WO2015043353A1 - 一种纺织品复合用湿固化反应型聚氨酯热熔胶的制备方法 - Google Patents

一种纺织品复合用湿固化反应型聚氨酯热熔胶的制备方法 Download PDF

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WO2015043353A1
WO2015043353A1 PCT/CN2014/085368 CN2014085368W WO2015043353A1 WO 2015043353 A1 WO2015043353 A1 WO 2015043353A1 CN 2014085368 W CN2014085368 W CN 2014085368W WO 2015043353 A1 WO2015043353 A1 WO 2015043353A1
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parts
antioxidant
hot melt
polyester polyol
vacuum degree
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PCT/CN2014/085368
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English (en)
French (fr)
Inventor
李哲龙
朱万育
肖虎鹏
马洪伟
曾作祥
沈艳
Original Assignee
昆山天洋热熔胶有限公司
上海天洋热熔粘接材料股份有限公司
华东理工大学
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Application filed by 昆山天洋热熔胶有限公司, 上海天洋热熔粘接材料股份有限公司, 华东理工大学 filed Critical 昆山天洋热熔胶有限公司
Priority to DE112014004472.5T priority Critical patent/DE112014004472T5/de
Priority to US14/917,393 priority patent/US20160215185A1/en
Priority to CH00396/16A priority patent/CH710287B1/de
Priority to JP2016521688A priority patent/JP5999828B1/ja
Publication of WO2015043353A1 publication Critical patent/WO2015043353A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/08—Polyurethanes from polyethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/16—Catalysts
    • C08G18/161—Catalysts containing two or more components to be covered by at least two of the groups C08G18/166, C08G18/18 or C08G18/22
    • C08G18/163—Catalysts containing two or more components to be covered by at least two of the groups C08G18/166, C08G18/18 or C08G18/22 covered by C08G18/18 and C08G18/22
    • C08G18/165—Catalysts containing two or more components to be covered by at least two of the groups C08G18/166, C08G18/18 or C08G18/22 covered by C08G18/18 and C08G18/22 covered by C08G18/18 and C08G18/24
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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    • C08G18/16—Catalysts
    • C08G18/18—Catalysts containing secondary or tertiary amines or salts thereof
    • C08G18/20—Heterocyclic amines; Salts thereof
    • C08G18/2081—Heterocyclic amines; Salts thereof containing at least two non-condensed heterocyclic rings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/16—Catalysts
    • C08G18/22—Catalysts containing metal compounds
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
    • C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4202—Two or more polyesters of different physical or chemical nature
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
    • C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4825—Polyethers containing two hydroxy groups
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
    • C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
    • C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
    • C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/06—Polyurethanes from polyesters
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M17/00—Producing multi-layer textile fabrics
    • D06M17/04—Producing multi-layer textile fabrics by applying synthetic resins as adhesives
    • D06M17/10—Polyurethanes polyurea
    • 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
    • D06N3/146—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 characterised by the macromolecular diols used
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2170/00—Compositions for adhesives
    • C08G2170/20—Compositions for hot melt adhesives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/014—Stabilisers against oxidation, heat, light or ozone
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/005—Stabilisers against oxidation, heat, light, ozone
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters

Definitions

  • the invention relates to a preparation method of a moisture curing reaction type polyurethane hot melt adhesive for textile composite.
  • Hot melt adhesives are gaining more and more attention due to their fast bonding, non-polluting, non-toxic, low organic volatiles (VOC).
  • Conventional hot melt adhesives are generally based on thermoplastic resins. Although they can be quickly cured and bonded, the adhesive layer is not resistant to high temperatures after curing, and is easily soluble in organic solvents. The bonding strength is not high, so the use of thermoplastic hot melt adhesives Limited.
  • thermoplastic hot melt adhesives Limited In order to overcome the above shortcomings, a new type of moisture-curing polyurethane hot melt adhesive has been developed. This type of hot melt adhesive not only has the advantages of high initial tackiness and rapid curing positioning of conventional hot melt adhesive, but also after physical curing of the adhesive layer.
  • the chemical cross-linking inside the system can significantly improve the bonding strength, water resistance and solvent resistance of the adhesive layer, and has the advantages of the traditional solvent-based adhesive and the thermoplastic hot-melt adhesive.
  • the moisture-curing reactive polyurethane hot melt adhesive is a type of polyurethane adhesive containing a terminal-NCO group.
  • the melt sizing is heated, and after the layer is cooled and physically solidified to produce a preliminary adhesive force, the end NCO in the glue layer is then reacted with moisture in the air or an active hydrogen compound on the surface of the adherend to produce chemical cross-linking. Cured.
  • the moisture-curing reactive polyurethane hot melt adhesive not only has the advantages of traditional thermoplastic hot melt adhesive for rapid bonding and positioning, but also provides high initial tack strength, and can further cure cross-linking, so that the adhesive strength and cohesive strength of the adhesive layer can be A significant improvement has been achieved.
  • moisture-curing reactive polyurethane hot melt adhesives are widely used in the bonding of textile composites, rubber, plastics, metals and automobile manufacturing, textiles, footwear, bookbinding, wood industry and furniture industries, and electronics industries.
  • the moisture-curing reactive polyurethane hot melt adhesive prepared by the invention is mainly used for textile compounding.
  • the moisture-curing reactive polyurethane hot melt adhesive has two types: a full polyether type prepolymer and a full polyester type prepolymer.
  • the all-polyether polyurethane hot melt adhesive has low melt viscosity and good melt viscosity stability. Good water resistance, low cost, etc., but low initial adhesion and final bond strength; and all-polyester polyurethane hot melt adhesive has good initial and final bond strength, but poor hydrolysis resistance and poor flexibility.
  • the main advantage of the moisture-curing reaction type polyurethane hot melt adhesive prepared by the invention is that the mixed polyol raw material of the polyether polyol and the polyester polyol is combined with the polyether type moisture curing reaction type polyurethane hot melt adhesive and the polyester type wet. The advantages of both curing reactive polyurethane hot melt adhesives.
  • One of the objects of the present invention is to provide a moisture-curing reactive polyurethane hot melt adhesive for textile composites in order to solve the above-mentioned technical problems in the prior art.
  • Another object of the present invention is to provide a method for preparing a moisture-curing reactive polyurethane hot melt adhesive for textile composites as described above.
  • the present invention provides a method for preparing a moisture-curing reactive polyurethane hot melt adhesive for textile composite, comprising the following steps:
  • the polyester polyol 3000H is a polyadipate-1,6 hexanediol ester having a molecular weight of 3000
  • the polyester polyol 2000N is a polypentylene glycol neoadipate glycol having a molecular weight of 2000; the tackifying resin is an acrylic resin; and the polyether polyol 4000E is a molecular weight of 4000.
  • the antioxidant is a mixture of an antioxidant 1010 and an antioxidant 1076;
  • the MDI is 4,4'-diphenylnonane diisocyanate;
  • the mass parts of the respective materials are: 11-13 parts for MDI, 37-51 parts for polyether polyol 4000E, and 8-13 parts for polyester polyol 3000H, based on 100 parts by mass of product.
  • the alcohol 2000N is 8 - 13 parts
  • the antioxidant 1010 is 0.22 parts
  • the antioxidant 1076 is 0.22 parts
  • the tackifying resin is 19 - 20 parts
  • the catalyst is 0.14 parts
  • the white carbon black is 0.5 part.
  • the catalyst is a mixture of stannous octoate and bis(2,2-morpholinoethyl)ether in a mass ratio of 1:1.
  • the main advantage of the moisture-curing reactive polyurethane hot melt adhesive prepared by the invention is that the moisture-curing reactive polyurethane hot melt adhesive prepared by the invention not only has the traditional thermoplastic property because of the wet curing reaction type bonding principle.
  • the hot melt adhesive can be quickly bonded and positioned to provide a high initial bond strength, and can further cure the cross-linking, so that the adhesive strength and cohesive strength of the adhesive layer can be significantly improved;
  • the mixed polyol raw material of the ester polyol, so that the moisture-curing reactive polyurethane hot melt adhesive prepared by the invention combines both the polyether moisture-curing reactive polyurethane hot melt adhesive and the polyester moisture-curing reactive polyurethane hot melt adhesive.
  • the moisture-curing reaction type polyurethane hot melt adhesive prepared by the invention is applied to the textile composite, and the average peeling strength is about 20N/2.5cm (gram weight is 15g/cm), and the hydrolysis resistance is good, and the specific results are shown in Table 1. Meet the requirements of the moisture curing reactive polyurethane hot melt adhesive in the textile composite industry.
  • Example 1 The invention is further illustrated by the following examples without restricting the invention.
  • Example 1
  • the technical parameters of the moisture-curing reactive polyurethane hot melt adhesive D for textile composites are shown in Table 1.
  • the application of the moisture-curing reactive polyurethane hot melt adhesive A B C D for textile composites in textile compounding, the application method thereof comprises the following steps:
  • the textile composite composite moisture-curing polyurethane hot melt adhesive product ABCD obtained in the above Examples 1-4 was heated at a temperature of 120 ° C and then coated with a circular mesh of 0.45 ⁇ pore size to compound the polyester cotton. Then, the coated polyester cotton fabric was pressed under a pressure of 80 C 3 kgf/cm 2 , and placed in a constant temperature and humidity environment of 20 C and a humidity of 70% for 24 hours. Then cut the fabric into strips 2.5cm wide and 20cm long, check the weight of the fabric (the quality of the rubber contained in the fabric per unit area), test the peel strength, and test the peel strength after soaking the water. The specific results are shown in Table 1. Technical parameters of wet-curing reactive polyurethane hot melt adhesive for textile composites and application of glass strength test results. 120 o C viscosity, heavy weight, peel strength, peeling strength after soaking (N/2.5c 00m)
  • the moisture-curing reactive polyurethane hot melt adhesive for textile composite provided by the present invention has a viscosity of about 5000 mPa ⁇ s at 120 C, which is used in textile compounding and is not easy to be bleed. Easy to coat, the glass strength of the weight of 15g/m 2 is 19.92 N/2.5cm, and the strength of the glass after washing is not greatly decreased, indicating that the glass has good strength and excellent hydrolysis resistance.
  • the hydrolysis resistance of the wet curing reaction type polyurethane hot melt adhesive ABCD for textile composite provided by the invention decreases in turn, but the hydrolysis resistance performance is still good, and the peel strength of the product B is the best (the maximum strength of the glass per unit weight),
  • the viscosity is moderate, so that the preferred embodiment 2 of product B is the preferred embodiment, and the formulation of product B is the optimum formulation.

Abstract

一种纺织品用湿固化反应型聚氨酯热熔胶的制备方法，主要包括如下步骤：（1）将聚醚多元醇4000E、聚酯多元醇3000H、聚酯多元醇2000N、抗氧剂搅拌混合，加热升温至120℃左右，在真空度小于100Pa下，脱水0.5h；（2）加入增粘树脂，继续升温至135-140℃，在真空度小于100Pa下，脱水1.5h；（3）降温至87℃，加入4,4'-二苯基甲烷二异氰酸酯、催化剂，搅拌，在真空度小于100Pa下反应2h；（4）解除真空，加入白炭黑，快速搅拌，混匀，在真空度小于100Pa下继续搅拌10min；（5）保持出料温度在85-100℃，快速出料并封装，然后在80-85℃的条件下熟化4h，得标的产物。该产品用于纺织品复合，具有优异的剥离强度、较短的开放时间、良好的耐水解性能及良好的储存稳定性。

Description

一种纺织品复合用湿固化反应型聚氨酯热熔胶的制备方法
技术领域
本发明涉及一种纺织品复合用湿固化反应型聚氨酯热熔胶的制备方法。
背景技术
热熔胶因其粘接迅速、 无污染、 无毒、 低有机挥发物 (VOC)等特点而得到 越来越多的重视。 传统热熔胶一般是以热塑性树脂为主组分， 虽能快速固化 粘接， 但固化后胶层不耐高温， 且易溶于有机溶剂， 粘接强度不高， 因而热 塑性热熔胶的使用受到了限制。 为克服上述缺点， 开发出一种新型的湿固化 聚氨酯热熔胶， 这类热熔胶不仅具有传统热熔胶的较高初粘性、 可快速固化 定位的优点， 而且胶层物理固化后， 在体系内部产生化学交联， 使胶层粘接 强度， 耐水性、 耐溶剂性等都能得到明显改善， 兼有传统溶剂型胶粘剂和热 塑性热熔胶的优点。
湿固化反应型聚氨酯热熔胶是一类含端 -NCO基团的聚氨酯胶粘剂。使用 时， 加热熔融施胶， 待胶层冷却物理固化产生初步的粘接力后， 胶层中的端 NCO再与空气中的湿气或被粘物表面的活泼氢化合物反应， 产生化学交联固 化。 湿固化反应型聚氨酯热熔胶不仅具有传统热塑性热熔胶快速粘接定位、 提供较高的初粘强度优点， 也能进一步固化交联， 使胶层的粘接力、 内聚强 度等都能得到明显的提高。 因此， 湿固化反应型聚氨酯热熔胶广泛应用于纺 织品复合、 橡胶、 塑料、 金属与汽车制造、 纺织业、 制鞋业、 书刊装订、 木 材工业及家具行业、 电子行业等的粘接。 本发明制备的湿固化反应型聚氨酯 热熔胶主要用于纺织品复合。
湿固化反应型聚氨酯热熔胶有全聚醚型预聚体类和全聚酯型预聚体类两 种。 全聚醚型的聚氨酯热熔性胶粘剂具有熔融粘度低、 熔体粘度稳定性好、 耐水性好、 成本低等优点， 但初粘和终粘强度较低； 而全聚酯的聚氨酯热熔 性胶粘剂具有很好的初粘和终粘强度， 但是耐水解性能差、 柔韧性差。 本发 明制备的湿固化反应型聚氨酯热熔胶主要优势在于， 釆用聚醚多元醇和聚酯 多元醇的混合多元醇原料， 兼有聚醚型湿固化反应型聚氨酯热熔胶和聚酯型 湿固化反应性聚氨酯热熔胶两者的优点。
发明内容
本发明的目的之一是为了解决现有技术中的上述技术问题而提供了一种 纺织品复合用湿固化反应型聚氨酯热熔胶。
本发明的目的之二是提供上述的一种纺织品复合用湿固化反应型聚氨酯 热熔胶的制备方法。
为达到上述目的， 本发明提供了一种纺织品复合用湿固化反应型聚氨酯 热熔胶的制备方法， 包括如下步骤：
( 1 )将聚醚多元醇 4000E、 聚酯多元醇 3000H、 聚酯多元醇 2000N、 抗氧 剂搅拌混合， 加热升温至 120。C左右， 在真空度小于 lOOPa下， 脱水 0.5h;
( 2 )加入增粘树脂， 继续升温至 135-140。C, 在真空度小于 lOOPa下， 脱 水 1.5h;
( 3 ) 降温至 87。C, 加入 MDI、 催化剂， 搅拌， 在 85-95。C、 真空度小于 lOOPa条件下反应 2h;
( 4 )解除真空， 加入白炭黑， 快速搅拌， 混勾， 在真空度小于 lOOPa下 继续搅拌 lOmin;
( 5 )保持温度在 85-100。C, 快速出料、 封装， 然后在 80-85。C的烘箱中 熟化 4h, 得标的产品；
所述的聚酯多元醇 3000H是分子量为 3000 的聚己二酸 -1,6 己二醇酯二 醇， 所述的聚酯多元醇 2000N是分子量为 2000的聚己二酸新戊二醇酯二醇； 所述的增粘树脂为丙烯酸树脂； 所述的聚醚多元醇 4000E是分子量为 4000的 聚氧化丙烯二醇； 所述抗氧剂为抗氧剂 1010和抗氧剂 1076的混合物； 所述 MDI为 4,4'-二苯基曱烷二异氰酸酯；
以 100份质量产品计， 所述各物质的质量份数分别为： MDI为 11-13份， 聚醚多元醇 4000E 为 37 - 51份， 聚酯多元醇 3000H为 8 -13份， 聚酯多元醇 2000N为 8 - 13份， 抗氧剂 1010为 0.22份， 抗氧剂 1076为 0.22份， 增粘树 脂为 19 - 20份， 催化剂为 0.14份， 白炭黑为 0.5份。
根据一较佳实施例， 所述的催化剂为辛酸亚锡和双 (2 , 2-吗啉乙基)醚的 混合物， 两者的质量比为 1 : 1。
与现有技术相比， 本发明制备的湿固化反应型聚氨酯热熔胶主要优势在 于， 由于为湿固化反应型粘接原理， 使得本发明制备的湿固化反应型聚氨酯 热熔胶不仅具有传统热塑性热熔胶快速粘接定位、 提供较高的初粘强度优点， 也能进一步固化交联， 使胶层的粘接力、 内聚强度等都能得到明显的提高； 釆用聚醚多元醇和聚酯多元醇的混合多元醇原料， 这样使得本发明制备的湿 固化反应型聚氨酯热熔胶兼有聚醚型湿固化反应型聚氨酯热熔胶和聚酯型湿 固化反应性聚氨酯热熔胶两者的优点——熔体粘度稳定性好、 耐水性好、 成 本低、 初粘和终粘强度好、 柔韧性较好。 本发明制备的湿固化反应型聚氨酯 热熔胶， 应用于纺织品复合中， 平均剥离强度为 20N/2.5cm (克重为 15g/cm ) 左右， 耐水解性能较好， 具体结果见表 1 , 从而达到纺织品复合行业对湿固化 反应型聚氨酯热熔胶的要求。
具体实施方式
下面通过实施例对本发明进一步阐述， 但并不限制本发明。 实施例 1
( 1 )将 51g聚醚多元醇 4000E, 8g聚酯多元醇 3000H、 8g聚酯多元醇 2000N, 0.22g抗氧剂 1010和 0.22g抗氧剂 1076放入三口烧瓶中搅拌混合并 加热升温至 120。C左右， 在真空度小于 lOOPa下， 脱水 0.5h;
(2)将 20g增粘树脂加入上述烧瓶中， 继续升温至 135-140。C, 在真空 度小于 lOOPa下， 脱水 1.5h;
(3) 降温至 87。C, 加入 12g 4,4，-二苯基曱烷二异氰酸酯（MDI)、 0.07g 辛酸亚锡和 0.07g双（2,2-吗啉乙基） 醚（DMDEE), 搅拌， 在 85-95。C、 真 空度小于 lOOPa下反应 2h;
(4)解除真空，加入 0.5g白炭黑，快速搅拌， 混匀 ,在真空度小于 lOOPa 下继续搅拌 lOmin;
(5)保持出料温度在 85-100。C, 快速出料， 氮气保护封装于铝箔袋中后 在 80-85。C的烘箱中熟化 4h, 得产品 A。
实施例 2
(1)将 46g聚醚多元醇 4000E, 10g聚酯多元醇 3000H、 10g聚酯多元醇 2000N, 0.22g抗氧剂 1010和 0.22g抗氧剂 1076放入三口烧瓶中搅拌混合并 加热升温至 120。C左右， 在真空度小于 lOOPa下， 脱水 0.5h;
(2)将 19g增粘树脂加入上述烧瓶中， 继续升温至 135-140。C, 在真空 度小于 lOOPa下， 脱水 1.5h;
( 3 )降温至 87。C, 加入 12g MDL 0.07g辛酸亚锡和 0.07g DMDEE, 搅 拌， 在 85-95。C、 真空度小于 lOOPa下反应 2h;
(4)解除真空,加入 0.5g白炭黑，快速搅拌， 混匀,在真空度小于 lOOPa 下继续搅拌 lOmin;
(5)保持出料温度在 85-100。C, 快速出料， 氮气保护封装于铝箔袋中后 在 80-85。C的烘箱中熟化 4h , 得产品 B。
实施例 3
( 1 )将 44g聚醚多元醇 4000E, llg聚酯多元醇 3000H、 llg聚酯多元醇 2000N, 0.22g抗氧剂 1010和 0.22g抗氧剂 1076放入三口烧瓶中搅拌混合并 加热升温至 120。C左右， 在真空度小于 lOOPa下， 脱水 0.5h;
( 2 )将 19g增粘树脂加入上述烧瓶中， 继续升温至 135-140。C, 在真空 度小于 lOOPa下， 脱水 1.5h;
( 3 ) 降温至 87。C, 加入 llg MDI、 0.07g辛酸亚锡和 0.07g DMDEE, 搅 拌， 在 85-95。C、 真空度小于 lOOPa下反应 2h;
( 4 )解除真空,加入 0.5g白炭黑，快速搅拌， 混匀,在真空度小于 lOOPa 下继续搅拌 lOmin;
( 5 )保持出料温度在 85-100。C, 快速出料， 氮气保护封装于铝箔袋中后 在 80-85。C的烘箱中熟化 4h, 得产品 C。
实施例 4
( 1 )将 37g聚醚多元醇 4000E, 13g聚酯多元醇 3000H、 13g聚酯多元醇 2000N, 0.22g抗氧剂 1010和 0.22g抗氧剂 1076放入三口烧瓶中搅拌混合并 加热升温至 120。C左右， 在真空度小于 lOOPa下， 脱水 0.5h;
( 2 )将 19g增粘树脂加入上述烧瓶中， 继续升温至 135-140。C, 在真空 度小于 lOOPa下， 脱水 1.5h;
( 3 )降温至 87。C, 加入 13g MDI、 0.07g辛酸亚锡和 0.07g DMDEE, 搅 拌， 在 85-95。C、 真空度小于 lOOPa下反应 2h;
( 4 )解除真空,加入 0.5g白炭黑，快速搅拌， 混匀,在真空度小于 lOOPa 下继续搅拌 lOmin;
( 5 )保持出料温度在 85-100。C, 快速出料， 氮气保护封装于铝箔袋中后 在 80-85 C的烘箱中熟化 4h, 得产品 D 应用实施例
上述的实施例 1-4所得的纺织品复合用湿固化反应型聚氨酯热熔胶 A、纺 织品复合用湿固化反应型聚氨酯热熔胶 B、 纺织品复合用湿固化反应型聚氨 酯热熔胶。、 纺织品复合用湿固化反应型聚氨酯热熔胶 D的技术参数见表 1 , 纺织品复合用湿固化反应型聚氨酯热熔胶 A B C D在纺织品复合中的应 用， 其应用方法包括如下步骤：
分别将上述实施例 1-4 所得的纺织品复合用湿固化反应型聚氨酯热熔胶 产品 A B C D在 120°C的温度下进行加热然后用 0.45μπι孔径的圓网进 行涂布， 对涤棉进行复合， 然后将涂布后的涤棉布料在 80 C 3kgf/cm2压力 下进行烫压， 至于 20 C、 湿度 70%的恒温恒湿环境中放置 24h。 然后将布料 剪成宽 2.5cm、 长 20cm的布条， 检测其克重（单位面积布料所含胶的质量）， 测试其剥离强度， 经泡水后再测试其剥离强度， 具体结果见表 1 纺织品复合用湿固化反应型聚氨酯热熔胶的技术参数及应用玻璃强度试验结果 产 120oC黏度 克重 剥离强度 泡水后的剥离强度 (N/2.5c 00m)
(mPa-s) (g/m2) (N/2.5cm) 1天 2天 3天
A 5675 30.2 18.59 17.63 17.34 17.22
B 4650 15.8 19.92 18.16
Figure imgf000007_0001
D 4767 28.3 20.98 17.96 从表 1 中的数据可以看出本发明提供的纺织品复合用湿固化反应型聚氨 酯热熔胶在 120 C下的黏度为 5000mPa · s左右， 用于纺织品复合中， 不易渗 胶， 易涂布， 15g/m2的克重下玻璃强度为 19.92 N/2.5cm, 且经水洗后玻璃强 度下降不大， 表明其玻璃强度好、 耐水解性能优良。 本发明提供的纺织品复 合用湿固化反应型聚氨酯热熔胶 A B C D耐水解性能依次下降， 但是其 耐水解性能依然很好，产品 B在的剥离强度最好（单位克重的玻璃强度最大）， 黏度适中， 故优选产品 B的实施例 2为最佳实施例， 产品 B的配方为最佳配 方。
以上所述内容仅为本发明构思下的基本说明， 而依据本发明的技术方案 所作的任何等效变换， 均应属于本发明的保护范围。

Claims

权利要求
1、 一种纺织品用湿固化反应型聚氨酯热熔胶的制备方法， 其特征在于， 包括如下步骤：
( 1 )将聚醚多元醇 4000E、 聚酯多元醇 3000H、 聚酯多元醇 2000N、 抗氧 剂搅拌混合， 加热升温至 120。C左右， 在真空度小于 lOOPa下， 脱水 0.5h;
( 2 )加入增粘树脂， 继续升温至 135-140。C, 在真空度小于 lOOPa下， 脱 水 1.5h;
( 3 ) 降温至 87。C, 加入 MDI、 催化剂， 搅拌， 在 85-95。C、 真空度小于 lOOPa条件下反应 2h;
( 4 )解除真空， 加入白炭黑， 快速搅拌， 混勾， 在真空度小于 lOOPa下 继续搅拌 lOmin;
( 5 )保持温度在 85-100。C, 快速出料、 封装， 然后在 80-85。C的烘箱中 熟化 4h, 得标的产品；
所述的聚酯多元醇 3000H是分子量为 3000的聚己二酸 -1,6己二醇酯二醇， 所述的聚酯多元醇 2000N是分子量为 2000的聚己二酸新戊二醇酯二醇；所述 的增粘树脂为丙烯酸树脂； 所述的聚醚多元醇 4000E是分子量为 4000的聚氧 化丙烯二醇； 所述抗氧剂为抗氧剂 1010和抗氧剂 1076的混合物； 所述 MDI 为 4,4'-二苯基曱烷二异氰酸酯；
以 100份质量产品计， 所述各物质的质量份数分别为： MDI为 11-13份， 聚醚多元醇 4000E 为 37 - 51份， 聚酯多元醇 3000H为 8 -13份， 聚酯多元醇 2000N为 8 - 13份， 抗氧剂 1010为 0.22份， 抗氧剂 1076为 0.22份， 增粘树 脂为 19 - 20份， 催化剂为 0.14份， 白炭黑为 0.5份。
2、 如权利要求 1所述的方法， 其特征在于： 所述的催化剂为辛酸亚锡和 双 (2, 2-吗啉乙基)醚的混合物， 两者的质量比为 1: 1。
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