CN112980386B - Polyurethane moisture-curing hot melt adhesive and preparation method and application thereof - Google Patents

Polyurethane moisture-curing hot melt adhesive and preparation method and application thereof Download PDF

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CN112980386B
CN112980386B CN202110164142.1A CN202110164142A CN112980386B CN 112980386 B CN112980386 B CN 112980386B CN 202110164142 A CN202110164142 A CN 202110164142A CN 112980386 B CN112980386 B CN 112980386B
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hot melt
melt adhesive
curing hot
polyurethane moisture
reaction
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CN112980386A (en
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何万萍
明俊江
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Valence Bonding Technology (shanghai) Co ltd
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Valence Bonding Technology (shanghai) 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
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B21/00—Layered products comprising a layer of wood, e.g. wood board, veneer, wood particle board
    • B32B21/02—Layered products comprising a layer of wood, e.g. wood board, veneer, wood particle board the layer being formed of fibres, chips, or particles, e.g. MDF, HDF, OSB, chipboard, particle board, hardboard
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B21/00—Layered products comprising a layer of wood, e.g. wood board, veneer, wood particle board
    • B32B21/04—Layered products comprising a layer of wood, e.g. wood board, veneer, wood particle board comprising wood as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B21/08—Layered products comprising a layer of wood, e.g. wood board, veneer, wood particle board comprising wood as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B32B37/1207—Heat-activated adhesive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B32B37/1207—Heat-activated adhesive
    • B32B2037/1215—Hot-melt adhesive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B32B2037/1253—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives curable adhesive
    • B32B2037/1261—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives curable adhesive moisture curable
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/554—Wear resistance
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/73—Hydrophobic
    • 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 application relates to the field of adhesive industry, and particularly discloses a polyurethane moisture-curing hot melt adhesive as well as a preparation method and application thereof. The preparation method comprises the steps of firstly melting polyester polyol, then sequentially putting the melted polyester polyol, polyether polyol and stabilizer into a reaction container, adding tackifying resin after uniformly mixing, carrying out vacuum concentration, then adding isocyanate and catalyst for reaction, then adding chain extender for reaction, stopping the reaction when the content of-NCO groups in the obtained reaction liquid accounts for 2-5wt% of the reaction liquid and the viscosity is 15000-30000cps, and obtaining the reaction liquid, namely the polyurethane moisture curing hot melt adhesive. The polyurethane moisture-curing hot melt adhesive is applied to furniture plates with PETG films, and the peel strength of the polyurethane moisture-curing hot melt adhesive can reach 2.45-3N/mm.

Description

Polyurethane moisture-curing hot melt adhesive as well as preparation method and application thereof
Technical Field
The application relates to the field of adhesives, in particular to a polyurethane moisture-curing hot melt adhesive, a preparation method and application thereof in a furniture board with a veneered PETG film.
Background
The PVC film is generally used as a veneering material in the furniture industry, but a large amount of plasticizer is added in the production process of the PVC film to ensure the softness and plasticity of the film, the plasticizer in the film can be slowly separated out along with the temperature and the pressure, and the health can be harmed when the plasticizer contacts with a human body, so that the furniture industry seeks safer veneering film materials at present, and PETG is one of the materials.
The PETG membrane material is used as a novel membrane material for the furniture industry, and no relevant report exists in the relevant technology.
Disclosure of Invention
In order to solve the technical problem of application of PETG membrane materials in the furniture industry, the application provides a polyurethane moisture-curing hot melt adhesive, a preparation method and application thereof in veneering PETG membrane furniture boards.
In a first aspect, the application provides a polyurethane moisture-curing hot melt adhesive, which adopts the following technical scheme:
the polyurethane moisture-curing hot melt adhesive comprises the following raw material components in percentage by weight:
Figure BDA0002936921730000011
the polyester polyol is polymerized by one or more than two of adipic acid, sebacic acid, dodecanedioic acid, terephthalic acid, isophthalic acid or phthalic acid and one or more than two of hexanediol, butanediol, diethylene glycol or neopentyl alcohol, and the weight-average molecular weight is 1000-5000;
the polyether polyol has the weight-average molecular weight of 400-2000, and is polyoxypropylene glycol or polytetrahydrofuran ether glycol; the tackifying resin is one or two of acrylic resin, terpene resin and petroleum resin;
the chain extender 1, 4-butanediol, trimethylolpropane (hereinafter referred to as TMP) or a mixture of 1, 4-butanediol and TMP;
the stabilizer is hindered phenol antioxidant which is 1010, 1076 or 168 produced by Basff;
the catalyst is at least one of dimorpholinodiethylether (hereinafter referred to as DMDEE), N-dimethylcyclohexylamine and triethylamine.
By adopting the technical scheme, the polyurethane moisture-curing hot melt adhesive contains polyether polyol, has the characteristics of liquid state at normal temperature and good fluidity, and has the characteristics of softness, elasticity and no brittleness at low temperature after the polyurethane moisture-curing hot melt adhesive is synthesized.
Furthermore, the components of the raw materials in the polyurethane moisture-curing hot melt adhesive have good compatibility, so that the obtained polyurethane moisture-curing hot melt adhesive is transparent.
Furthermore, because the raw materials contain components which are liquid at normal temperature, the finally obtained polyurethane moisture curing hot melt adhesive has low viscosity and better fluidity, and the viscosity is 15000-30000cps when detected at 120 ℃.
Furthermore, the polyurethane moisture curing hot melt adhesive contains crystalline polyester polyol, and has the characteristics of good initial adhesion and high cohesive force, so that the finally obtained polyurethane moisture curing hot melt adhesive has the characteristic of high adhesive strength.
Preferably, the polyurethane moisture-curing hot melt adhesive is prepared from the following raw material components in percentage by weight:
Figure BDA0002936921730000021
the polyester polyol is XCP3000B, XCP3000H or XCP-44 with the weight-average molecular weight of 1000-5000 produced by Asahi Chuan chemical company, or Dynacoll7360, dynacoll7380 or Dynacoll7361 with the weight-average molecular weight of 1000-5000 produced by Asahi Chuan chemical company, or POL-S3500 or POL-328 with the weight-average molecular weight of 1000-5000 produced by Yutian chemical company;
the polyoxypropylene diol is DL-400, DL-1000 or DL-2000 produced by Toddard chemical, or VONOL-2110TB or VONOL-1000LM produced by the Dow company; the polytetrahydrofuran ether glycol is PolyTHF1000 or PolyTHF2000 produced by basf company, or PTMG650 or PTNG1000 produced by Mitsubishi company;
the acrylic resin is BR-106, BR-113, AC1630, AC1520, AC-1631 or AC-1750 produced by Mitsubishi chemical company, or Lucite 2013, lucite 2016, lucite 2044 or Lucite4026 produced by Lucite chemical company;
the terpene resin is SYLVARES TP96, SYLVARES TP300, SYLVARES TP115P or SYLVARES TP2019 produced by Arizona chemical company;
the petroleum resin is NOVARES TN100, NOVARES TK100, NOVARES TN120 or NOVARES TN150 produced by Luger chemical company.
By adopting the preferable technical scheme, the finally obtained polyurethane moisture-curing hot melt adhesive has better fluidity and higher initial adhesion and final bonding strength, is used for manufacturing furniture boards with PETG films, and the finally obtained furniture boards with PETG films have the peel strength of 2.45-3N/mm.
In a second aspect, the present application provides a method for preparing a polyurethane moisture-curable hot melt adhesive, which adopts the following technical scheme, and specifically comprises the following steps:
(1) Firstly, adding polyester polyol into a reaction container, and controlling the temperature to be 110-120 ℃ for melting to obtain molten polyester polyol;
(2) Sequentially adding polyether polyol and a stabilizer into molten polyester polyol, controlling the temperature to be 110-130 ℃, stirring and mixing uniformly, adding tackifying resin while stirring, and continuously stirring and mixing uniformly after the tackifying resin is completely added to obtain a mixture;
(3) Then controlling the pressure of the mixture obtained in the step (2) to be minus 0.09MPa plus or minus 0.01, maintaining the temperature at 110-130 ℃ for 50-70min to remove water vapor generated by storing the raw materials, then cooling to 80-100 ℃, adding isocyanate and a catalyst while stirring, and after the addition is finished, carrying out aldol condensation reaction at 90-110 ℃ under the condition of stirring and controlling the pressure to be minus 0.09MPa plus or minus 0.01 to obtain a reaction solution 1;
(4) Adding a chain extender into the reaction solution 1 obtained in the step (3), and then continuously reacting under the stirring condition at the pressure of minus 0.09MPa +/-0.01 and the temperature of 90-110 ℃ to obtain a reaction solution 2;
and (3) sampling to test the-NCO group content and viscosity in the reaction process, stopping the reaction when the-NCO group content in the reaction liquid 2 accounts for 2-5% of the weight of the reaction liquid 2 and the viscosity at 120 ℃ is 15000-30000cps, and obtaining the reaction liquid 2 which is the polyurethane moisture-curing hot melt adhesive.
By adopting the technical scheme and the preparation method of the polyurethane moisture-curing hot melt adhesive, the whole process is in vacuum, and the reaction temperature and time are accurately controlled in the preparation process, so that the finally obtained polyurethane moisture-curing hot melt adhesive has the technical effects of no water vapor and good batch stability of products.
Preferably, in the step (2) of the above preparation process, the addition rate of the tackifier resin is controlled to be 80 to 120g/min.
By adopting the technical scheme, the addition rate of the tackifying resin is controlled in the step (2) of the preparation process, so that hot liquid can be prevented from splashing due to the fact that the addition rate of the tackifying resin is too high, and the addition rate is controlled to ensure that the added tackifying resin is melted as soon as possible, so that the safety and the controllability of the preparation process and the smooth operation of the next step of the process are ensured.
In a third aspect, the present application provides a composite furniture board with a PETG film, which adopts the following technical scheme:
a composite furniture board with a PETG film is of a layered structure and comprises a base layer board, an adhesive layer and a PETG film layer from bottom to top in sequence;
the adhesive layer is obtained by curing the polyurethane moisture-curing hot melt adhesive coated on the base layer plate between the base layer plate and the PETG film layer for 3-7 days after roller pressing treatment;
the thickness of the PETG film layer is 0.01-0.1cm;
the base layer board is a plywood or a medium density fiberboard.
By adopting the technical scheme, the air and water vapor among the base layer board and the PETG film layer are subjected to chemical reaction with the-NCO group in the polyurethane moisture-curing hot melt adhesive to generate polyurea groups for bonding connection, namely the PETG film layer and the base layer board are firmly bonded and adhered together through the polyurethane moisture-curing hot melt adhesive, so that the finally obtained composite furniture board with the PETG film has the characteristic of good peel strength. Furthermore, the polyurethane moisture-curing hot melt adhesive is transparent, so that the characteristic of transparency of the PETG membrane material after adhesion is not influenced. Furthermore, because the PETG film is adopted for veneering, the obtained composite furniture board with the PETG film has good water resistance and wear resistance.
In a fourth aspect, the present application provides a method for preparing the composite furniture board with the PETG film, which specifically includes the following steps:
(1) Pre-treating a base layer plate, and removing surface dust;
(2) Coating polyurethane moisture-curing hot melt adhesive on the pretreated base layer plate at the temperature of 120 ℃;
(3) And then covering a PETG film on the coated polyurethane moisture-curing hot melt adhesive, then carrying out roller pressing treatment, controlling the pressure to be 0.3-0.5MPa in the roller pressing process, carrying out pressing for 0.05-0.1min, standing and curing for 3-7 days after pressing, and finally obtaining the composite furniture board with the PETG film.
By adopting the technical scheme, the composite furniture board with the PETG film is obtained by simple coating, rolling and curing in the preparation process, so that the preparation method is simple, convenient to operate and convenient for industrial production.
Preferably, in the step (2), the thickness of the polyurethane moisture-curing hot melt adhesive coated on the substrate sheet material is 30-70g/m 2 。
By adopting the technical scheme, the finally obtained composite furniture board with the PETG film has better peel strength which can reach 2.45-3N/mm.
In summary, the present application has the following beneficial effects:
the polyurethane moisture-curing hot melt adhesive is transparent and low in viscosity, so that the polyurethane moisture-curing hot melt adhesive has good fluidity, has the viscosity of 15000-30000cps at 120 ℃, and has the characteristics of softness, elasticity and no brittleness at low temperature.
Furthermore, the polyurethane moisture curing hot melt adhesive has the advantages that the whole process is in vacuum, and the reaction temperature and time are accurately controlled in the preparation process, so that the product does not contain water vapor, and the batch stability of the product is good.
Furthermore, the composite furniture board with the PETG film, which is prepared by utilizing the polyurethane moisture-curing hot melt adhesive, has good peel strength, and the peel strength is 2.45-3N/mm when tested according to GB/T2790-1995 standard. Meanwhile, the polyurethane moisture-curing hot melt adhesive is transparent, so that the characteristic of transparency of the PETG membrane material after adhesion is not influenced.
Furthermore, the composite furniture board with the PETG film has good water resistance and wear resistance due to the adoption of the PETG film adhesive surface, and meanwhile, the polyurethane moisture-curing hot melt adhesive used for the adhesive layer in the composite furniture board with the PETG film also has good water resistance due to the selection of water-resistant raw materials, and the water resistance are synergistic, so that the obtained composite furniture board with the PETG film cannot be separated from the base layer board when the composite furniture board with the PETG film meets water.
Furthermore, the preparation method of the composite furniture board with the PETG membrane has the advantages of simple preparation process, convenience in operation and convenience in industrial production.
Detailed Description
The present application will be described in further detail with reference to examples.
The starting materials used in the examples of the present application are commercially available, except for the following special descriptions:
Figure BDA0002936921730000051
Figure BDA0002936921730000061
in the embodiments of the present application:
measurement of the viscosity and-NCO group content of the polyurethane moisture-curing hotmelt, i.e.reaction liquid 2 in the examples of the present application:
method for determining the viscosity in polyurethane moisture-curing hotmelt adhesives, using a Brookfield DV-II viscometer, the viscosity being the intermolecular production of a liquid while it is flowingThe viscosity property of the internal friction is expressed by viscosity, and is used for characterizing a resistance factor related to the liquid property. Has a unit of Pa.s and is characterized in that the area of the two blocks is 1m 2 The plate of (2) is immersed in a liquid at a distance of 1m, and if a shear stress of 1N is applied to give a relative velocity of 1 m/sec between the two plates, the viscosity of the liquid is 1Pa · s,1Pa · s =1000mPa · s =1000cps, and the test method comprises the steps of:
(1) Sample preparation: directly using a specified container (sample tube) to contain the polyurethane moisture curing hot melt adhesive to be detected, wherein the polyurethane moisture curing hot melt adhesive is uniform and has no bubbles, and the amount of the polyurethane moisture curing hot melt adhesive is 2/3;
(2) The method comprises the following operation steps:
the same sample I should select the same rotor and rotation speed, the reading is in the range of 20% -80% of the dial;
II, placing the container containing the sample into a heating sleeve, balancing the temperature of the sample with the test temperature, and keeping the temperature of the sample uniform;
III, vertically immersing the rotor into the central part of the polyurethane moisture-curing hot melt adhesive to be measured, and enabling the liquid level to reach a rotor liquid level marking (a protective frame should be arranged);
IV, starting the rotational viscometer to read the reading when the pointer is unchanged on the disk during rotation;
v Each sample was measured three times and the average value was taken.
Detecting the content of-NCO groups in the polyurethane moisture curing hot melt adhesive, namely producing urea by using isocyanate based on excessive di-n-butylamine reaction, and then titrating the excessive di-n-butylamine by hydrochloric acid to quantitatively calculate the content of the isocyanate, wherein the specific test method comprises the following steps:
(1) Weighing 3.5-6.5 g of polyurethane moisture curing hot melt adhesive to be detected, putting the polyurethane moisture curing hot melt adhesive into a dried flask, adding 25mL of anhydrous toluene, covering the flask with a bottle cap, and shaking to completely dissolve a sample;
(2) 20mL of a di-n-butylamine solution (338 mL of di-n-butylamine diluted with dry toluene to 1000mL in a volumetric flask) was added by pipette;
(3) Adding 100mL of anhydrous isopropanol;
(4) 0.5mL of bromophenol blue solution is used as an indicator (0.1 g of bromophenol blue is taken, 1.5mL of 1N NaOH solution is added, and the solution is diluted to 1000mL by distilled water), 1.0N hydrochloric acid solution is used for titration until the yellow end point, and the volume of the consumed 1.0N hydrochloric acid solution is V1 (mL);
(5) Adding 25mL of toluene as a reference without adding a polyurethane hot melt adhesive in the step (1), performing a blank test, repeating the steps (2) - (4), and finally, taking the volume of the 1.0N hydrochloric acid solution consumed in the step (4) as V0 (mL);
the calculation formula of the content of the-NCO group in the polyurethane moisture-curing hot melt adhesive is as follows:
the content of-NCO groups in the polyurethane moisture-curing hot melt adhesive (%) = (V0-V1)/the weight of the polyurethane moisture-curing hot melt adhesive to be tested multiplied by 4.2.
Testing the bonding strength of the polyurethane moisture-curing hot melt adhesive:
according to the GB/T2790-2015 method, the 180-degree peeling test is carried out on the peel strength of the composite furniture board with the PETG film under the test conditions of 23 +/-2 ℃ and 300mm/min, the adopted equipment for the measurement is a tensile testing machine which is CMT-2103, and the manufacturer is Miss Taijie electric equipment Co.
Example 1
The polyurethane moisture-curing hot melt adhesive comprises the following raw material components in percentage by weight:
Figure BDA0002936921730000081
the polyester polyol is produced by Asahi Chun chemical company, and the label is XCP3000B;
the polyether polyol is polyoxypropylene diol which is produced by great eastern chemicals and is marked by DL-1000D;
the tackifying resin is acrylic resin, wherein the acrylic resin is produced by Mitsubishi chemical company and is marked by BR-113;
the chain extender is 1, 4-butanediol;
the stabilizer is a hindered phenol antioxidant produced by basf and the number of the hindered phenol antioxidant is 1010;
the catalyst is dimorpholinyl diethyl ether.
The preparation method of the polyurethane moisture-curing hot melt adhesive comprises the following specific steps:
(1) Firstly, adding polyester polyol into a reaction container, and controlling the temperature to be 110-120 ℃ for melting to obtain molten polyester polyol;
(2) Sequentially adding polyether polyol and a stabilizer into the molten polyester polyol obtained in the step (1), controlling the temperature to be 120 ℃ and the rotating speed to be 90-110r/min, stirring and mixing for 10min, adding tackifying resin while stirring, wherein the adding speed of the tackifying resin is 100g/min, after the tackifying resin is completely added, increasing the stirring rotating speed to be 150r/min, stirring for 30min, and uniformly mixing to obtain a mixture;
(3) Then controlling the pressure of the mixture obtained in the step (2) to be minus 0.09MPa +/-0.01, maintaining the temperature at 120 ℃ for 60min, then cooling to 80-100 ℃, breaking vacuum, controlling the rotating speed at normal pressure to be 100r/min, adding isocyanate and a catalyst while stirring, and after the addition is finished, controlling the stirring rotating speed to be 150r/min, the pressure to be minus 0.09MPa +/-0.01, and the temperature to be 100 ℃ to react for 60min to obtain a reaction solution 1;
(4) Breaking vacuum of the reaction liquid 1 obtained in the step (3), adding a chain extender under normal pressure, controlling the stirring speed to be 150r/min, the pressure to be minus 0.09MPa +/-0.01 and the temperature to be 100 ℃ for reaction to obtain a reaction liquid 2, and sampling and testing the NCO group content and the viscosity of the reaction liquid 2 in the reaction process;
and when the content of the-NCO group in the reaction liquid 2 accounts for 5 percent of the weight of the reaction liquid 2 and the viscosity is 15000-30000cps at 120 ℃, stopping the reaction, and obtaining the reaction liquid 2, namely the polyurethane moisture-curing hot melt adhesive.
Application example 1
The preparation method of the polyurethane moisture-curing hot melt adhesive used for the composite furniture board with the PETG film, which is obtained in the embodiment 1, comprises the following steps:
(1) Taking a base layer plate, and removing surface dust;
the base layer board is a medium-density fiberboard with the thickness of about 1cm;
(2) Coating polyurethane moisture-curing hot melt adhesive on the pretreated base layer plate at the temperature of 120 ℃, wherein the coating thickness is 70g/m 2 ；
(3) Covering a PETG film on the coated polyurethane moisture-curing hot melt adhesive, then performing roller pressing treatment, controlling the pressure to be 0.5MPa in the pressing process, performing pressing for 0.05min, standing and curing for 5 days after pressing, and finally respectively obtaining a composite furniture board A1 with the PETG film;
the thickness of the PETG film is 0.1cm.
The obtained composite furniture board A1 with the PETG film is of a layered structure and sequentially comprises a base layer board, an adhesive layer and a PETG film layer from bottom to top;
the adhesive layer is arranged between the base layer plate and the PETG film layer, coated on the base layer plate and coated with the adhesive layer with the thickness of 70g/m 2 The polyurethane moisture-curing hot melt adhesive is subjected to roller pressing treatment, the pressure is controlled to be 0.5MPa in the pressing process, pressing is carried out for 0.05min, standing and curing are carried out for 5 days after pressing, and the composite furniture board A1 with the PETG film is obtained;
the thickness of the PETG film layer is 0.1cm;
the base layer board is a medium-density fiberboard with the thickness of about 1cm.
Application example 2
The preparation method of the polyurethane moisture-curing hot melt adhesive obtained in the embodiment 1 is respectively used for preparing composite furniture boards with PETG films, and specifically comprises the following steps:
(1) Taking a base layer plate, and removing surface dust;
the base layer board is a medium-density fiberboard with the thickness of about 1cm;
(2) Coating polyurethane moisture-curing hot melt adhesive on the pretreated base layer plate at the temperature of 120 ℃, wherein the coating thickness is 30g/m 2 ；
(3) Covering a PETG film on the coated polyurethane moisture-curing hot melt adhesive, then performing roller press-fitting treatment, controlling the pressure to be 0.5MPa in the press-fitting process, performing press-fitting for 0.05min, standing and maintaining for 5 days after press-fitting, and finally respectively obtaining a composite furniture board A2 with the PETG film;
the thickness of the PETG film is 0.01cm.
The obtained composite furniture board A1 with the PETG film is of a layered structure and sequentially comprises a base layer board, an adhesive layer and a PETG film layer from bottom to top;
the adhesive layer is arranged between the base layer plate and the PETG film layer, coated on the base layer plate and coated with the adhesive layer with the thickness of 30g/m 2 The polyurethane moisture-curing hot melt adhesive is subjected to roller pressing treatment, the pressure is controlled to be 0.5MPa in the pressing process, pressing is carried out for 0.05min, and standing and curing are carried out for 5 days after pressing to obtain a composite furniture board A1 with a PETG membrane;
the thickness of the PETG film layer is 0.01cm;
the base layer board is a medium-density fiberboard with the thickness of about 1cm;
the peel strength of the composite furniture board A1 and A2 with PETG film is 2.5N/mm and 2.45N/mm respectively. The results show that the polyurethane moisture-curing hot melt adhesive disclosed by the invention is good in adhesive force and high in peel strength when used for bonding a PETG film and a base layer plate. The reason for analyzing the polyurethane moisture-curing hot melt adhesive is that-NCO groups in isocyanate components contained in the polyurethane moisture-curing hot melt adhesive chemically react with air and water vapor in the PETG film and between base layer plates to generate polyurea groups to generate bonding connection, so that the bonding strength between the PETG film and the base layer plates is synergistically enhanced.
Furthermore, through the comparison of the peel strength of the composite furniture board A1 and A2 with the PETG film, it can be seen that the polyurethane moisture-curing hot melt adhesive has good adhesive force to the PETG film and the base layer board, and the coating thickness is only 30g/m 2 (ii) a The peel strength can reach 2.45N/mm.
Example 2
The polyurethane moisture-curing hot melt adhesive comprises the following raw material components in percentage by weight:
Figure BDA0002936921730000101
the polyester polyol is produced by Asahi Sichuan chemical company, and is marked as XCP-44;
the polyether glycol is polytetrahydrofuran ether glycol which is produced by Toddard chemical industry and is marked with DL-2000D;
the tackifying resin is terpene resin, and the terpene resin is produced by Arizona chemical company and is marked as SYLVARES TP96;
the chain extender is TMP;
the stabilizer is a hindered phenol antioxidant produced by Basff, and the number of the hindered phenol antioxidant is 1076;
the catalyst is N, N-dimethyl cyclohexylamine.
The preparation method of the polyurethane moisture-curing hot melt adhesive comprises the following specific steps:
(1) The same procedure as in step (1) of the preparation method of the polyurethane moisture-curable hot melt adhesive of example 1;
(2) The same as the step (2) of the preparation method of the polyurethane moisture-curing hot melt adhesive in the embodiment 1, so as to obtain a mixture;
(3) The same as the step (3) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the example 1, a reaction solution 1 is obtained;
(4) Obtaining a reaction liquid 2 in the same step (4) of the preparation method of the polyurethane moisture-curing hot melt adhesive in the embodiment 1, and sampling and testing the content of-NCO groups and the viscosity of the reaction liquid 2 in the reaction process;
when the content of-NCO group in the reaction liquid 2 accounts for 2 percent of the weight of the reaction liquid 2 and the viscosity is 15000-30000cps at 120 ℃, the reaction is stopped, and the reaction liquid 2 is the polyurethane moisture curing hot melt adhesive.
Example 3
The polyurethane moisture-curing hot melt adhesive comprises the following raw material components in percentage by weight:
Figure BDA0002936921730000111
the polyester polyol is produced by Yingchuang chemical company and is marked by Dynacoll 7360;
the polyether polyol is polytetrahydrofuran ether glycol which is produced by basf company and is marked as PolyTHF1000;
the tackifying resin is petroleum resin which is produced by Lwight chemical company and is marked by NOVARES TN100;
the chain extender is a mixture of 1, 4-butanediol and TMP according to a mass ratio of 1;
the stabilizer is a hindered phenol antioxidant produced by BASF, and the number of the hindered phenol antioxidant is 168;
the catalyst is triethylamine.
The preparation method of the polyurethane moisture-curing hot melt adhesive comprises the following specific steps:
(1) The same procedure as in step (1) of the preparation method of the polyurethane moisture-curable hot melt adhesive of example 1;
(2) The same as the step (2) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the embodiment 1, so as to obtain a mixture;
(3) The same as the step (3) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the example 1, a reaction solution 1 is obtained;
(4) Obtaining a reaction liquid 2 in the same step (4) of the preparation method of the polyurethane moisture-curing hot melt adhesive in the embodiment 1, and sampling and testing the content of-NCO groups and the viscosity of the reaction liquid 2 in the reaction process;
when the content of-NCO group in the reaction liquid 2 accounts for 3.5 percent of the weight of the reaction liquid 2 and the viscosity is 15000-30000cps at 120 ℃, the reaction is stopped, and the reaction liquid 2 is the polyurethane moisture curing hot melt adhesive.
Example 4
The polyurethane moisture-curing hot melt adhesive comprises the following raw material components in percentage by weight:
Figure BDA0002936921730000121
the polyester polyol is produced by Yutian chemical company, and the label is POL-S3500;
the polyether polyol is polytetrahydrofuran ether glycol, and the label is produced by BASF company, and the label is PolyTHF 2000;
the tackifying resin is petroleum resin which is produced by Luger chemical company and is marked as NOVARES TN150;
the chain extender is a mixture of 1, 4-butanediol and TMP according to a mass ratio of 1;
the stabilizer is a hindered phenol antioxidant produced by Basff, and the number of the hindered phenol antioxidant is 168;
the catalyst is triethylamine.
The preparation method of the polyurethane moisture-curing hot melt adhesive comprises the following specific steps:
(1) The preparation method of the polyurethane moisture-curing hot melt adhesive in the example 1 comprises the following steps (1);
(2) The same as the step (2) of the preparation method of the polyurethane moisture-curing hot melt adhesive in the embodiment 1, so as to obtain a mixture;
(3) The same as the step (3) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the example 1, a reaction solution 1 is obtained;
(4) The same as the step (4) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the embodiment 1, obtaining a reaction solution 2, and sampling and testing the content of-NCO groups and the viscosity of the reaction solution 2 in the reaction process;
when the content of-NCO groups in the reaction liquid 2 accounts for 4 percent of the weight of the reaction liquid 2 and the viscosity is 15000-30000cps at 120 ℃, the reaction is stopped, and the reaction liquid 2 is the polyurethane moisture curing hot melt adhesive.
Example 5
The polyurethane moisture-curing hot melt adhesive comprises the following raw material components in percentage by weight:
Figure BDA0002936921730000131
the polyester polyol is produced by Yutian chemical company and is marked as POL-328;
the polyether polyol is polyoxypropylene diol which is produced by the Dow company and is marked as VORANOL 2110TB;
the tackifying resin is composed of acrylic resin and terpene resin, wherein the acrylic resin is produced by Mitsubishi chemical company and is marked as AC1630; the terpene resin is produced by Arizona chemical company and is marked as SYLVARES TP115P;
the chain extender is 1, 4-butanediol;
the stabilizer is a hindered phenol antioxidant produced by basf and the number of the hindered phenol antioxidant is 1010;
the catalyst is N, N-dimethylcyclohexylamine and triethylamine in a mass ratio of 1:1 are mixed.
The preparation method of the polyurethane moisture-curing hot melt adhesive comprises the following specific steps:
(1) The same procedure as in step (1) of the preparation method of the polyurethane moisture-curable hot melt adhesive of example 1;
(2) The same as the step (2) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the embodiment 1, so as to obtain a mixture;
(3) The same as the step (3) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the example 1, a reaction solution 1 is obtained;
(4) The same as the step (45) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the embodiment 1, obtaining a reaction solution 2, and sampling and testing the content of-NCO groups and the viscosity of the reaction solution 2 in the reaction process;
when the content of-NCO group in the reaction liquid 2 accounts for 4 percent of the weight of the reaction liquid 2 and the viscosity is 15000-30000cps at 120 ℃, the reaction is stopped, and the reaction liquid 2 is the polyurethane moisture curing hot melt adhesive.
Example 6
The polyurethane moisture-curing hot melt adhesive comprises the following raw material components in percentage by weight:
Figure BDA0002936921730000132
Figure BDA0002936921730000141
the polyester polyol is produced by Asahi Sichuan chemical company, and the label is XCP3000H;
the polyether polyol is polytetrahydrofuran ether glycol-propylene oxide glycol, is produced by BASF corporation and is marked as PolyTHF1000;
the tackifying resin is composed of terpene resin and petroleum resin, wherein the terpene resin is produced by Arizona chemical company and is marked as SYLVARES TP300; the petroleum resin is produced by Luger chemical company and is marked as NOVARES TN120;
the chain extender is TMP;
the stabilizer is a hindered phenol antioxidant produced by Basff, and the number of the hindered phenol antioxidant is 1076;
the catalyst is DMDEE.
The preparation method of the polyurethane moisture-curing hot melt adhesive comprises the following specific steps:
(1) The preparation method of the polyurethane moisture-curing hot melt adhesive in the example 1 comprises the following steps (1);
(2) The same as the step (2) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the embodiment 1, so as to obtain a mixture;
(3) The same as the step (3) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the example 1, a reaction solution 1 is obtained;
(4) The same as the step (4) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the embodiment 1, obtaining a reaction solution 2, and sampling and testing the content of-NCO groups and the viscosity of the reaction solution 2 in the reaction process;
when the content of-NCO groups in the reaction liquid 2 accounts for 4 percent of the weight of the reaction liquid 2 and the viscosity is 15000-30000cps at 120 ℃, the reaction is stopped, and the reaction liquid 2 is the polyurethane moisture curing hot melt adhesive.
Example 7
The polyurethane moisture-curing hot melt adhesive comprises the following raw material components in percentage by weight:
Figure BDA0002936921730000142
Figure BDA0002936921730000151
the polyester polyol is produced by Yingchuang chemical company and is marked by Dynacoll7380;
the polyether polyol is polytetrahydrofuran ether glycol which is produced by basf company and is marked with polyTHF 2000;
the tackifying resin is petroleum resin, wherein the petroleum resin is produced by Luger chemical company and is marked as NOVARES TK100;
the chain extender is TMP;
the stabilizer is a hindered phenol antioxidant produced by basf and the number of the hindered phenol antioxidant is 1010;
the catalyst is prepared by mixing DMDEE and triethylamine according to the mass ratio of 1.
The preparation method of the polyurethane moisture-curing hot melt adhesive comprises the following specific steps:
(1) The same procedure as in step (1) of the preparation method of the polyurethane moisture-curable hot melt adhesive of example 1;
(2) The same as the step (2) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the embodiment 1, so as to obtain a mixture;
(3) The same as the step (3) of the preparation method of the polyurethane moisture-curing hot melt adhesive of the example 1, a reaction solution 1 is obtained;
(4) Obtaining a reaction liquid 2 in the same step (4) of the preparation method of the polyurethane moisture-curing hot melt adhesive in the embodiment 1, and sampling and testing the content of-NCO groups and the viscosity of the reaction liquid 2 in the reaction process;
when the content of-NCO group in the reaction liquid 2 accounts for 3.8 percent of the weight of the reaction liquid 2 and the viscosity is 15000-30000cps at 120 ℃, the reaction is stopped, and the reaction liquid 2 is the polyurethane moisture curing hot melt adhesive.
Application example 3
The preparation method of the polyurethane moisture-curing hot melt adhesive obtained in the above examples 2 to 7 respectively used for the composite furniture board with the PETG film comprises the following specific steps:
(1) Taking 6 same base layer plates, and removing surface dust;
the base layer board is a medium-density fiberboard with the thickness of 1cm;
(2) Respectively coating polyurethane moisture-curing hot melt adhesive on the 6 pretreated base layer plates at the temperature of 120 ℃, wherein the coating thickness is 50g/m 2 ；
(3) Respectively covering PETG films on the coated polyurethane moisture-curing hot melt adhesive, respectively performing roller pressing treatment, controlling the pressure to be 0.3MPa in the pressing process, performing pressing for 0.1min, standing and curing for 5 days after pressing, and finally obtaining 6 composite furniture plates with the PETG films;
the thickness of the PETG film is 0.1cm.
The 6 obtained composite furniture boards with the PETG film are all of a layered structure, and are sequentially a base layer board, an adhesive layer and a PETG film layer from bottom to top;
the adhesive layer is arranged between the base layer plate and the PETG film layer, is coated on the base layer plate and has the coating thickness of 50g/m 2 The polyurethane moisture-curing hot melt adhesive is subjected to roller pressing treatment, the pressure is controlled to be 0.3MPa in the pressing process for pressing for 0.1min, and the polyurethane moisture-curing hot melt adhesive is kept still for 3 days after pressing to obtain 6 composite furniture boards with PETG films;
the thickness of the PETG film layer is 0.1cm;
the base layer board is a medium-density fiberboard with the thickness of about 1cm.
The 6 composite furniture boards with PETG film obtained by the above test have the peel strength of 2.5-3N/mm.
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 (3)

1. A composite furniture board with a PETG membrane is characterized in that the composite furniture board with the PETG membrane is of a layered structure and sequentially comprises a base layer board, an adhesive layer and a PETG membrane layer from bottom to top;
the adhesive layer is obtained by laminating a polyurethane moisture-curing hot melt adhesive coated on the base layer plate between the base layer plate and the PETG film layer through a roller and then standing for 3-7 days;
the thickness of the PETG film layer is 0.01-0.1cm;
the base layer board is a plywood or a medium density fiberboard;
the content of-NCO groups in the polyurethane moisture-curing hot melt adhesive is 2-5% of that of the polyurethane moisture-curing hot melt adhesive in percentage by weight, the viscosity of the polyurethane moisture-curing hot melt adhesive is 15000-30000cps at 120 ℃, and the components and the content of the raw materials for preparing the polyurethane moisture-curing hot melt adhesive are as follows in percentage by weight:
20 to 40 percent of polyester polyol
20 to 40 percent of polyether polyol
10 to 30 percent of tackifying resin
1 to 10 percent of chain extender
0.2 to 0.5 percent of stabilizer
0.01 to 0.1 percent of catalyst
10-30% of isocyanate;
the polyester polyol is polymerized by one or more than two of adipic acid, sebacic acid, dodecanedioic acid, terephthalic acid, isophthalic acid or phthalic acid and one or more than two of hexanediol, butanediol, diethylene glycol or neopentyl alcohol, and the weight-average molecular weight is 1000-5000;
the polyether glycol is polyoxypropylene glycol or polytetrahydrofuran ether glycol, and the weight-average molecular weight of the polyether glycol is 400-2000;
the tackifying resin is one or two of acrylic resin, terpene resin and petroleum resin;
the chain extender is 1, 4-butanediol, trimethylolpropane or a mixture of 1, 4-butanediol and TMP;
the stabilizer is a hindered phenol antioxidant which is 1010, 1076 or 168 produced by BASF;
the catalyst is at least one of dimorpholinodiethylether, N-dimethylcyclohexylamine and triethylamine;
the preparation method of the polyurethane moisture-curing hot melt adhesive specifically comprises the following steps:
(1) Firstly, controlling the temperature of polyester polyol to be 110-120 ℃ for melting to obtain molten polyester polyol;
(2) Sequentially adding polyether polyol and a stabilizer into the molten polyester polyol obtained in the step (1), controlling the temperature to be 110-130 ℃, stirring and mixing uniformly, adding tackifying resin while stirring, and continuously stirring and mixing uniformly after the tackifying resin is completely added to obtain a mixture;
(3) Then controlling the pressure of the mixture obtained in the step (2) to be minus 0.09MPa +/-0.01, maintaining the temperature at 110-130 ℃ for 50-70min to remove water vapor generated by raw material storage, then cooling to 80-100 ℃, adding isocyanate and a catalyst while stirring, and after the addition is finished, carrying out aldol condensation reaction for 50-70min under the condition of stirring at the temperature of 90-110 ℃ and controlling the pressure to be minus 0.09MPa +/-0.01 to obtain a reaction solution 1;
(4) Adding a chain extender into the reaction solution 1 obtained in the step (3), and then controlling the pressure to be minus 0.09MPa +/-0.01 and the temperature to be 90-110 ℃ under the stirring condition to carry out reaction to obtain a reaction solution 2;
and (3) sampling and testing the content and viscosity of the-NCO group in the reaction liquid 2 in the reaction process, stopping the reaction when the content of the-NCO group in the reaction liquid 2 accounts for 2-5% of the weight of the reaction liquid 2 and the viscosity of the reaction liquid 2 at 120 ℃ is 15000-30000cps, and obtaining the reaction liquid 2 which is the polyurethane moisture curing hot melt adhesive.
2. The composite furniture board with PETG film according to claim 1, wherein the polyurethane moisture-curing hot melt adhesive coated on the base sheet material is coated to a thickness of 30-70g/m 2 。
3. The composite furniture board with PETG film according to claim 1, wherein the rollers are used for pressing, and the pressing is carried out for 0.05-0.1min under the control of the pressure of 0.3-0.5MPa in the pressing process.
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CN111073583A (en) * 2019-12-31 2020-04-28 华威粘结材料（上海）股份有限公司 Novel heat-resistant polyurethane hot melt adhesive for lamp industry and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010234797A (en) * 2009-03-09 2010-10-21 Dainippon Printing Co Ltd Method for manufacturing decorative sheet and decorative sheet obtained by the same
JP2016203507A (en) * 2015-04-23 2016-12-08 Dic株式会社 Mirror surface decorative plate
CN107090268A (en) * 2017-06-09 2017-08-25 南通恒华粘合材料科技有限公司 Fabric is compound with high moisture-inhibiting monocomponent polyurethane hot melt adhesive and preparation method thereof
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