CN114736642A - Reactive polyurethane hot melt adhesive for fabricated building and preparation method thereof - Google Patents

Reactive polyurethane hot melt adhesive for fabricated building and preparation method thereof Download PDF

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CN114736642A
CN114736642A CN202110880365.8A CN202110880365A CN114736642A CN 114736642 A CN114736642 A CN 114736642A CN 202110880365 A CN202110880365 A CN 202110880365A CN 114736642 A CN114736642 A CN 114736642A
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hot melt
melt adhesive
tackifying resin
polyurethane hot
reactive polyurethane
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徐彬彬
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Wuxi Wanli Adhesion Materials Co ltd
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Wuxi Wanli Adhesion Materials Co ltd
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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
    • 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
    • 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
    • C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
    • C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
    • 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
    • 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
    • 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
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/91—Use of waste materials as fillers for mortars or concrete

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention relates to the technical field of polyurethane hot melt adhesives, in particular to a reactive polyurethane hot melt adhesive for an assembly type building and a preparation method thereof. The preparation raw materials comprise the following components in parts by weight: 15-40 parts of polyester polyol, 15-30 parts of polyether polyol, 10-40 parts of tackifying resin A, 15-25 parts of tackifying resin B, 10-35 parts of isocyanate, 0-0.1 part of catalyst, 1-2 parts of coupling agent and 0-1 part of antioxidant; the tackifying resin A and the tackifying resin B are resins obtained by polymerizing acrylate derivatives serving as monomers. The regulation and control of the components and the proportion of the tackifying resin, the polyhydric alcohol and the coupling agent adopted in the application can obviously improve the initial viscosity of the hot melt adhesive, so that the hot melt adhesive can be firmly bonded when being bonded with materials such as thicker fireproof skins, rebound is avoided, the opening time can be prolonged, and the construction can be performed for sufficient time for constructors. Meanwhile, the hot melt adhesive has excellent water bubble performance, so that the hot melt adhesive can still keep good bonding performance to the base material when being soaked in water.

Description

Reactive polyurethane hot melt adhesive for fabricated building and preparation method thereof
Technical Field
The invention relates to the technical field of polyurethane hot melt adhesives, in particular to a reactive polyurethane hot melt adhesive for an assembly type building and a preparation method thereof.
Background
The calcium silicate board is a siliceous material (the main component is SiO)2)、The novel inorganic building material is prepared by matching the components such as a calcareous material (main component CaO), reinforcing fibers, some auxiliaries and the like according to a certain proportion and performing the procedures of mould pressing, steam pressing and the like, has the advantages of excellent fireproof performance, moisture resistance and long service life besides the functions of the traditional gypsum board, but cannot be widely used due to single color and pattern of the calcium silicate board, and can meet the market demand by being adhered with PVC or fireproof skins with various patterns. However, due to the special surface of the calcium silicate plate, the method of hot pressing and integrating cannot be used, so that the calcium silicate plate needs to be adhered by glue. Conventional gum products are available in a wide variety of forms, but have varying properties.
For example, chinese patent CN201910702184 discloses a light/wet dual-curing polyurethane hot melt adhesive and a preparation method thereof, wherein multiple components such as multiple polyols, thermoplastic resins, acrylic acid active monomers, diluents, stabilizers, defoamers, coupling agents and the like are adopted to obtain the polyurethane hot melt adhesive with characteristics of high bonding efficiency, low viscosity, no wire drawing, long open time and the like. However, due to the surface specificity of calcium silicate boards and the application characteristics in the field of fabricated construction, the hot melt adhesives have not yet fully met the requirements.
Disclosure of Invention
In order to solve the technical problems, the first aspect of the invention provides a reactive polyurethane hot melt adhesive, which comprises the following raw materials in parts by weight:
Figure BDA0003192010110000011
the tackifying resin A and the tackifying resin B are resins obtained by polymerizing acrylate derivatives serving as monomers.
In a preferred embodiment of the present invention, the acrylate derivative is selected from one or more of methyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, and hydroxyethyl methacrylate.
The tackifying resin A and the tackifying resin B in the application can be prepared by adopting the acrylate derivative reaction monomer through bulk polymerization or suspension polymerization.
Furthermore, the hydroxyl value of the tackifying resin B is 1-5 mg KOH/g.
Furthermore, the weight average molecular weight of the tackifying resin B is 30000-80000.
Furthermore, the weight average molecular weight of the tackifying resin B is 30000-50000.
The tackifying resin B of the application can be selected from related products on the market, such as products 4014, 2978 and 2903 of Mitsubishi in Japan, and products BM19 and BM758 of Brinell chemical industry.
Furthermore, the weight average molecular weight of the tackifying resin A is 30000-70000.
Further, the weight average molecular weight of the tackifying resin a is 30000, 45000.
Further, the glass transition temperature of the tackifying resin A is not lower than 30 ℃.
Further, the tackifying resin A has a glass transition temperature of 50 ℃ and a glass transition temperature of 75 ℃.
The tackifying resin A of the present application can be selected from the related products on the market, such as products with the brand numbers BR113, 106, 116 of Mitsubishi, Japan.
As a preferred technical scheme of the invention, the preparation monomers of the polyester polyol are dibasic acid and dihydric alcohol; the dibasic acid is selected from one or more of adipic acid, sebacic acid, suberic acid, dodecanedioic acid and tetradecanedioic acid.
Further, the dihydric alcohol is selected from one or more of 1, 2-ethanediol, 1, 4-butanediol, 1, 6-hexanediol, 1, 8-octanediol, 1, 10-decanediol, 1, 12-dodecanediol, diethylene glycol and neopentyl glycol.
Further, the polyester polyol is a crystalline polyester polyol.
Furthermore, the hydroxyl value of the polyester polyol is 10-34 mgKOH/g.
Further, the hydroxyl value of the polyester polyol is 27-34 mgKOH/g.
Furthermore, the molecular weight of the polyester polyol is 3500-8500 g/mol.
Further, the molecular weight of the polyester polyol is 3500 g/mol.
The polyester polyol in the application can be selected from related products on the market, such as products with the trade names Dynacoll 7360, 7390, 7380, 7361 and the like which win Chuangdegusai.
As a preferred technical scheme of the invention, the polyether polyol in the application is one or a mixture of more of polyoxypropylene glycol, polyethylene glycol, polytetrahydrofuran ether glycol and tetrahydrofuran-propylene oxide copolymerized glycol.
Further, the number average molecular weight of the polyether polyol is 400-4000.
Further, the number average molecular weight of the polyether polyol is 500-3000.
Further, the number average molecular weight of the polyether polyol is 1000-2500.
The polyether polyol used in the present application may be any commercially available product, including but not limited to Dow chemical products having the designations 2110TB, 2120, 222-.
As a preferable technical scheme of the invention, the coupling agent is an isocyanate silane coupling agent.
The isocyanatosilane coupling agent as used herein refers to a siloxane containing isocyanate groups in its molecular structure. The isocyanate silane coupling agent can be prepared by the reaction between a conventional isocyanate component and a silane coupling agent component, and related products on the market can also be selected.
Further, the isocyanate silane coupling agent is selected from one or more of 3-isocyanate propyl trimethoxy silane (T-03), 3-isocyanate propyl triethoxy silane (T-13) and 3-isocyanate propyl methyl dimethoxy silane (T-02).
Furthermore, 3-isocyanate propyl trimethoxy silane (T-03) can be a T-03 product of a Huaian macrograph new material.
The isocyanate used in the present application is an isocyanate having a functionality of 2, and the specific type is not particularly limited, and various diisocyanates known to those skilled in the art, including aliphatic diisocyanate, alicyclic diisocyanate, and aromatic diisocyanate, may be used. The aliphatic diisocyanate includes, but is not limited to, propylene diisocyanate, tetramethylene diisocyanate, pentamethylene diisocyanate, 1, 6-hexamethylene diisocyanate, 1, 2-propylene diisocyanate, 1, 2-butylene diisocyanate, 2, 3-butylene diisocyanate, 1, 3-butylene diisocyanate, 2,4, 4-or 2,2, 4-trimethyl 1, 6-hexamethylene diisocyanate, methyl 2, 6-diisocyanatohexanoate, and the like. As the alicyclic diisocyanate, there may be mentioned, but not limited to, 1, 3-cyclopentane diisocyanate, 1, 4-cyclohexane diisocyanate, 1, 3-cyclohexane diisocyanate, 3-isocyanatomethyl-3, 5, 5-trimethylcyclohexane isocyanate (alias: isophorone diisocyanate), 4' -methylenebis (cyclohexyl isocyanate), methyl-2, 4-cyclohexane diisocyanate, methyl-2, 6-cyclohexane diisocyanate, 1, 3-bis (isocyanatomethyl) cyclohexane, 1, 3-bis (isocyanatoethyl) cyclohexane, 1, 4-bis (isocyanatoethyl) cyclohexane, 2, 5-or 2, 6-bis (isocyanatomethyl) Norbornane (NBDI), mixtures thereof and the like. The aromatic diisocyanate includes, but is not limited to, 2, 4-tolylene diisocyanate and 2, 6-tolylene diisocyanate, and isomer mixtures of the tolylene diisocyanates, 4' -diphenylmethane diisocyanate, 2,4' -diphenylmethane diisocyanate and 2,2' -diphenylmethane diisocyanate, and arbitrary isomer mixtures of the diphenylmethane diisocyanates, tolylene diisocyanate, p-phenylene diisocyanate, naphthalene diisocyanate, and the like.
Further, the isocyanate is MDI.
The catalyst is a component for improving the hardening speed between components such as isocyanate and polyol, and the specific selection of the catalyst is not particularly limited, and conventional catalyst components in the field can be selected. Including but not limited to tertiary amine-based catalysts, organometallic-based catalysts, and the like. Examples thereof include triethylenediamine, bis (dimethylaminoethyl) ether, N-methylmorpholine, N-methylimidazole, N, N-dimethylcyclohexylamine, N, N, N ', N ' -tetramethylalkylenediamine, N, N-dimethylbenzylamine, N-ethylmorpholine, triethanolamine, N, N ' -dimethylpyridine, bismuth laurate, bismuth neodecanoate, bismuth naphthenate, stannous octoate (T9), dibutyltin dilaurate (T12), and zinc isooctanoate.
The antioxidant of the present invention may be selected from various antioxidants known to those skilled in the art, including but not limited to phenolic antioxidants, amine antioxidants, heterocyclic antioxidants, peroxide decomposition antioxidants, organic phosphorus antioxidants, and the like. Examples of the antioxidant include antioxidant 1010 and antioxidant 168.
The applicant finds that the initial viscosity of the hot melt adhesive can be obviously improved by regulating and controlling the components and the proportion of the tackifying resin, the polyhydric alcohol and the coupling agent adopted in the application, so that the hot melt adhesive can be firmly bonded when being bonded with materials such as thicker fireproof skins and the like, the rebound is avoided, the opening time can be prolonged, and the sufficient time is left for construction of constructors. Meanwhile, the water bubble performance of the hot melt adhesive can be improved to a great extent by optimizing the relevant physicochemical properties of the tackifying resin A, the tackifying resin B and the polyester polyol, so that the hot melt adhesive can still keep good bonding performance to a base material when being soaked in water. Particularly, when the tackifying resin A with the molecular weight of about 45000 and the glass transition temperature of 50 ℃ and the tackifying resin B with the molecular weight of about 34000 and the crystalline polyester polyol with the specific molecular weight and the hydroxyl value are adopted to prepare the hot melt adhesive, an obtained sample does not crack after being soaked for 4 hours at the high temperature of 60 ℃, the problems of cracking and the like do not occur in two days at the normal temperature, and the effect is very good. The applicant speculates that under the interaction among the technical parameters, when the hot melt adhesive is used for bonding a substrate, the adhesive layer forms a compact and orderly arranged microstructure, so that the permeation of water molecules in the outside can be effectively prevented, and meanwhile, the further damage of the water molecules to the adhesive layer is also prevented due to the close accumulation of molecular chains, so that the hot melt adhesive has good stability when being soaked in high-temperature or normal-temperature water.
The second aspect of the present invention provides a preparation method of the reactive polyurethane hot melt adhesive, which comprises the following steps:
(1) putting the polyol, the tackifying resin A, the tackifying resin B and the antioxidant into a reaction kettle according to a ratio, dissolving and stirring for 1-3 hours at 140-160 ℃, then cooling to 120 ℃, and vacuumizing and drying for 1-3 hours;
(2) cooling the system to 70-85 ℃, adding isocyanate while stirring, reacting for 0.5-1.5 hours at 80-90 ℃, then heating to 110 ℃, vacuumizing for 30 minutes, adding a catalyst, dispersing for 5-15 minutes, adding a coupling agent, dispersing and discharging to obtain the catalyst.
Further, the preparation method of the reactive polyurethane hot melt adhesive comprises the following steps:
(1) and (3) putting the polyol, the tackifying resin A, the tackifying resin B, the antioxidant and the like into a reaction kettle, and dissolving and stirring for 1.5 hours at 150 ℃. Cooling to 120 ℃, starting to vacuumize, and dehydrating for 1.5 hours under the condition that the vacuum degree is less than or equal to 0.1 MPa;
(2) cooling to 75-80 deg.C, and adding isocyanate under high speed stirring. Keeping the temperature of 80-90 ℃ for reaction for 40 minutes, slowly heating to 110 ℃, and heating for 40 minutes. Vacuumizing for 30 minutes, adding a catalyst, dispersing for 10 minutes, adding a coupling agent, dispersing for 5 minutes, and discharging to obtain the catalyst.
The third aspect of the invention provides application of the reactive polyurethane hot melt adhesive, which is applied to the field of fabricated buildings.
Compared with the prior art, the application has the following beneficial effects: the regulation and control of the components and the proportion of the tackifying resin, the polyhydric alcohol and the coupling agent adopted in the application can obviously improve the initial viscosity of the hot melt adhesive, so that the hot melt adhesive can be firmly bonded when being bonded with thicker fireproof skins and other materials, the rebound is avoided, the open time can be prolonged, and the sufficient time for construction can be reserved for constructors. Meanwhile, the water bubble performance of the hot melt adhesive can be improved to a great extent by optimizing the relevant physicochemical properties of the tackifying resin A, the tackifying resin B and the polyester polyol, so that the hot melt adhesive can still keep good bonding performance to a base material when being soaked in water. But also has excellent water bubble performance, and can keep excellent stability in high-temperature water for intestinal anastomosis.
Detailed Description
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention. In addition, the starting materials used are all commercially available products, unless otherwise specified.
Example 1: the embodiment provides a reactive polyurethane hot melt adhesive, which comprises the following raw materials in parts by weight:
Figure BDA0003192010110000061
the weight-average molecular weight of the tackifying resin A is 45000, the glass transition temperature is 50 ℃, and a product with the Japanese mitsubishi brand BR113 is adopted; the weight-average molecular weight of the tackifying resin B is 34000, the hydroxyl value is 3.2mg KOH/g, and a product of Brilliant chemical industry with the brand number of BM19 is adopted; the isocyanate is MDI; the polyester polyol is crystalline polyester polyol, the hydroxyl value is 27-34 mgKOH/g, the molecular weight is 3500g/mol, and the grade of Yingchuangdegai is Dynacoll 7390; the polyether polyol is 2110TB of Dow chemical; the catalyst is dibutyltin dilaurate; the coupling agent is 3-isocyanate propyl trimethoxy silane, and a T-03 product of a Huaian macro pattern new material is adopted; the antioxidant is antioxidant 1010.
The preparation method of the reactive polyurethane hot melt adhesive comprises the following steps:
(1) putting the polyol, the tackifying resin A, the tackifying resin B, the antioxidant and the like into a reaction kettle, and dissolving and stirring for 1.5 hours at 150 ℃; cooling to 120 ℃, starting to vacuumize, and dehydrating for 1.5 hours under the condition that the vacuum degree is less than or equal to 0.1 MPa;
(2) cooling to 80 ℃, and adding isocyanate under the condition of high-speed stirring; keeping the temperature at 85 ℃ for reacting for 40 minutes, slowly heating to 110 ℃, and heating for 40 minutes; vacuumizing for 30 minutes, adding a catalyst, dispersing for 10 minutes, adding a coupling agent, dispersing for 5 minutes, and discharging to obtain the catalyst.
Example 2: the embodiment provides a reactive polyurethane hot melt adhesive, which comprises the following raw materials in parts by weight:
Figure BDA0003192010110000062
Figure BDA0003192010110000071
the tackifying resin A adopts a product with the brand number BR116 of Mitsubishi of Japan; the tackifying resin B adopts a product with the name of 4014 of Mitsubishi of Japan; the isocyanate is MDI; the polyester polyol is crystalline polyester polyol, the hydroxyl value is 27-34 mgKOH/g, the molecular weight is 3500g/mol, and the grade of Yingchuangdegai is Dynacoll 7380; the polyether polyol is 2110TB of Dow chemical; the catalyst is dibutyltin dilaurate; the coupling agent is 3-isocyanate propyl trimethoxy silane, and a T-03 product of a Huaian macro pattern new material is adopted; the antioxidant is antioxidant 1010.
The preparation method of the reactive polyurethane hot melt adhesive comprises the following steps:
(1) putting the polyol, the tackifying resin A, the tackifying resin B, the antioxidant and the like into a reaction kettle, and dissolving and stirring for 1.5 hours at 150 ℃; cooling to 120 ℃, starting to vacuumize, and dehydrating for 1.5 hours under the condition that the vacuum degree is less than or equal to 0.1 MPa;
(2) cooling to 80 ℃, and adding isocyanate under the condition of high-speed stirring; keeping the temperature at 85 ℃ for reacting for 40 minutes, slowly heating to 110 ℃, and heating for 40 minutes; vacuumizing for 30 minutes, adding a catalyst, dispersing for 10 minutes, adding a coupling agent, dispersing for 5 minutes, and discharging to obtain the catalyst.
Example 3: this example provides a reactive polyurethane hot melt adhesive, which comprises the following raw materials (by weight portion)The following components:
Figure BDA0003192010110000072
the weight-average molecular weight of the tackifying resin A is 45000, the glass transition temperature is 50 ℃, and a product with the Japanese mitsubishi brand BR113 is adopted; the weight-average molecular weight of the tackifying resin B is 34000, the hydroxyl value is 3.2mg KOH/g, and a product of Brilliant chemical industry with the brand number of BM19 is adopted; the isocyanate is MDI; the polyester polyol is crystalline polyester polyol, the hydroxyl value is 27-34 mgKOH/g, the molecular weight is 3500g/mol, and the grade of Yingchuangdegai is Dynacoll 7360; the polyether polyol is 2110TB of Dow chemical; the catalyst is dibutyltin dilaurate; the coupling agent is 3-isocyanate propyl trimethoxy silane, and a T-03 product of a Huaian macro pattern new material is adopted; the antioxidant is antioxidant 1010.
The preparation method of the reactive polyurethane hot melt adhesive comprises the following steps:
(1) putting the polyol, the tackifying resin A, the tackifying resin B, the antioxidant and the like into a reaction kettle, and dissolving and stirring for 1.5 hours at 150 ℃; cooling to 120 ℃, starting to vacuumize, and dehydrating for 1.5 hours under the condition that the vacuum degree is less than or equal to 0.1 MPa;
(2) cooling to 80 ℃, and adding isocyanate under the condition of high-speed stirring; keeping the temperature at 85 ℃ for reacting for 40 minutes, slowly heating to 110 ℃, and heating for 40 minutes; vacuumizing for 30 minutes, adding a catalyst, dispersing for 10 minutes, adding a coupling agent, dispersing for 5 minutes, and discharging to obtain the catalyst.
Example 4: the embodiment provides a reactive polyurethane hot melt adhesive, which comprises the following raw materials in parts by weight:
Figure BDA0003192010110000081
the weight average molecular weight of the tackifying resin A is 45000, the glass transition temperature is 50 ℃, and a product with the brand number of Mitsubishi of Japan as BR113 is adopted; the isocyanate is MDI; the polyester polyol is crystalline polyester polyol, the hydroxyl value is 27-34 mgKOH/g, the molecular weight is 3500g/mol, and the grade of Yingchuangdegai is Dynacoll 7360; the polyether polyol is 2110TB of Dow chemical; the catalyst is dibutyltin dilaurate; the coupling agent is 3-isocyanate propyl trimethoxy silane, and a T-03 product of a Huaian macro pattern new material is adopted; the antioxidant is antioxidant 1010.
The preparation method of the reactive polyurethane hot melt adhesive comprises the following steps:
(1) putting the polyol, the tackifying resin A, the tackifying resin B, the antioxidant and the like into a reaction kettle, and dissolving and stirring for 1.5 hours at 150 ℃; cooling to 120 ℃, starting to vacuumize, and dehydrating for 1.5 hours under the condition that the vacuum degree is less than or equal to 0.1 MPa;
(2) cooling to 80 ℃, and adding isocyanate under the condition of high-speed stirring; keeping the temperature at 85 ℃ for reacting for 40 minutes, slowly heating to 110 ℃, and heating for 40 minutes; vacuumizing for 30 minutes, adding a catalyst, dispersing for 10 minutes, adding a coupling agent, dispersing for 5 minutes, and discharging to obtain the catalyst.
Example 5: the embodiment provides a reactive polyurethane hot melt adhesive, which comprises the following raw materials in parts by weight:
Figure BDA0003192010110000091
the weight-average molecular weight of the tackifying resin B is 34000, the hydroxyl value is 3.2mg KOH/g, and a product of Brilliant chemical industry with the brand number of BM19 is adopted; the isocyanate is MDI; the polyol is crystalline polyester polyol, the hydroxyl value is 27-34 mgKOH/g, the molecular weight is 3500g/mol, and the grade of Yingchuangdegai is Dynacoll 7360; the polyether polyol is 2110TB of Dow chemical; the catalyst is dibutyltin dilaurate; the coupling agent is 3-isocyanate propyl trimethoxy silane, and a T-03 product of a Huaian macro pattern new material is adopted; the antioxidant is antioxidant 1010.
The preparation method of the reactive polyurethane hot melt adhesive comprises the following steps:
(1) putting the polyol, the tackifying resin A, the tackifying resin B, the antioxidant and the like into a reaction kettle, and dissolving and stirring for 1.5 hours at 150 ℃; cooling to 120 ℃, starting to vacuumize, and dehydrating for 1.5 hours under the condition that the vacuum degree is less than or equal to 0.1 MPa;
(2) cooling to 80 ℃, and adding isocyanate under the condition of high-speed stirring; keeping the temperature at 85 ℃ for reacting for 40 minutes, slowly heating to 110 ℃, and heating for 40 minutes; vacuumizing for 30 minutes, adding a catalyst, dispersing for 10 minutes, adding a coupling agent, dispersing for 5 minutes, and discharging to obtain the catalyst.
Example 6: the embodiment provides a reactive polyurethane hot melt adhesive, which comprises the following raw materials in parts by weight:
Figure BDA0003192010110000092
Figure BDA0003192010110000101
the weight-average molecular weight of the tackifying resin A is 45000, the glass transition temperature is 50 ℃, and a product with the Japanese mitsubishi brand BR113 is adopted; the weight-average molecular weight of the tackifying resin B is 34000, the hydroxyl value is 3.2mg KOH/g, and a product of Brilliant chemical industry with the brand number of BM19 is adopted; the isocyanate is MDI; the polyester polyol is polyether polyol, namely polytetrahydrofuran polyol, the functionality is 2, and the number average molecular weight is 2000; the polyether polyol is 2110TB of Dow chemical; the catalyst is dibutyltin dilaurate; the coupling agent is 3-isocyanate propyl trimethoxy silane and adopts a T-03 product of a Huai' an macrograph new material; the antioxidant is antioxidant 1010.
The preparation method of the reactive polyurethane hot melt adhesive comprises the following steps:
(1) putting the polyol, the tackifying resin A, the tackifying resin B, the antioxidant and the like into a reaction kettle, and dissolving and stirring for 1.5 hours at 150 ℃; cooling to 120 ℃, starting to vacuumize, and dehydrating for 1.5 hours under the condition that the vacuum degree is less than or equal to 0.1 MPa;
(2) cooling to 80 ℃, and adding isocyanate under the condition of high-speed stirring; keeping the temperature at 85 ℃ for reacting for 40 minutes, slowly heating to 110 ℃, and heating for 40 minutes; vacuumizing for 30 minutes, adding a catalyst, dispersing for 10 minutes, adding a coupling agent, dispersing for 5 minutes, and discharging to obtain the catalyst.
Example 7: the embodiment provides a reactive polyurethane hot melt adhesive, which comprises the following raw materials in parts by weight:
Figure BDA0003192010110000102
Figure BDA0003192010110000111
the weight-average molecular weight of the tackifying resin A is 45000, the glass transition temperature is 50 ℃, and a product with the Japanese mitsubishi brand BR113 is adopted; the weight average molecular weight of the tackifying resin B is 34000, the hydroxyl value is 3.2mg KOH/g, and a product with the trademark of BM19 of Brillier chemical industry is adopted; the isocyanate is MDI; the polyester polyol is crystalline polyester polyol, the hydroxyl value is 27-34 mgKOH/g, the molecular weight is 3500g/mol, and the grade of Yingchuangdegai is Dynacoll 7360; the polyether polyol is 2110TB of Dow chemical; the catalyst is dibutyltin dilaurate; the antioxidant is antioxidant 1010.
The preparation method of the reactive polyurethane hot melt adhesive comprises the following steps:
(1) putting the polyol, the tackifying resin A, the tackifying resin B, the antioxidant and the like into a reaction kettle, and dissolving and stirring for 1.5 hours at 150 ℃; cooling to 120 ℃, starting to vacuumize, and dehydrating for 1.5 hours under the condition that the vacuum degree is less than or equal to 0.1 MPa;
(2) cooling to 80 ℃, and adding isocyanate under the condition of high-speed stirring; keeping the temperature at 85 ℃ for reacting for 40 minutes, slowly heating to 110 ℃, and heating for 40 minutes; vacuumizing for 30 minutes, adding a catalyst, dispersing for 10 minutes, adding a coupling agent, dispersing for 5 minutes, and discharging to obtain the catalyst.
Example 8: the embodiment provides a reactive polyurethane hot melt adhesive, which comprises the following raw materials in parts by weight:
Figure BDA0003192010110000112
the weight-average molecular weight of the tackifying resin A is 45000, the glass transition temperature is 50 ℃, and a product with the Japanese mitsubishi brand BR113 is adopted; the weight-average molecular weight of the tackifying resin B is 34000, the hydroxyl value is 3.2mg KOH/g, and a product of Brilliant chemical industry with the brand number of BM19 is adopted; the isocyanate is MDI; the polyester polyol is crystalline polyester polyol, the hydroxyl value is 27-34 mgKOH/g, the molecular weight is 3500g/mol, and the grade of Yingchuangdegai is Dynacoll 7360; the polyether polyol is 2110TB of Dow chemical; the catalyst is dibutyltin dilaurate; the coupling agent is a silane coupling agent KH-560; the antioxidant is antioxidant 1010.
The preparation method of the reactive polyurethane hot melt adhesive comprises the following steps:
(1) putting the polyol, the tackifying resin A, the tackifying resin B, the antioxidant and the like into a reaction kettle, and dissolving and stirring for 1.5 hours at 150 ℃; cooling to 120 ℃, starting to vacuumize, and dehydrating for 1.5 hours under the condition that the vacuum degree is less than or equal to 0.1 MPa;
(2) cooling to 80 ℃, and adding isocyanate under the condition of high-speed stirring; keeping the temperature at 85 ℃ for reacting for 40 minutes, slowly heating to 110 ℃, and heating for 40 minutes; vacuumizing for 30 minutes, adding a catalyst, dispersing for 10 minutes, adding a coupling agent, dispersing for 5 minutes, and discharging to obtain the catalyst.
Performance testing
The applicant found that the samples of examples 1 to 3, in which a 5mm thick fire-retardant coating was adhered to a conventional calcium silicate board, had high initial strength and no rebound occurred even when the thickness of the fire-retardant coating was 5mm or more, and the sample of example 3 was most effective. In addition, the open time of the samples can reach 5-8 minutes, wherein the open time of the samples in the embodiment 3 can reach 8 minutes on average, the open time of the samples in the embodiments 1 and 2 is about 6 minutes respectively, however, the open time of the other samples is different, the open time of the samples in the embodiment 6 is shortest and is only 2 minutes, the open time of the samples in the embodiment 7 is 4 minutes, and the operational time of workers is very short, so that the normal use of the samples is seriously influenced. In addition, the applicant attaches the above sample to a PVC plate and performs a peeling test, and finds that the sample in example 3 can be made to pull apart the PVC substrate, the samples in examples 7 and 8 are adhesive layer fracture, and the rest of the samples are fractured at the interface between the adhesive layer and the PVC substrate.
Further, the applicant classified the samples in the above examples according to specific experimental groups and performed the blister performance test. Specifically, the method comprises the following steps: the method comprises the steps of gluing the same base material layer of a sample in each experimental group, curing the same base material layer under the same condition, respectively placing the samples in water at 60 ℃ for 4 hours and water at normal temperature (25 ℃) for 48 hours, then observing whether the samples in each experimental group have the problems of glue failure or air bubbles and the like, and classifying the samples into 1-3 grades according to the severity of the phenomena, wherein the 1 grade is that the problems of glue failure or air bubbles and the like do not occur, the 3 grade is that obvious problems of glue failure and air bubbles and the like occur, and the 2 grade is between the 1 grade and the 3 grade and has the problems of slight glue failure and/or air bubbles and the like. The specific experimental groups are as follows:
experimental group 1 corresponds to the sample of example 3;
experimental group 2 corresponds to the sample of example 4;
experimental group 3 corresponds to the sample of example 5;
experimental group 4 corresponds to the sample of example 6;
experimental group 5 corresponds to the sample of example 7;
experimental group 6 corresponds to the sample of example 8.
The specific performance test results are shown in table 1 below.
Normal temperature water bubble 60 ℃ water bubble
Experimental group 1 Level 1 Level 1
Experimental group 2 Level 1 Stage 2
Experimental group 3 Stage 2 Stage 2
Experimental group 4 Stage 2 Grade 3
Experimental group 5 Stage 2 Stage 2
Experimental group 6 Level 1 Stage 2
Operations and steps disclosed in embodiments of the invention may be directed to specific aspects of the invention and other steps may be performed in accordance with operations well known to those skilled in the art.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; without conflict, embodiments of the present disclosure and features of the embodiments may be combined with each other to arrive at new embodiments. Various modifications, adaptations, and equivalents may occur to those skilled in the art without departing from the scope and spirit of the present invention.

Claims (10)

1. The reactive polyurethane hot melt adhesive is characterized by comprising the following raw materials in parts by weight:
Figure FDA0003192010100000011
the tackifying resin A and the tackifying resin B are resins obtained by polymerizing acrylate derivatives serving as monomers.
2. The reactive polyurethane hot melt adhesive of claim 1, wherein the acrylate derivative is selected from one or more of methyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, and hydroxyethyl methacrylate.
3. The reactive polyurethane hot melt adhesive according to claim 2, wherein the hydroxyl value of the tackifying resin B is 1-5 mg KOH/g.
4. The reactive polyurethane hot melt adhesive as claimed in claim 2, wherein the weight average molecular weight of the tackifying resin A is 30000-70000.
5. The reactive polyurethane hot melt adhesive of claim 4, wherein the glass transition temperature of the tackifying resin A is not lower than 30 ℃.
6. The reactive polyurethane hot melt adhesive according to any one of claims 1 to 5, wherein the polyester polyol is prepared from dibasic acid and diol; the dibasic acid is selected from one or more of adipic acid, sebacic acid, suberic acid, dodecanedioic acid and tetradecanedioic acid; the dihydric alcohol is selected from one or more of 1, 2-ethanediol, 1, 4-butanediol, 1, 6-hexanediol, 1, 8-octanediol, 1, 10-decanediol, 1, 12-dodecanediol, diethylene glycol and neopentyl glycol.
7. The reactive polyurethane hot melt adhesive of claim 6, wherein the polyester polyol is a crystalline polyester polyol.
8. The reactive polyurethane hot melt adhesive according to claim 1, wherein the coupling agent is an isocyanatosilane coupling agent.
9. The preparation method of the reactive polyurethane hot melt adhesive according to any one of claims 1 to 8, characterized by comprising the following steps:
(1) putting the polyol, the tackifying resin A, the tackifying resin B and the antioxidant into a reaction kettle according to a ratio, dissolving and stirring for 1-3 hours at 140-160 ℃, then cooling to 120 ℃, and vacuumizing and drying for 1-3 hours;
(2) cooling the system to 70-85 ℃, adding isocyanate while stirring, reacting for 0.5-1.5 hours at 80-90 ℃, then heating to 110 ℃, vacuumizing for 30 minutes, adding a catalyst, dispersing for 5-15 minutes, adding a coupling agent, dispersing and discharging to obtain the catalyst.
10. The application of the reactive polyurethane hot melt adhesive according to any one of claims 1 to 8 is characterized by being applied to the field of fabricated buildings.
CN202110880365.8A 2021-08-02 2021-08-02 Reactive polyurethane hot melt adhesive for fabricated building and preparation method thereof Pending CN114736642A (en)

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