyester polyol is preferably 15 to 35 parts by weight.
The amount of the amorphous polyester polyol is preferably 5 to 25 parts by weight.
In a preferred embodiment of the present invention, the crystalline polyester polyol is a crystalline polyester polyol obtained by polycondensation of one or any two or more of adipic acid, suberic acid, sebacic acid, dodecanedioic acid, or tetradecanedioic acid with one or any two or more of ethylene glycol, butanediol, hexanediol, octanediol, decanediol, dodecanediol, or diethylene glycol. A large number of experiments show that the crystalline polyester can improve the initial bonding strength and the final bonding strength of the polyurethane hot melt adhesive.
The crystalline polyester polyol is preferably polycaprolactone polyol or polycarbonate polyol.
The average weight average molecular weight of the crystalline polyester polyol is preferably 1000-10000.
In a preferred embodiment of the present invention, the amorphous polyester polyol is a polymer obtained by polycondensation of one or more of adipic acid, sebacic acid, maleic acid, fumaric acid, terephthalic acid, isophthalic acid, and phthalic acid, and one or more of ethylene glycol, butanediol, pentanediol, diethylene glycol, and neopentyl glycol.
The preferable average weight average molecular weight of the amorphous polyester polyol is 1000-10000.
The polyether polyol is preferably used in an amount of 5 to 25 parts by weight.
In a preferred embodiment of the present invention, the polyether polyol is any one or more of polyoxypropylene glycol, polyoxypropylene-oxyethylene glycol, polyethylene glycol, polytetrahydrofuran ether glycol or tetrahydrofuran-oxypropylene copolymer glycol.
The polyether polyol preferably has an average weight average molecular weight of 400 to 8000.
The amount of the thermoplastic resin is preferably 0 to 15 parts by weight.
In a preferred embodiment of the present invention, the thermoplastic resin is any one or more of an acrylic resin, a high molecular polyester, a thermoplastic polyurethane, an EVA resin, or a polyolefin resin.
The preferable dosage of the tackifying resin is 0-15 parts by weight according to the polyurethane hot melt adhesive.
In a preferred embodiment of the present invention, the tackifying resin is any one or more of phenolic resin, terpene resin and aldehyde ketone resin.
The amount of the adhesion promoter is preferably 0-5 parts by weight.
In a preferred embodiment of the present invention, the adhesion promoter is any one or more of epoxy resin, core-shell resin, and phosphate ester.
The antioxidant is preferably used in an amount of 0 to 1 part by weight.
In a preferred embodiment of the invention, the antioxidant is any one or more of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (1010) and tris [2, 4-di-tert-butylphenyl ] phosphite (168).
The amount of the ultraviolet absorber is preferably 0 to 1 part by weight.
In a preferred embodiment of the present invention, the ultraviolet absorber is any one or more of 2- (2 '-hydroxy-3', 5 '-di-tert-butylphenyl) -benzotriazole (UV320), 2- (2' -hydroxy-3 ',5' -ditert-pentylphenyl) benzotriazole (UV-328), or 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole (UV-P).
The amount of the stabilizer is preferably 0 to 0.5 part by weight.
In a preferred embodiment of the present invention, the stabilizer is any one or more of phosphoric acid, erucic acid, benzoic acid or citric acid.
In a preferred embodiment of the present invention, any one or more of the diisocyanate diphenylmethane diisocyanate (MDI), hydrogenated diphenylmethane diisocyanate (HMDI) or isophorone diisocyanate (IPDI), carbodiimide modified diphenylmethane diisocyanate (hdmdi).
In a preferred embodiment of the present invention, the catalyst is any one or more of trioctylamine, triethylene diamine, triethanolamine or dimorpholinodiethyl ether.
In a preferred embodiment of the present invention, the silane coupling agent is any one or more of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma mercaptopropyltriethoxysilane, gamma-mercaptopropyltrimethoxysilane, vinyltriethoxysilane, or vinyltrimethoxysilane and vinyltris (beta-methoxyethoxy) silane.
In order to realize the second purpose of the invention, the adopted technical scheme is as follows:
a preparation method of a reactive polyurethane hot melt adhesive for sealing household appliances comprises the following steps:
mixing: sequentially adding the polyester polyol, the polyether polyol, the thermoplastic resin, the tackifying resin, the adhesion promoter, the antioxidant, the ultraviolet absorbent and the stabilizer into a reaction kettle, melting, stirring and mixing, and then vacuumizing and dehydrating (the dehydration time is about 0.5-3.0 hours) at the temperature of 100-130 ℃ and the vacuum degree of-0.08-0.1 MPa to obtain a mixture;
a vacuum reaction step: then cooling the obtained mixture to 70-100 ℃, stirring and adding the diisocyanate, and heating and vacuumizing under the temperature condition of 100-130 ℃ and the vacuum degree condition of-0.08-0.1 MPa for reaction (the reaction time is about 0.5-3.0 hours); and finally, cooling to 80-100 ℃, and then adding the catalyst and the coupling agent to perform vacuum defoaming reaction to prepare the product.
In a preferred embodiment of the invention, the vacuum defoaming reaction is specifically performed by vacuumizing at 100-130 ℃ until no bubbles appear, and sampling to test the NCO% content and viscosity; when the content of NCO% reaches 1.0% -3.0% and the viscosity at 110-150 ℃ is 1000-20000 mPa.S, discharging, and hermetically packaging to obtain the product.
The invention has the beneficial effects that:
effectively improve the sealed assembly efficiency of present household electrical appliances part, solve the problem of reaction type polyurethane hot melt adhesive to the bonding of galvanized iron, coating aluminium simultaneously.
Detailed Description
The invention is further described with reference to the following examples, but is not intended to be limited thereto.
Example 1
The preparation method of the reactive polyurethane hot melt adhesive for sealing household appliances of the embodiment comprises the following steps:
1) adding 15 parts by weight of amorphous polyester polyol, 30 parts by weight of crystalline polyester polyol, 20 parts by weight of polyether polyol, 7 parts by weight of thermoplastic resin, 2 parts by weight of adhesion promoter, 0.1 part by weight of antioxidant, 0.1 part by weight of ultraviolet absorbent and 0.05 part by weight of stabilizer into a reaction kettle, and carrying out vacuum dehydration for 60 minutes at the temperature of 100-130 ℃;
2) cooling to 90 ℃, and adding 25 parts by weight of diisocyanate while stirring;
3) slowly heating to 100-120 ℃, and carrying out vacuum defoaming reaction for 60 minutes;
4) cooling to 100 ℃, adding 0.05 part by weight of catalyst and 0.7 part by weight of silane coupling agent, heating, vacuumizing at 100-130 ℃ until no bubbles appear, and testing viscosity and NCO%;
5) and discharging, sealing and packaging after the viscosity and the NCO% are qualified to obtain the product.
The amorphous polyester polyol in this example is Asahi Kawakawa chemical EPPI-2000NP or Dynacoll7200, and has an average weight average molecular weight of 2000-5500.
The crystalline polyester polyol in the embodiment is a product in Dynacoll7300 series or PHA, and the average weight average molecular weight of the crystalline polyester polyol is 2000-3500.
The polyether polyol in the embodiment is polyoxyethylene glycol, and the average weight average molecular weight of the polyether polyol is 400-2000.
The thermoplastic resin in this example is TPU.
The adhesion promoter in this example was bisphenol a epoxy E-44.
The antioxidant in this example is 1010; the ultraviolet absorbent is UV-328; the stabilizer is erucic acid; isocyanate is diphenylmethane and isocyanate; the catalyst is dimorpholinodiethyl ether; the silane coupling agent is gamma-glycidol ether oxygen propyl trimethoxy silane.
The technical indexes of the household appliance sealing reaction type polyurethane hot melt adhesive are as follows:
the viscosity is 8000 mPa.S/120 ℃;
NCO％:1.8％；
opening time: 3 min;
and (3) storage period: filling nitrogen, sealing, and storing at 5-30 deg.C for 6 months;
example 2
The preparation method of the reactive polyurethane hot melt adhesive for sealing household appliances of the embodiment comprises the following steps:
1) adding 25 parts by weight of amorphous polyester polyol, 30 parts by weight of crystalline polyester polyol, 15 parts by weight of polyether polyol, 6 parts by weight of tackifying resin, 2 parts by weight of adhesion promoter, 0.1 part by weight of antioxidant, 0.1 part by weight of ultraviolet absorbent and 0.05 part by weight of stabilizer into a reaction kettle, and carrying out vacuum dehydration for 60 minutes at 100-130 ℃;
2) cooling to 85 ℃, and adding 21 parts by weight of isocyanate while stirring;
3) slowly heating to 100-130 ℃, and carrying out vacuum defoaming reaction for 60 minutes;
4) cooling to 110 ℃, adding 0.05 part by weight of catalyst and 0.7 part by weight of silane coupling agent, heating, vacuumizing at 100-130 ℃ until no bubbles appear, and testing viscosity and NCO%;
5) and discharging, sealing and packaging after the viscosity and the NCO% are qualified to obtain the product.
The amorphous polyester polyol in the embodiment is Dynacoll7200 and/or Spodopan PH-56, PD-56 and PDP-70, and the average weight average molecular weight of the amorphous polyester polyol is 1000-5500.
The crystalline polyester polyol in the embodiment is a product in Dynacoll7300 series or a product in Changxing 5600 series, and the average weight average molecular weight of the crystalline polyester polyol is 2000-10000.
The polyether polyol in the embodiment is polyoxypropylene glycol, and the average weight average molecular weight of the polyether polyol is 1000-4000.
The tackifying resin in this example is an aldehyde ketone resin.
The adhesion promoter in this example is a phosphate ester.
The antioxidant in this example is 1010; the ultraviolet absorbent is UV-328; the stabilizer is oxalic acid;
the isocyanate in this example is diphenylmethane and isocyanate;
the catalyst in this example was dimorpholinodiethyl ether;
the silane coupling agent in this example was gamma-glycidoxypropyltrimethoxysilane.
The technical indexes of the household appliance motor sealing reaction type polyurethane hot melt adhesive in the embodiment are as follows:
the viscosity is 6000 mPa.S/120 ℃;
NCO％:2.1％；
opening time is 4 min;
and (3) storage period: filling nitrogen, sealing, and storing at 5-30 deg.C for 6 months;
example 3
1) Adding 10 parts by weight of amorphous polyester polyol, 20 parts by weight of crystalline polyester polyol, 25 parts by weight of polyether polyol, 20 parts by weight of thermoplastic resin, 5 parts by weight of tackifying resin, 0.1 part by weight of antioxidant, 0.1 part by weight of ultraviolet absorbent and 0.05 part by weight of stabilizer into a reaction kettle, and carrying out vacuum dehydration for 60 minutes at the temperature of 110-130 ℃;
2) cooling to 80 ℃, and adding 18 parts by weight of isocyanate while stirring;
3) slowly heating to 100-130 ℃, and carrying out vacuum defoaming reaction for 60 minutes;
4) cooling to 90 ℃, adding 0.05 weight part of catalyst and 1.7 weight parts of silane coupling agent, heating, vacuumizing at 100-130 ℃ until no bubbles appear, and testing viscosity and NCO%;
5) and discharging, sealing and packaging after the viscosity and the NCO% are qualified to obtain the product.
The amorphous polyester polyol in the embodiment is Dynacoll7200 and/or Asahi XCP244C, and the average weight average molecular weight is 3500-5500.
The crystalline polyester polyol in the embodiment is a product in Dynacoll7300 series or Hooke F-900 series, and the average weight average molecular weight of the crystalline polyester polyol is 2000-8500.
The polyether polyol in the embodiment is polyoxypropylene glycol, and the average weight average molecular weight of the polyether polyol is 400-4000.
The thermoplastic resin in this example is an acrylic resin.
The tackifying resin in this example is an aldehyde ketone resin.
The antioxidant in this example is 1010; the ultraviolet absorbent is UV-328; the stabilizer is phosphoric acid;
the isocyanate in this example is diphenylmethane and isocyanate;
the catalyst in this example was dimorpholinodiethyl ether;
the silane coupling agent in this example was gamma-glycidoxypropyltrimethoxysilane.
The technical indexes of the household appliance motor sealing reaction type polyurethane hot melt adhesive in the embodiment are as follows:
the viscosity is 8000 mPa.S/120 ℃;
NCO％:1.5％；
the opening time is 2 min;
and (3) storage period: filling nitrogen, sealing, and storing at 5-30 deg.C for 6 months;
the detection method of the above embodiment:
measurement of viscosity:
and testing the viscosity by using a vertebral plate viscometer at the rotating speed of 100 revolutions and the temperature of 120 ℃, setting the time detection for 60 seconds, and filling the product on a vertebral plate for detection.
Determination of NCO%:
the product was reacted with an excess of di-n-butylamine standard solution in butanone and then titrated with HCl solution to determine NCO%.
Determination of the open time:
the product was melted at 120 ℃ for 30min, and then 1mm strips of wood were coated with a glass rod and touched with a fingertip, ending with a time to develop dry tackiness.
Determination of tensile shear strength:
and preparing samples and testing according to the GB/T7124-2008 standard.
Bonding material: galvanized iron and coated iron, galvanized iron and metal aluminum, and coated iron and metal aluminum
Curing: curing at 23 ℃ and 65% for 7 days;
tensile shear strength rate: v is 5 mm/min.
Preparing a household appliance sealing sample piece:
1. heating the product to 110-130 ℃ for melting, and striking the product at the seam of the motor shell to be sealed at 110-130 ℃.
2. And testing the positioning performance and the motor mobility of the glue.
3. Curing and solidifying at 23 ℃ and 65%.
Low-temperature experiment:
the motor casing is placed in a test box at the temperature of minus 35 ℃, after 72-hour low-temperature test, the motor casing is placed in an environment with the humidity of 50 percent at the temperature of 23 ℃ for 16 hours, and then whether the sealing position of gluing is well sealed or not is observed, and the hardness has no obvious change.
High temperature experiment:
the motor casing is placed in a test box at 120 ℃ for 96 hours of high-temperature test, then placed in an environment with the humidity of 50 percent at 23 ℃ for 16 hours, and then whether the sealing position of the gluing seal is well sealed or not is observed, and the hardness has no obvious change.
Rain test:
the swinging pipe is provided with water spray holes in a radian section of 180 degrees, the swinging pipe swings to each side to the maximum extent at the speed of 60 degrees/s, so that the motor is sprayed with water in all directions for at least 10min, and no harmful influence is caused after the test.
And (3) corrosion test:
the solidified sample is put into No. 68 lubricating oil to be soaked for 24 hours without foaming phenomenon, and then is put into air without reaction phenomenon.
Flame retardant property:
after the product is burnt by a lighter for 15S and leaves, the product is self-extinguished within 5S.
Salt spray test:
the samples were uniformly coated on copper foil and tested according to the regulations of GB/T2423.17 for a duration of 72 hours, and the protected copper foil after the test should be free of corrosion.
Insulating property:
insulation resistance tester, voltage not less than 18 KV/mm.
TABLE 1 comparison of test results for Motor casing samples
Wherein the silica gel material is a common material in the market.
TABLE 2 shear Strength comparison test results
From the test situation, the samples sealed by the product of the invention in comparative examples 1, 2 and 3 and silica gel can meet the requirements of motor sealing performance in low temperature resistance, high temperature resistance, water resistance, corrosion resistance, flame retardant performance, salt spray performance and insulating performance.
Compared with the silica gel, the hot melt adhesive has shorter opening time and shorter movable time of the motor, thereby greatly improving the assembly efficiency of motor production;
meanwhile, the comparison test of the tensile shear strength confirms that the reaction type polyurethane hot melt adhesive has higher bonding strength to coating paste, galvanized iron and metal aluminum, and also proves the requirement of the composite household appliance industry on the sealing performance.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (2)
1. The reactive polyurethane hot melt adhesive for sealing household appliances is characterized by comprising the following components in parts by weight:
the polyester polyol is a mixture of amorphous polyester polyol and crystalline polyester polyol,
the mixing ratio of the amorphous polyester polyol to the crystalline polyester polyol in the mixture is 15:30, 25: 30 or 10: 20;
the average weight average molecular weight of the amorphous polyester polyol is 1000-5500;
the average weight average molecular weight of the crystalline polyester polyol is 2000-10000;
the polyether polyol has an average weight average molecular weight of 400-8000;
the crystalline polyester polyol is any one or more of polycaprolactone polyol or polycarbonate polyol;
the amorphous polyester polyol is a polymer formed by polycondensation of one or more than two of adipic acid, sebacic acid, maleic acid, fumaric acid, terephthalic acid, isophthalic acid or phthalic acid and one or more than two of ethylene glycol, butanediol, pentanediol, diethylene glycol or neopentyl glycol;
the polyether glycol is any one or more of polyoxypropylene glycol, polyoxypropylene-ethylene oxide glycol, polyethylene glycol, polytetrahydrofuran ether glycol or tetrahydrofuran-propylene oxide copolymerization glycol;
the thermoplastic resin is any one or more of acrylic resin, high-molecular polyester, thermoplastic polyurethane, EVA resin or polyolefin resin;
the tackifying resin is any one or more of phenolic resin, terpene resin and aldehyde ketone resin;
the adhesion promoter is any one or more of epoxy resin, core-shell resin and phosphate ester;
the antioxidant is one or more of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and tri [2, 4-di-tert-butylphenyl ] phosphite;
the ultraviolet absorbent is any one or more of 2- (2 '-hydroxy-3', 5 '-di-tert-butylphenyl) -benzotriazole, 2- (2' -hydroxy-3 ',5' -ditert-pentylphenyl) benzotriazole or 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole;
the stabilizer is phosphoric acid;
the diisocyanate is diphenylmethane diisocyanate;
the catalyst is dimorpholinodiethylether;
the silane coupling agent is gamma-glycidol ether oxygen propyl trimethoxy silane;
the parts of at least two of the thermoplastic resin, the tackifying resin or the adhesion promoter are not 0.
2. The preparation method of the reactive polyurethane hot melt adhesive for sealing household appliances, according to claim 1, is characterized by comprising the following steps:
mixing: sequentially adding the polyester polyol, the polyether polyol, the thermoplastic resin, the tackifying resin, the adhesion promoter, the antioxidant, the ultraviolet absorbent and the stabilizer into a reaction kettle, melting, stirring and mixing, and then vacuumizing and dehydrating at the temperature of 100-130 ℃ and the vacuum degree of-0.08-0.1 MPa for about 0.5-3.0 hours to obtain a mixture;
a vacuum reaction step: then cooling the obtained mixture to 70-100 ℃, stirring and adding the diisocyanate, heating and vacuumizing for reaction at the temperature of 100-130 ℃ and the vacuum degree of-0.08-0.1 MPa, wherein the reaction time is about 0.5-3.0 hours; finally, cooling to 80-100 ℃, and then adding the catalyst and the coupling agent to carry out vacuum defoaming reaction to prepare a product;
the vacuum defoaming reaction is to pump vacuum at 100-130 ℃ until no bubbles appear, and sample to test the NCO% content and viscosity; when the content of NCO% reaches 1.0% -3.0% and the viscosity at 110-150 ℃ is 1000-20000 mPa.S, discharging, and hermetically packaging to obtain the product.
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