CN113106765A - Environment-friendly high-flame-retardance multilayer composite polyurethane synthetic leather and preparation method thereof - Google Patents
Environment-friendly high-flame-retardance multilayer composite polyurethane synthetic leather and preparation method thereof Download PDFInfo
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- CN113106765A CN113106765A CN202110390398.4A CN202110390398A CN113106765A CN 113106765 A CN113106765 A CN 113106765A CN 202110390398 A CN202110390398 A CN 202110390398A CN 113106765 A CN113106765 A CN 113106765A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0013—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using multilayer webs
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
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- D06N3/0095—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique by inversion technique; by transfer processes
- D06N3/0097—Release surface, e.g. separation sheets; Silicone papers
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention provides an environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather and a preparation method thereof; the polyurethane synthetic leather comprises a surface layer, an intermediate layer, a bonding layer, base cloth, a composite layer, base cloth and a finishing layer which are sequentially attached; the surface layer is made of polyurethane resin added with organic flame retardant; the middle layer and the composite layer are respectively and independently made of polyurethane resin containing a flame retardant and a flame-retardant synergist; the finishing layer is prepared from polyacrylate emulsion containing a flame retardant and a flame-retardant synergist; the adhesive layer is made of a polyurethane resin containing a flame retardant. The polyurethane synthetic leather provided by the invention has a good flame retardant effect, and keeps the appearance and the negotiated physical properties of the polyurethane synthetic leather on the basis of not influencing the color fastness of the polyurethane synthetic leather. According to the preparation method, a multi-layer composite design is adopted, and different flame retardants and auxiliaries are added into different layer structures, so that the polyurethane synthetic leather can meet basic use, and the flame retardant property of the polyurethane synthetic leather can be greatly improved.
Description
Technical Field
The invention belongs to the technical field of synthetic leather manufacturing, particularly relates to flame-retardant polyurethane synthetic leather, and particularly relates to environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather and a preparation method thereof.
Background
The polyurethane synthetic leather has excellent performances of good glossiness, genuine leather hand feeling, good wear resistance and folding resistance, good cold resistance, air permeability, moisture permeability, aging resistance and the like, and replaces the best position of natural leather. Because the appearance of the polyurethane synthetic leather is similar to that of natural leather, the polyurethane synthetic leather has better performance, and is widely applied to industries such as automobiles, home furnishings, clothes, shoemaking, bags and the like.
Although polyurethane synthetic leather has excellent properties and a wide range of applications, it is very combustible, and burns off a large amount of heat and a large amount of smoke and toxic gases, thereby limiting the application of polyurethane synthetic leather. In order to improve the flame retardant property of the polyurethane synthetic leather, the polyurethane synthetic leather needs to be subjected to flame retardant treatment by using a flame retardant.
Polyurethane synthetic leather treated by the existing flame-retardant finishing technology has the defects of poor hand feeling, reduced mechanical property and insufficient flame retardance, and cannot meet the use requirement. Therefore, with the continuous development of the polyurethane synthetic leather market, research and development of polyurethane synthetic leather with high flame retardant property are carried out to meet the requirement of the market on functional synthetic leather products, so that the polyurethane synthetic leather has important social significance and economic significance.
Disclosure of Invention
The invention aims to solve the problems that the polyurethane synthetic leather has poor flame retardant property and the existing flame retardant finishing technology has damage to various properties of the polyurethane synthetic leather, and provides the environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather and the preparation method thereof.
An environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather comprises a surface layer, a middle layer, a bonding layer, a base fabric, a composite layer, a base fabric and a finishing layer which are sequentially attached;
the surface layer is made of polyurethane resin added with an organic flame retardant; the middle layer and the composite layer are respectively and independently made of polyurethane resin containing a flame retardant and a flame-retardant synergist;
the finishing layer is prepared from polyacrylate emulsion containing a flame retardant and a flame-retardant synergist; the adhesive layer is made of a polyurethane resin containing a flame retardant.
According to the technical scheme, by designing each layer structure of the polyurethane synthetic leather, adding different flame retardants and auxiliaries into different hierarchical structures, and carrying out different treatments, the polyurethane synthetic leather can meet basic use and can achieve a higher flame retardant effect. And on the premise of not influencing the color fastness and other properties of the synthetic leather, the appearance and the negotiated physical properties of the polyurethane synthetic leather are kept to the maximum extent.
According to the technical scheme, the finishing layer is made of the polyacrylate emulsion with good weather resistance, so that the production cost can be reduced, and the polyacrylate emulsion is flexible and elastic after film forming and can be firmly bonded with the fabric and the flame retardant, so that the added flame retardant is not easy to fall off, and the service cycle is long.
Preferably, the polyurethane resin for preparing the surface layer, the intermediate layer and the bonding layer is respectively and independently added with a bridging agent, butanone, color paste, a leveling agent and a light-resistant variable additive.
Preferably, the organic flame retardant is one or a mixture of more of halogen-free phosphate flame retardants (including phosphate esters or substituted phosphonate esters and the like), phosphaphenanthrene flame retardants and phosphazene flame retardants.
In the technical scheme, the surface layer is made of the liquid phosphorus-containing organic flame retardant and the solid organic flame retardant which is well compatible with the solvent type polyurethane resin, so that the good wear resistance of the surface layer resin can be maintained, the powder flame retardant in the lower layer structure can be prevented from falling off from the surface, and certain flame retardance can be improved.
Further preferably, the organic flame retardant is one or a mixture of several of methyl phosphonic acid dimethyl ester, DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), tricresyl phosphate, triethyl phosphate and trimethyl phosphate.
Preferably, in the intermediate layer: the flame retardant is one or a mixture of more of ammonium polyphosphate aluminium hypophosphite, alkyl aluminium hypophosphite (such as diethyl aluminium hypophosphite) and melamine polyphosphate which are subjected to thinning treatment, and the average particle size is 3-12 mu m;
in the intermediate layer: the flame-retardant synergist is one or a mixture of more of silicon dioxide, zinc borate, boron phosphate, hydrotalcite, organic montmorillonite, magnesium hydroxide and aluminum hydroxide.
According to the technical scheme, the middle layer is made of the powder flame retardant and the flame-retardant synergist which are subjected to refining treatment, powder settlement generated by long-time placement of the prepared flame-retardant slurry can be slowed down, agglomeration in a slurry tank in the processing process is reduced, and the flame retardant is uniformly dispersed in the middle layer. Compared with a low-valence organic flame retardant containing P, the inorganic powder flame retardant has high valence of P, mainly plays a role in condensed phase flame retardance, can promote resin to form a compact carbon layer in the combustion process, covers the surface of a fabric and reduces damage.
Preferably, in the bonding layer, the flame retardant is one or a mixture of more of halogen-free phosphate flame retardants, phosphaphenanthrene flame retardants and phosphazene flame retardants.
When the inorganic powder flame retardant is added into a polymer matrix, the inorganic powder flame retardant gradually migrates out of the matrix under the change of external conditions (damp heat or external force action) due to poor compatibility, so that white frost and other phenomena are generated, and the appearance and the performance of a product are influenced.
In the technical scheme, the adhesive layer is made of organic liquid and solid flame retardant which are well compatible with the solvent type polyurethane resin, so that the water-soluble powder flame retardant in the middle layer can greatly reduce the contact with water vapor, reduce the phenomenon of white frost and improve the flame retardance of the resin and the base cloth.
Preferably, the flame retardant used in the adhesive layer is one or a mixture of several of dimethyl methylphosphonate, DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), tricresyl phosphate, triethyl phosphate and trimethyl phosphate.
Preferably, the base fabric is a woven fabric (cloth) or a knitted fabric (cloth) of ultrafine fibers.
Preferably, in the composite layer and the finishing layer: the flame retardants are respectively and independently selected from expandable graphite and one or more of refined ammonium polyphosphate, aluminum hypophosphite, alkyl aluminum hypophosphite (such as diethyl aluminum hypophosphite) and melamine polyphosphate, and the average particle size is 3-12 μm;
in the composite layer and the finishing layer: the flame-retardant synergist is respectively and independently one or a mixture of more of silicon dioxide, zinc borate, boron phosphate, hydrotalcite, organic montmorillonite, magnesium hydroxide and aluminum hydroxide.
Preferably, the base fabric is one of fiber woven fabrics (cloths).
Preferably, the weight of the polyurethane resin is 100 parts: the weight of the flame retardant in the surface layer is 15-25 parts; the weight of the flame retardant in the middle layer is 15-35 parts, and the weight of the flame retardant synergist is 1-5 parts; the weight of the flame retardant in the bonding layer is 10-25 parts; the weight of the flame retardant in the composite layer is 10-40 parts, and the weight of the flame retardant synergist is 1-5 parts;
the weight of the polyacrylate emulsion is 100 parts: the weight of the flame retardant in the finishing layer is 10-40 parts, and the weight of the flame retardant synergist is 1-5 parts.
As a specific preference, the formulation of the slurry for preparing the surface layer is, by mass: 100 parts of polyurethane resin, 3-15 parts of bridging agent, 100 parts of butanone, 15-25 parts of flame retardant, 2-8 parts of color paste, 0.1-2 parts of flatting agent and 1-2 parts of light-resistant variable additive.
Specifically, the formula of the slurry for preparing the intermediate layer is as follows by mass: 100 parts of polyurethane resin, 3-15 parts of bridging agent, 100 parts of butanone, 15-35 parts of flame retardant, 1-5 parts of flame retardant synergist, 2-8 parts of color paste, 0.1-2 parts of flatting agent and 1-2 parts of light-resistant variable assistant.
Specifically, the formula of the slurry for preparing the bonding layer is as follows by mass: 100 parts of polyurethane resin, 3-15 parts of bridging agent, 90 parts of butanone, 10-25 parts of flame retardant, 2-8 parts of color paste, 0.1-2 parts of flatting agent and 1-2 parts of light-resistant color-changing assistant.
In the invention, the bridging agent comprises isocyanate bridging agent (such as LA-75) and melamine bridging agent (such as bridging agent 619); the color paste is an oily dry color paste; the leveling agent is an organic silicon leveling agent; the light-resistant optical change assistant comprises benzophenone light-resistant optical change assistant and hindered amine light-resistant optical change assistant.
Preferably, the thickness of the surface layer is 10-20 μm; the thickness of the middle layer is 10-25 mu m; the thickness of the bonding layer is 10-20 mu m; the thickness of the composite layer is 0.5-1 mm.
According to the technical scheme, the flame retardant subjected to refining treatment and the flame-retardant synergist are selected and compounded for use, and meanwhile, the thickness (0.5-1 mm) of the composite layer is increased, so that the polyurethane synthetic leather can achieve a better flame-retardant effect.
A preparation method of the multilayer composite polyurethane synthetic leather comprises the following steps:
(1) coating the surface layer, the intermediate layer and the bonding layer on the surface of the release paper in sequence, and respectively heating and drying the coated surface layer and the coated intermediate layer to obtain a coating layer;
(2) hot-pressing and attaching the bonding layer of the coating layer obtained in the step (1) and the base cloth, drying, stripping the release paper and rolling to obtain a semi-finished product;
(3) coating a finishing layer on the back of the base fabric; and (3) bonding the base cloth bonded with the bonding layer in the step (2) with the front side of the base cloth by using a composite layer, and then rolling, heating and curing to obtain the environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather.
Further preferably, the release paper is one of plain paper and embossed paper.
Specifically, the preparation method of the multilayer composite polyurethane synthetic leather comprises the following steps:
(1) coating the polyurethane surface layer slurry on the surface of release paper in a scraping way, and heating and drying at 80-120 ℃;
(2) coating the polyurethane intermediate layer slurry on the surface layer by scraping, and heating and drying at 80-120 ℃;
(3) coating the polyurethane adhesive layer slurry on the middle layer by scraping to form an adhesive layer;
(4) hot-pressing and attaching the bonding layer and the base cloth at the temperature of 80-140 ℃, drying at the speed of 5-30 m/min, stripping the release paper and rolling to obtain a semi-finished synthetic leather;
(5) treating the back surface of the base fabric by using the flame-retardant finishing layer slurry to form a flame-retardant finishing layer;
(6) and (3) using polyurethane resin added with a flame retardant and a flame-retardant synergist, enabling the semi-finished synthetic leather prepared in the step (4) to be tightly combined with the surface of the base fabric through a compounding process, then rolling and curing at 80-130 ℃ for 8-16h, and preparing the environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather.
According to the preparation method, on the basis of a dry process of common synthetic leather, various halogen-free phosphate ester flame retardants, inorganic powder flame retardants and flame retardant synergists are added, so that the flame retardant property of the polyurethane synthetic leather is greatly improved. On the premise of not influencing the color fastness and other properties of the synthetic leather, the flame retardant property of the synthetic leather can meet the requirements of' BS 5852: 2006, (source0 and source1) "requirements. In addition, the appearance and the negotiated physical properties of the polyurethane synthetic leather are kept to the maximum extent.
Preferably, the compounding process in the step (6) is one of hot melt adhesive compounding and bi-component PU adhesive compounding.
Compared with the prior art, the invention has the beneficial effects that:
the environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather has good flame-retardant effect, and keeps the appearance and the negotiated physical properties of the polyurethane synthetic leather to the maximum extent on the basis of not influencing the color fastness and other properties of the polyurethane synthetic leather.
According to the preparation method of the polyurethane synthetic leather, on the basis of a common synthetic leather dry process, a multi-layer composite design is adopted, different flame retardants and auxiliaries are added into different layer structures, and different treatments are carried out, so that the polyurethane synthetic leather can meet basic use requirements, and the flame retardant property of the polyurethane synthetic leather can be greatly improved.
Drawings
Fig. 1 is a schematic view of a layered structure of an environment-friendly high-flame-retardant multi-layer composite polyurethane synthetic leather fabric.
In the figure: 1. a polyurethane surface layer; 2. a polyurethane intermediate layer; 3. a polyurethane adhesive layer; 4. a base cloth; 5. compounding layers; 6. base fabric; 7. and a flame retardant finishing layer.
Detailed Description
The present invention will be further illustrated by the following examples, but the present invention is not limited to the following examples.
As shown in figure 1, the environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather comprises a surface layer 1, an intermediate layer 2, a bonding layer 3, a base fabric 4, a composite layer 5, a base fabric 6 and a finishing layer 7 which are sequentially attached.
The sources of the raw materials in the following examples are: the polyurethane resin 0130, 595, the color paste RX-851 and the organic silicon leveling agent 26G are from the company of Roxing, Zhejiang industries, Ltd;
the isocyanate bridging agent LA-75 and the hot melt adhesive JUR-628 are from Zhejiang maple science and technology Limited;
the melamine bridging agent 619 is from Shaoxing Olympic chemical industry Co., Ltd;
polyacrylate emulsion 908 was from Hangzhou Point wetting chemical Co., Ltd;
ammonium polyphosphate TF-201S is from Taifeng novel flame retardant, Inc., Xiushu, aluminum hypophosphite and diethyl aluminum hypophosphite are from Suzhou joint-male chemical engineering technologies, and melamine polyphosphate is from Zhenjiu star flame retardant, Inc.;
the light-resistant assistant Tinuvin770 and C81 are from Pasteur Germany;
the superfine fiber woven fabric and knitted fabric come from China town Dian space short plush factory, thickness of 0.4 + -0.05 mm, and gram weight of 120g/m2；
The base fabric is from Ming-Guang warp knitting works of Hainin, has a thickness of 2.3 + -0.10 mm and a gram weight of 210g/m2；
Example 1
(1) Coating polyurethane surface layer slurry on the surface of embossed release paper in a scraping way, heating and drying at 80 ℃ to form a surface layer with the thickness of 15 mu m, wherein the formula of the slurry comprises the following components in percentage by mass: 100 parts (about 20kg) of polyurethane resin (0130), 3 parts of isocyanate bridging agent (LA-75), 100 parts of butanone, 10 parts of dimethyl methylphosphonate, 5 parts of DOPO, 2 parts of color paste (RX-851), 0.1 part of organosilicon leveling agent (26G) and 2 parts of light-resistant variable assistant (Tinuvin 770);
(2) the polyurethane intermediate layer slurry is spread on the surface layer, and then is heated and dried at 85 ℃ to form a 25-micron intermediate layer, wherein the formula of the slurry comprises the following components in percentage by mass: 100 parts of polyurethane resin (595) (about 20kg), 4 parts of melamine bridging agent (619), 100 parts of butanone, 15 parts of ammonium polyphosphate (refined with the particle size of 12 mu m), 5 parts of aluminum hypophosphite (refined with the particle size of 3 mu m), 2 parts of zinc borate, 1 part of silicon dioxide, 3 parts of color paste (RX-851), 0.5 part of organic silicon leveling agent (26G) and 2 parts of light-resistant variable additive (Tinuvin 770);
(3) and (2) coating the polyurethane adhesive layer slurry on the middle layer by scraping to form a 15-micron adhesive layer, wherein the formula of the slurry comprises the following components in mass percent: 100 parts (about 20kg) of polyurethane resin (0130), 5 parts of isocyanate bridging agent (LA-75), 90 parts of butanone, 20 parts of trimethyl phosphate, 5 parts of DOPO, 3 parts of color paste (RX-851), 2 parts of organosilicon leveling agent (26G) and 1 part of light-resistant variable assistant (C81);
(4) hot-pressing and laminating the bonding layer and the superfine fiber woven fabric at 100 ℃, drying at the speed of 8m/min, stripping release paper and rolling to obtain a semi-finished synthetic leather;
(5) treating the back of the base fabric by using the flame-retardant finishing layer slurry to form a flame-retardant finishing layer, wherein the slurry comprises the following components in parts by mass: 100 parts (about 30kg) of polyacrylate emulsion (908), 10 parts of ammonium polyphosphate (refined and processed with the particle size of 12 mu m), 5 parts of expandable graphite and 2 parts of zinc borate;
(6) using polyurethane resin (595) (about 30kg) added with the same flame retardant and flame retardant synergist (the components and the dosage are the same) as the flame retardant and the flame retardant synergist in the step (5), enabling the semi-finished synthetic leather prepared in the step (4) to be tightly combined with the surface of the base fabric through a compounding process, then rolling and curing at 80 ℃ for 12 hours to prepare the environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather; wherein the thickness of the composite layer is about 0.8 mm.
Example 2
(1) Coating polyurethane surface layer slurry on the surface of embossed release paper in a scraping way, heating and drying at 115 ℃ to form a surface layer with the thickness of 15 mu m, wherein the formula of the slurry comprises the following components in percentage by mass: 100 parts (about 20kg) of polyurethane resin (0130), 10 parts of isocyanate bridging agent (LA-75), 100 parts of butanone, 15 parts of tricresyl phosphate, 5 parts of triethyl phosphate, 5 parts of color paste (RX-851), 1 part of organosilicon leveling agent (26G) and 1 part of light-resistant variable assistant (Tinuvin 770);
(2) the polyurethane intermediate layer slurry is spread on the surface layer, and then is heated and dried at 120 ℃ to form a 25-micron intermediate layer, wherein the formula of the slurry comprises the following components in percentage by mass: 100 parts of polyurethane resin (595) (about 20kg), 12 parts of melamine bridging agent (619), 100 parts of butanone, 5 parts of diethyl aluminum hypophosphite (with the grain diameter of 3 mu m), 15 parts of melamine polyphosphate (with the grain diameter of 5 mu m), 1 part of silicon dioxide, 1 part of magnesium hydroxide, 2 parts of aluminum hydroxide, 8 parts of color paste (RX-851), 2 parts of organosilicon leveling agent (26G) and 1 part of light-resistant variable additive (Tinuvin 770);
(3) and (2) coating the polyurethane adhesive layer slurry on the middle layer to form a 10-micron adhesive layer, wherein the slurry comprises the following components in percentage by mass: 100 parts (about 20kg) of polyurethane resin (595), 10 parts of melamine bridging agent (619), 90 parts of butanone, 15 parts of tricresyl phosphate, 5 parts of DOPO, 2 parts of color paste (RX-851), 1 part of organosilicon leveling agent (26G) and 1 part of light-resistant variable assistant (C81);
(4) hot-pressing and laminating the bonding layer and the superfine fiber woven fabric at 120 ℃, drying at the speed of 10m/min, stripping release paper and rolling to obtain a semi-finished synthetic leather;
(5) treating the back of the base fabric by using the flame-retardant finishing layer slurry to form a flame-retardant finishing layer, wherein the slurry comprises the following components in parts by mass: 100 parts (about 30kg) of polyacrylate emulsion (908), 8 parts of ammonium polyphosphate (with the grain size of 12 mu m) by thinning treatment, 2 parts of diethyl aluminum hypophosphite (with the grain size of 3 mu m) by thinning treatment, 2 parts of melamine polyphosphate (with the grain size of 5 mu m) by thinning treatment, 8 parts of expandable graphite and 2 parts of boron phosphate;
(6) using polyurethane resin (595) (about 30kg) added with the same flame retardant and flame retardant synergist as the step (5), enabling the semi-finished synthetic leather prepared in the step (4) to be tightly combined with the surface of the base fabric through a compounding process, then rolling and curing at 100 ℃ for 8h to prepare the environment-friendly high-flame retardant multilayer composite polyurethane synthetic leather; wherein the thickness of the composite layer is about 0.7 mm.
Comparative example 1 (middle layer added with gas phase flame retardant organic flame retardant)
This comparative example differs from example 1 in that:
in the step (2), the formula of the slurry of the middle layer comprises the following components in parts by mass: 100 parts (about 20kg) of polyurethane resin (595), 4 parts of melamine bridging agent (619), 100 parts of butanone, 10 parts of dimethyl methylphosphonate, 7 parts of tricresyl phosphate, 8 parts of triethyl phosphate, 3 parts of color paste (RX-851), 0.5 part of organosilicon leveling agent (26G) and 2 parts of light-resistant variable additive (Tinuvin 770);
comparative example 2 (surface layer resin added with inorganic powder flame retardant and flame retardant synergist)
This comparative example differs from example 1 in that:
in the step (1), the formula of the slurry of the surface layer comprises the following components in mass percent: 100 parts of polyurethane resin (0130) (about 20kg), 3 parts of isocyanate bridging agent (LA-75), 100 parts of butanone, 12 parts of ammonium polyphosphate (with the grain diameter of 12 mu m) subjected to refining treatment, 3 parts of melamine polyphosphate (with the grain diameter of 5 mu m) subjected to refining treatment, 1 part of silicon dioxide, 2 parts of color paste (RX-851), 0.1 part of organosilicon leveling agent (26G) and 2 parts of light-resistant variable assistant (Tinuvin 770);
comparative example 3 (composite layer non-flame retardant)
This comparative example differs from example 2 in that:
and (6) using polyurethane resin (595) (about 30kg) without adding a flame retardant and a flame retardant synergist, enabling the semi-finished synthetic leather prepared in the step (4) to be tightly combined with the surface of the base fabric through a compounding process, then rolling and curing at 100 ℃ for 8 hours to prepare the environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather.
COMPARATIVE EXAMPLE 4 (base fabric flame-retardant free finish)
This comparative example differs from example 2 in that: and (5) carrying out flame retardant treatment on the back surface of the base fabric.
The polyurethane synthetic leathers obtained in examples 1 to 2 and comparative examples 1 to 4 were subjected to a surface color fastness test (see GB/T8949-2008), an LOI (limiting oxygen index) test (see GB/T5455-1997), and a flammability evaluation test (see BS5852-2006), respectively, and the test structures are shown in the following tables.
TABLE 1 results of performance test of polyurethane synthetic leathers prepared in examples 1 to 2 and comparative examples 1 to 4
As can be seen from Table 1, the polyurethane synthetic leathers prepared in examples 1-2 and comparative examples 1-2 both passed the following procedures of BS 5852-2006: tests of Source0 and Source1 show that in examples 1-2, under the combined action of various phosphate flame retardants, inorganic powder flame retardants and flame retardant synergist, the environment-friendly and efficient flame retardance of the multilayer composite polyurethane synthetic leather is realized, the limit oxygen index reaches over 28%, and the surface color fastness is not less than grade 3.
Comparative example 1 the flame propagation rate during combustion was relatively fast and the limiting oxygen index was low due to the lack of condensed phase flame retardance in the intermediate layer. Comparative example 2 because the surface layer had an inorganic powder flame retardant, the powder particles were partially detached from the substrate during abrasion, affecting the color fastness. Comparative examples 3 and 4 have a lower limiting oxygen index although having a certain flame retardancy because of the presence of a non-flame retardant portion in the layer structure. By designing the flame-retardant function of each structural layer of the synthetic leather, the environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather meeting the relevant test requirements can be prepared.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and it should be understood that any person skilled in the art can make modifications and equivalents of the above-described embodiments without departing from the scope of the present invention.
Claims (10)
1. The environment-friendly high-flame-retardance multilayer composite polyurethane synthetic leather is characterized by comprising a surface layer, a middle layer, a bonding layer, base cloth, a composite layer, a base cloth and a finishing layer which are sequentially attached;
the surface layer is made of polyurethane resin added with an organic flame retardant; the middle layer and the composite layer are respectively and independently made of polyurethane resin containing a flame retardant and a flame-retardant synergist;
the finishing layer is prepared from polyacrylate emulsion containing a flame retardant and a flame-retardant synergist; the adhesive layer is made of a polyurethane resin containing a flame retardant.
2. The multilayer composite polyurethane synthetic leather according to claim 1, wherein the polyurethane resins for preparing the surface layer, the intermediate layer and the bonding layer are respectively and independently added with a bridging agent, butanone, color paste, a leveling agent and a light-resistant variable assistant.
3. The multilayer composite polyurethane synthetic leather according to claim 1, wherein the organic flame retardant is one or more of a halogen-free phosphate flame retardant, a phosphaphenanthrene flame retardant and a phosphazene flame retardant.
4. The multilayer composite polyurethane synthetic leather of claim 1, wherein in the intermediate layer: the flame retardant is one or a mixture of more of refined ammonium polyphosphate, aluminum hypophosphite, alkyl aluminum hypophosphite and melamine polyphosphate, and the average particle size of the flame retardant is 3-5 mu m;
the flame-retardant synergist is one or a mixture of more of silicon dioxide, zinc borate, boron phosphate, hydrotalcite, organic montmorillonite, magnesium hydroxide and aluminum hydroxide.
5. The multilayer composite polyurethane synthetic leather according to claim 1, wherein in the bonding layer, the flame retardant is one or a mixture of halogen-free phosphate flame retardants, phosphaphenanthrene flame retardants and phosphazene flame retardants.
6. The multilayer composite polyurethane synthetic leather of claim 1, wherein in the composite layer and the finishing layer: the flame retardants are respectively and independently selected from expandable graphite, one or a mixture of more of ammonium polyphosphate subjected to refining treatment, aluminum hypophosphite, alkyl aluminum hypophosphite and melamine polyphosphate, and the average particle size is 3-12 mu m;
the flame-retardant synergist is respectively and independently one or a mixture of more of silicon dioxide, zinc borate, boron phosphate, hydrotalcite, organic montmorillonite, magnesium hydroxide and aluminum hydroxide.
7. The multilayer composite polyurethane synthetic leather according to claim 1, wherein the weight of the polyurethane resin is 100 parts: the weight of the flame retardant in the surface layer is 15-25 parts; the weight of the flame retardant in the middle layer is 15-35 parts, and the weight of the flame retardant synergist is 1-5 parts; the weight of the flame retardant in the bonding layer is 10-25 parts; the weight of the flame retardant in the composite layer is 10-40 parts, and the weight of the flame retardant synergist is 1-5 parts;
the weight of the polyacrylate emulsion is 100 parts: the weight of the flame retardant in the finishing layer is 10-40 parts, and the weight of the flame retardant synergist is 1-5 parts.
8. The multilayer composite polyurethane synthetic leather according to claim 1, wherein the thickness of the surface layer is 10-20 μm; the thickness of the middle layer is 10-25 mu m; the thickness of the bonding layer is 10-20 mu m.
9. A method for preparing the multilayer composite polyurethane synthetic leather according to any one of claims 1 to 8, wherein the method comprises the following steps:
(1) coating the surface layer, the intermediate layer and the bonding layer on the surface of the release paper in sequence, and respectively heating and drying the coated surface layer and the coated intermediate layer to obtain a coating layer;
(2) hot-pressing and attaching the bonding layer of the coating layer obtained in the step (1) and the base cloth, drying, stripping the release paper and rolling to obtain a semi-finished product;
(3) coating a finishing layer on the back of the base fabric; and (3) attaching the semi-finished product in the step (2) to the front side of the base fabric by using a composite layer, and then rolling, heating and curing to obtain the environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather.
10. A method of preparing a multilayer composite polyurethane synthetic leather according to claim 9, which comprises:
(1) coating the polyurethane surface layer slurry on the surface of release paper in a scraping way, and heating and drying at 80-120 ℃;
(2) coating the polyurethane intermediate layer slurry on the surface layer by scraping, and heating and drying at 80-120 ℃;
(3) coating the polyurethane adhesive layer slurry on the middle layer by scraping to form a coating layer with an adhesive layer;
(4) hot-pressing and attaching the bonding layer of the coating layer and the base fabric at the temperature of 80-140 ℃, drying at the speed of 5-30 m/min, stripping release paper and rolling to obtain a semi-finished synthetic leather;
(5) treating the back surface of the base fabric by using the flame-retardant finishing layer slurry to form a flame-retardant finishing layer;
(6) and (3) taking polyurethane resin added with a flame retardant and a flame-retardant synergist as composite layer slurry, tightly combining the semi-finished synthetic leather prepared in the step (4) with the front surface of the base fabric through a composite process, then rolling and curing at 80-130 ℃ for 8-16h, and preparing the environment-friendly high-flame-retardant multilayer composite polyurethane synthetic leather.
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