WO2015039615A1 - 一种阻燃聚氨酯泡沫体及其制备方法 - Google Patents

一种阻燃聚氨酯泡沫体及其制备方法 Download PDF

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WO2015039615A1
WO2015039615A1 PCT/CN2014/086832 CN2014086832W WO2015039615A1 WO 2015039615 A1 WO2015039615 A1 WO 2015039615A1 CN 2014086832 W CN2014086832 W CN 2014086832W WO 2015039615 A1 WO2015039615 A1 WO 2015039615A1
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parts
polyurethane foam
flame
flame retardant
catalyst
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PCT/CN2014/086832
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English (en)
French (fr)
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秦升益
张雪芳
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北京仁创科技集团有限公司
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Publication of WO2015039615A1 publication Critical patent/WO2015039615A1/zh

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    • C—CHEMISTRY; METALLURGY
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • 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
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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
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0014—Use of organic additives
    • C08J9/0038—Use of organic additives containing phosphorus
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0066—Use of inorganic compounding ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/125—Water, e.g. hydrated salts
    • 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
    • C08K3/34—Silicon-containing compounds
    • 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
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/51—Phosphorus bound to oxygen
    • C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
    • C08K5/5317—Phosphonic compounds, e.g. R—P(:O)(OR')2
    • C08K5/5333—Esters of phosphonic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
    • 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
    • C08G2101/00—Manufacture of cellular products
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
    • C08J2201/022—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments premixing or pre-blending a part of the components of a foamable composition, e.g. premixing the polyol with the blowing agent, surfactant and catalyst and only adding the isocyanate at the time of foaming
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/10—Water or water-releasing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • C08J2375/06—Polyurethanes from polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • C08J2375/08—Polyurethanes from polyethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
    • C08J2483/10—Block- or graft-copolymers containing polysiloxane sequences
    • C08J2483/12—Block- or graft-copolymers containing polysiloxane sequences containing polyether sequences

Definitions

  • the invention relates to a flame-retardant polyurethane foam and a preparation method thereof, in particular to adding graphite on the basis of water glass foamed polyurethane to improve flame retardancy and a preparation method thereof.
  • the polyurethane foam is a body made of a resin based on chemical or physical methods to produce numerous small pores in the interior thereof. According to its application, it is divided into soft foam, hard foam and semi-rigid foam.
  • Ordinary polyurethane is a combustible material. It burns and decomposes in the fire to produce a large amount of toxic fumes, which brings difficulties to fire extinguishing.
  • polyurethane soft foam has a high opening ratio, many combustible components, and is flammable and difficult to self-extinguish.
  • the application fields of polyurethane foams such as building materials, mattresses, furniture, thermal insulation materials, automobile seat cushions and interior materials all have flame retardant requirements. Therefore, many enterprises have adopted flame retardant polyurethane foam.
  • the traditional flame retardant method is to achieve flame retardant effect by adding a flame retardant in the raw material, or to improve flame retardancy by introducing a flame retardant group into the polyether polyol, but the effect is not satisfactory, and the oxygen index does not exceed "27. ".
  • the present invention proposes a new polyurethane foam formulation.
  • the new polyurethane foam has an oxygen index of up to "35" and its color changes from a conventional pale yellow to a black color, and is more suitable for use in the fields of building materials, furniture, thermal insulation materials, automobile seat cushions and interiors.
  • a flame-retardant polyurethane foam prepared by foaming black and white materials according to a mass ratio of 1:1.2-1.4;
  • the black material is an isocyanate, preferably one or more of tolylene diisocyanate (TDI), diphenylmethane diisocyanate (MDI), and polymethylene polyphenyl polyisocyanate (PAPI); further preferably, multi-Asia Methyl polyphenyl polyisocyanate (PAPI);
  • TDI tolylene diisocyanate
  • MDI diphenylmethane diisocyanate
  • PAPI polymethylene polyphenyl polyisocyanate
  • PAPI multi-Asia Methyl polyphenyl polyisocyanate
  • the white material is composed of the following components by weight: 5-15 parts of water glass, 40-55 parts of polyether polyol, 40-60 parts of polyester polyol, 0.1-0.5 parts of catalyst, foam stabilizer 2-5 Parts, 5-15 parts of halogen-free flame retardant, 5-15 parts of graphite flame retardant.
  • the invention effectively improves the flame retardant performance of the polyurethane foam by selecting the components of the polyurethane foam and adjusting the proportion of the polyurethane foam.
  • water glass is selected from the group consisting of sodium water glass or potassium water glass;
  • the polyether polyol of the present invention is selected from one or more of a polyoxypropylene polyol, a polytetrahydrofuran polyol, a tetrahydrofuran-propylene oxide copolyol or a special polyether polyol; wherein the special polyether is polyether
  • the alcohol is a mixture of polyether 4110 and polyether 403 in a mass ratio of 30-50:10-20; preferably 35:15.
  • polyester polyol of the present invention is selected from one or more selected from the group consisting of aliphatic polyester polyols, aromatic polyester polyols, and alicyclic polyester polyols; polyester polyol 400A is preferred.
  • the catalyst of the present invention is selected from the group consisting of an amine catalyst and/or an organotin catalyst;
  • the amine catalyst is selected from one or more of an aliphatic amine catalyst, an alicyclic amine catalyst, an alcohol amine catalyst or an aromatic amine catalyst;
  • the aliphatic amine catalyst is selected from the group consisting of N,N-dimethylcyclohexylamine, bis(2-dimethylaminoethyl)ether, N,N,N',N'-tetramethylalkylene
  • a diamine, triethylamine, triethylenediamine or N,N-dimethylbenzylamine is selected from the group consisting of N,N-dimethylcyclohexylamine, bis(2-dimethylaminoethyl)ether, N,N,N',N'-tetramethylalkylene
  • a diamine triethylamine, triethylenediamine or N,N-dimethylbenzylamine
  • the alicyclic amine catalyst is one or more selected from the group consisting of a fixed amine, N-ethylmorpholine, methylmorpholine (NMM) or N,N'-diethylpiperazine;
  • the alcohol amine catalyst is selected from the group consisting of triethanolamine and/or N,N-dimethylethanolamine (DMEA);
  • aromatic amines are selected from the group consisting of pyridine and/or N,N-lutidine;
  • the organotin catalyst is selected from one or more of dibutyltin dilaurate, stannous octoate, dibutyltin dodecylsulfate or dibutyltin diacetate;
  • catalysts are dibutyltin dilaurate and triethylenediamine.
  • the foam stabilizer is a silicone foam stabilizer, preferably a foam stabilizer AK-8805;
  • the halogen-free flame retardant is an organophosphorus flame retardant, preferably dimethyl methylphosphonate (DMMP);
  • the graphite flame retardant is one of micron-sized graphite powder, expandable graphite or graphite milk.
  • the raw materials mentioned in the present invention are all commercially available.
  • the white material is composed of the following components by weight: 8-12 parts of water glass, 40-50 parts of polyether polyol, 40-50 parts of polyester polyol, catalyst 0.2. - 0.4 parts, 2-4 parts of foam stabilizer, 8-12 parts of halogen-free flame retardant, and 8-12 parts of graphite flame retardant.
  • the white material is composed of the following components by weight: 10 parts of water glass, 45-55 parts of polyether polyol, 50 parts of polyester polyol, and 0.2-0.4 parts of catalyst. 3 parts of foam stabilizer, 10 parts of halogen-free flame retardant and 10 parts of graphite flame retardant.
  • the white material is composed of the following components by weight: 10 parts of water glass, 50-55 parts of polyether polyol, 50 parts of polyester polyol, 0.2 parts of catalyst, and foam stability. 3 parts, 10 parts of halogen-free flame retardant, 10 parts of graphite flame retardant.
  • the flame-retardant polyurethane foam prepared by foaming the black material and the white material according to the mass ratio of 1:1.1-1.2 also has good comprehensive performance.
  • the invention also provides a preparation method of the above polyurethane foam, which is obtained by uniformly mixing water glass, polyether polyol, polyester polyol, catalyst, foam stabilizer, halogen-free flame retardant and graphite flame retardant at room temperature.
  • Polyether system that is, white material;
  • the black material and the white material are mixed according to the mass ratio (for example, 1:1.2-1.4 or 1:1.1-1.2), and after being fully stirred, they are poured into a mold to be foamed, matured, and demolded to obtain a polyurethane foam.
  • the group distribution ratio of the white material is the same as described above; the black material component is selected as described above.
  • the stirring time is 5-20 s; the stirring speed is 1200-1800 r/min.
  • the preparation method of the present invention at 10-25 ° C, First, water glass, polyether polyol, polyester polyol, catalyst, foam stabilizer, halogen-free flame retardant, graphite flame retardant are mixed to obtain a polyether system, which is white material; then black material and white material After mixing by mass ratio (such as 1:1.2-1.4 or 1:1.1-1.2), stirring at 1500r/min for 10s, the mixture is poured into a mold, foamed, matured, and demolded to obtain a polyurethane foam;
  • each component of the white material is as follows: 10 parts of water glass, 45-55 parts of polyether polyol, 50 parts of polyester polyol, 0.2-0.4 parts of catalyst, 3 parts of foam stabilizer, halogen-free flame retardant 10 parts of the agent, 10 parts of the graphite flame retardant.
  • the invention adopts water glass instead of the traditional chlorofluorocarbon foaming agent in the existing polyurethane foam formulation, which can effectively reduce environmental pollution; at the same time, the water glass cooperates with the halogen-free flame retardant and the graphite flame retardant to improve the flame retardancy of the polyurethane foam.
  • Sex the oxygen index is as high as "35”.
  • the polyurethane foam changes from the traditional light yellow to black, which breaks the traditional color from the appearance, and is more suitable for building materials, furniture, thermal insulation materials, car seats. Pads and interiors.
  • dibutyl dilaurate and triethylene diamine are placed in a container and mechanically stirred for 20-30 minutes to form a uniform polyether system, which is a white material;
  • the white material and the black material are mixed and reacted at room temperature, stirred at 1500 r/min for 10 s, and then poured into a constant temperature vertical climbing mold to be foamed and solidified. After the foam body is matured, it is taken out from the mold to obtain a polyurethane foam.
  • Example 7 A method for preparing a polyurethane foam
  • the polyurethane foam of Example 2 was prepared according to the method described in Example 6, except that the stirring time was 5 s; the stirring speed was 1800 r/min.
  • Example 8 A method for preparing a polyurethane foam
  • the polyurethane foam of Example 3 was prepared according to the method described in Example 6, except that the stirring time was 20 s; the stirring speed was 1200 r/min.
  • the polyurethane foam of Example 4 was prepared according to the method described in Example 6, except that the stirring time was 15 s; the stirring speed was 1400 r/min.
  • a polyurethane foam was prepared in accordance with the method of Example 6, and its specific formulation is shown in Table 1.
  • a polyurethane foam compared with the first embodiment, differs only in:
  • the polyether polyol is replaced by a mixture obtained by mixing a polyoxypropylene polyol and a polytetrahydrofuran polyol in a mass ratio of 2:1;
  • a polyurethane foam compared with the first embodiment, differs only in:
  • the catalyst was replaced by a mixture of triethanolamine and N,N-dimethylpyridine in a mass ratio of 1:1.
  • the oxygen index of the comparative example was only 27, and the oxygen index of the polyurethane foam obtained in Example 1-5 was greatly improved, and the flame retarding effect was remarkable. Further, the properties of the polyurethane foams obtained in Examples 10 and 11 were tested, which were substantially consistent with the properties of the polyurethane foams described in Examples 1-5 in terms of density, thermal conductivity, dimensional change rate, compressive strength, and oxygen index. .
  • the invention adopts water glass instead of the traditional chlorofluorocarbon foaming agent, which can effectively reduce environmental pollution; at the same time, the water glass cooperates with the halogen-free flame retardant and the graphite flame retardant to improve the flame retardancy of the polyurethane foam and make the oxygen index as high as “ 35", after adding graphite flame retardant, the polyurethane foam changes from the traditional light yellow to black, which breaks the traditional color from the appearance, and is more suitable for the fields of building materials, furniture, thermal insulation materials, car seat cushions and interiors.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Polyurethanes Or Polyureas (AREA)

Abstract

本发明涉及一种阻燃聚氨酯泡沫体，是由黑料和白料按照质量比1:1.2-1.4发泡制备而得；所述黑料为异氰酸酯类；所述白料由如下重量份的组分组成：水玻璃5-15份；聚醚多元醇40-55份；聚酯多元醇40-60份；催化剂0.1-0.5份；泡沫稳定剂2-5份；无卤阻燃剂5-15份；石墨阻燃剂5-15份。本发明还提供上述阻燃聚氨酯泡沫体的制备方法。

Description

一种阻燃聚氨酯泡沫体及其制备方法 技术领域
本发明涉及一种阻燃聚氨酯泡沫体及其制备方法，具体涉及在水玻璃发泡聚氨酯的基础上加入石墨提高阻燃性及其制备方法。
背景技术
聚氨酯泡沫体是以树脂为基础，采用化学或物理方法在其内部产生无数小气孔而制成的体。根据其应用，分为软泡、硬泡、半硬泡。
普通聚氨酯是可燃物，遇火燃烧分解产生大量有毒烟雾，给灭火带来困难，特别是聚氨酯软泡开孔率较高，可燃成分多，易燃且不易自熄。但是目前聚氨酯泡沫体的应用领域如建筑材料，床垫，家具，保温材料，汽车座垫及内饰材料等，都有阻燃要求，因此，已有很多企业已经采用阻燃级聚氨酯泡沫。
传统的阻燃方法是在原料中通过加入阻燃剂达到阻燃效果，或通过在聚醚多元醇中引入阻燃基团提高阻燃性，但是效果并不理想，氧指数都不超过“27”。
发明内容
为了进一步提高阻燃效果，本发明提出一种新的聚氨酯泡沫体配方。所述新的聚氨酯泡沫体的氧指数高达“35”，并且其颜色由传统的淡黄色变成黑色，更适宜应用到建筑材料、家具、保温材料、汽车座垫及内饰等领域。
为了达到上述目的，本发明采用如下技术方案：
一种阻燃聚氨酯泡沫体，由黑料和白料按照质量比1：1.2-1.4发泡制备而得；
所述黑料为异氰酸酯类，优选甲苯二异氰酸酯(TDI)、二苯基甲烷二异氰酸酯(MDI)、多亚甲基多苯基多异氰酸酯(PAPI)中一种或两种以上；进一步优选多亚甲基多苯基多异氰酸酯(PAPI)；
所述白料由如下重量份的组分组成：水玻璃5-15份，聚醚多元醇40-55份，聚酯多元醇40-60份，催化剂0.1-0.5份，泡沫稳定剂2-5份，无卤阻燃剂5-15份，石墨阻燃剂5-15份。
本发明通过对聚氨酯泡沫体组分的选择和用量比例的调整，有效进一步提高聚氨酯泡沫体的阻燃性能。
其中，所述水玻璃选自钠水玻璃或钾水玻璃；
本发明所述聚醚多元醇选自聚氧化丙烯多元醇、聚四氢呋喃多元醇、四氢呋喃-氧化丙烯共聚多元醇或特种聚醚多元醇中一种或两种以上；其中，所述特种聚醚多元醇由聚醚4110与聚醚403按质量比30-50：10-20混合而成；优选35：15。
本发明所述聚酯多元醇选自脂肪族聚酯多元醇、芳香族聚酯多元醇或脂环族聚酯多元醇中的一种或两种以上；优选聚酯多元醇400A。
本发明所述催化剂选自胺类催化剂和/或有机锡催化剂；
其中，所述胺类催化剂选自脂肪族胺类催化剂、脂环族胺类催化剂、醇胺类催化剂或芳香族胺类催化剂中的一种或两种以上；
其中，所述脂肪族胺类催化剂选自N,N-二甲基环已胺、双(2-二甲氨基乙基)醚、N,N,N’,N’-四甲基亚烷基二胺、三乙胺、三乙烯二胺或N,N-二甲基苄胺中的一种或两种以上；
其中，所述脂环族胺类催化剂选自固胺、N-乙基吗啉、甲基吗啉(NMM)或N,N’-二乙基哌嗪中的一种或两种以上；
所述醇胺类催化剂选自三乙醇胺和/或N,N-二甲基乙醇胺(DMEA)；
所述芳香族胺类选自吡啶和/或N,N-二甲基吡啶；
所述有机锡催化剂选自二丁基锡二月桂酸锡、辛酸亚锡、二(十二烷基硫)二丁基锡或二醋酸二丁基锡中的一种或两种以上；
所述催化剂中最优选二丁基锡二月桂酸锡和三乙烯二胺。
所述泡沫稳定剂为有机硅泡沫稳定剂，优选泡沫稳定剂 AK-8805；
所述无卤阻燃剂为有机磷系阻燃剂，优选甲基膦酸二甲酯(DMMP)；
所述石墨阻燃剂为微米级石墨粉、可膨胀石墨或石墨乳中的一种。
本发明中所提及的原料均为市售采购。
作为本发明的一种优选实施方式，所述白料由如下重量份的组分组成：水玻璃8-12份，聚醚多元醇40-50份，聚酯多元醇40-50份，催化剂0.2-0.4份，泡沫稳定剂2-4份，无卤阻燃剂8-12份，石墨阻燃剂8-12份。
作为本发明的一种优选实施方式，所述白料由如下重量份的组分组成：水玻璃10份，聚醚多元醇45-55份，聚酯多元醇50份，催化剂0.2-0.4份，泡沫稳定剂3份，无卤阻燃剂10份，石墨阻燃剂10份。
作为本发明的一种优选实施方式，所述白料由如下重量份的组分组成：水玻璃10份，聚醚多元醇50-55份，聚酯多元醇50份，催化剂0.2份，泡沫稳定剂3份，无卤阻燃剂10份，石墨阻燃剂10份。
在本发明技术方案中，由黑料和白料按照质量比1：1.1-1.2发泡制备得到的阻燃聚氨酯泡沫体同样具有良好的综合性能。
本发明还提供上述聚氨酯泡沫体的制备方法，在室温下，先将水玻璃、聚醚多元醇、聚酯多元醇、催化剂、泡沫稳定剂、无卤阻燃剂、石墨阻燃剂混合均匀得到聚醚体系，即为白料；
再将黑料和白料按照质量比(如1:1.2-1.4或1:1.1-1.2)混合，充分搅拌后，倒入模具中发泡、熟化，脱模，得到聚氨酯泡沫体。
其中，所述白料中组分配比同上所述；所述黑料组分选择同上所述。
所述的搅拌时间5-20s；搅拌速度1200-1800r/min。
作为本发明制备方法的一个优选实施方式，在10-25℃条件下， 先将水玻璃、聚醚多元醇、聚酯多元醇、催化剂、泡沫稳定剂、无卤阻燃剂、石墨阻燃剂混合均匀得到聚醚体系，即为白料；再将黑料与白料按质量比(如1:1.2-1.4或1:1.1-1.2)混合后，转速1500r/min搅拌10s后，将混合物倒入模具中发泡、熟化，脱模，得到聚氨酯泡沫体；
其中，所述白料各组分重量比如下：水玻璃10份，聚醚多元醇45-55份，聚酯多元醇50份，催化剂0.2-0.4份，泡沫稳定剂3份，无卤阻燃剂10份，石墨阻燃剂10份。
本发明在现有聚氨酯泡沫配方中采用水玻璃替代传统氟氯烃发泡剂，可有效减少环境污染；同时水玻璃与无卤阻燃剂、石墨阻燃剂共同作用，提高聚氨酯泡沫的阻燃性，使氧指数高达“35”，加入石墨阻燃剂后聚氨酯泡沫由传统的淡黄色变成黑色，从外观上打破传统颜色的束缚，更适宜应用到建筑材料、家具、保温材料、汽车座垫及内饰等领域。
具体实施方式
以下实施例用于说明本发明，但不用来限制本发明的范围。
实施例1-5 一种聚氨酯发泡体
实施例1-5聚氨酯发泡体的具体配方见表1。
表1 聚氨酯泡沫体的配方(单位：kg)
Figure PCTCN2014086832-appb-000001
Figure PCTCN2014086832-appb-000002
实施例6 一种聚氨酯发泡体的制备方法
制备实施例1所述聚氨酯发泡体的方法：
常温下，按表1中实施例1所述用量将聚醚多元醇4110、聚醚多元醇403、聚酯多元醇400A、钠水玻璃、阻燃剂DMMP、石墨乳、泡沫稳定剂AK-8805、二丁基二月桂酸锡、三乙烯二胺置于容器中机械混合搅拌20-30min，形成均匀的聚醚体系，即为白料；
再将白料与黑料在室温下混合反应，1500r/min下搅拌10s后倒入恒温垂直爬升模具中发泡固化，待泡体熟化后，将其从模具中取出，得到聚氨酯泡沫体。
按照国标要求进行式样切割，测定泡体各项性能，见表2。
实施例7 一种聚氨酯发泡体的制备方法
按照实施例6所述方法制备实施例2所述聚氨酯泡沫体，区别在于，所述的搅拌时间5s；搅拌速度1800r/min。
实施例8 一种聚氨酯发泡体的制备方法
按照实施例6所述方法制备实施例3所述聚氨酯泡沫体，区别在于，所述的搅拌时间20s；搅拌速度1200r/min。
实施例9 一种聚氨酯发泡体的制备方法
按照实施例6所述方法制备实施例4所述聚氨酯泡沫体，区别在于，所述的搅拌时间15s；搅拌速度1400r/min。
对比例
按照实施例6的方法制备聚氨酯泡沫体，其具体配方见表1。
实施例10
一种聚氨酯发泡体，与实施例1相比，区别点仅在于：
1)黑料替换为甲苯二异氰酸酯；
2)聚醚多元醇替换为由聚氧化丙烯多元醇与聚四氢呋喃多元醇以质量比2:1混合得到的混合物；
3)聚酯多元醇替换为脂肪族聚酯多元醇；
4)催化剂替换为N-乙基吗啉。
实施例11
一种聚氨酯发泡体，与实施例1相比，区别点仅在于：
1)黑料替换为二苯基甲烷二异氰酸酯；
2)聚醚多元醇替换为四氢呋喃-氧化丙烯共聚多元醇；
3)聚酯多元醇替换为脂环族聚酯多元醇；
4)催化剂替换为由三乙醇胺和N,N-二甲基吡啶以质量比1:1的混合物。
效果验证
对实施例1-5及对比例所述的聚氨酯泡沫体进行性能检测，其结果见表2。
表2 聚氨酯泡沫体的性能测试
Figure PCTCN2014086832-appb-000003
Figure PCTCN2014086832-appb-000004
由表2可知，对比例的氧指数仅为27，而实施例1-5所得聚氨酯泡沫体氧指数大幅度提高，阻燃效果显著。此外，对实施例10、11所得聚氨酯泡沫体的性能进行测试，其在密度、导热系数、尺寸变化率、抗压强度、氧指数方面与实施例1-5所述聚氨酯泡沫体的性能基本一致。
以上的实施例仅仅是对本发明的优选实施方式进行描述，并非对本发明的范围进行限定，在不脱离本发明设计精神的前提下，本领域普通工程技术人员对本发明的技术方案作出的各种变型和改进，均应落入本发明的权利要求书确定的保护范围内。
工业实用性
本发明采用水玻璃替代传统氟氯烃发泡剂，可有效减少环境污染；同时水玻璃与无卤阻燃剂、石墨阻燃剂共同作用，提高聚氨酯泡沫的阻燃性，使氧指数高达“35”，加入石墨阻燃剂后聚氨酯泡沫由传统的淡黄色变成黑色，从外观上打破传统颜色的束缚，更适宜应用到建筑材料、家具、保温材料、汽车座垫及内饰等领域。

Claims (12)

  1. 一种阻燃聚氨酯泡沫体，其特征在于，由黑料和白料按照质量比1:1.2-1.4发泡制备而得；其中，
    所述黑料为异氰酸酯类；
    所述白料由如下重量份的组分组成：水玻璃5-15份；聚醚多元醇40-55份；聚酯多元醇40-60份；催化剂0.1-0.5份；泡沫稳定剂2-5份；无卤阻燃剂5-15份；石墨阻燃剂5-15份；
    所述异氰酸酯类优选选自甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、多亚甲基多苯基多异氰酸酯中一种或两种以上；进一步优选多亚甲基多苯基多异氰酸酯。
  2. 根据权利要求1所述的阻燃聚氨酯泡沫体，其特征在于，所述白料由如下重量份的组分组成：水玻璃8-12份；聚醚多元醇40-50份；聚酯多元醇40-50份；催化剂0.2-0.4份；泡沫稳定剂2-4份；无卤阻燃剂8-12份；石墨阻燃剂8-12份。
  3. 根据权利要求1所述的阻燃聚氨酯泡沫体，其特征在于，所述水玻璃选自钠水玻璃或钾水玻璃中的一种。
  4. 根据权利要求1所述的阻燃聚氨酯泡沫体，其特征在于，所述石墨阻燃剂为微米级的石墨粉、可膨胀石墨或石墨乳中的一种；所述无卤阻燃剂为有机磷系阻燃剂。
  5. 根据权利要求1所述的阻燃聚氨酯泡沫体，其特征在于，所述聚醚多元醇选自聚氧化丙烯多元醇、聚四氢呋喃多元醇、四氢呋喃-氧化丙烯共聚多元醇或特种聚醚多元醇中一种或两种以上；
    其中，所述特种聚醚多元醇优选由聚醚4110与聚醚403按质量比30-50:10-20混合而成。
  6. 根据权利要求1所述的阻燃聚氨酯泡沫体，其特征在于，所述聚酯多元醇选自脂肪族聚酯多元醇、芳香族聚酯多元醇、或脂环族聚酯多元醇中的一种或两种以上。
  7. 根据权利要求1所述的阻燃聚氨酯泡沫体，其特征在于，所述催化剂选自胺类催化剂和/或有机锡催化剂；
    其中，胺类催化剂优选选自脂肪族胺类催化剂、脂环族胺类催化剂、醇胺类催化剂、芳香族胺类催化剂中的一种或两种以上；
    所述有机锡催化剂优选选自二丁基锡二月桂酸锡、辛酸亚锡、二(十二烷基硫)二丁基锡、二醋酸二丁基锡中的一种或两种以上。
  8. 根据权利要求1所述的阻燃聚氨酯泡沫体，其特征在于，所述泡沫稳定剂为有机硅泡沫稳定剂。
  9. 根据权利要求1所述的阻燃聚氨酯泡沫体，其特征在于，所述白料由如下重量份的组分组成：水玻璃10份，聚醚多元醇45-55份，聚酯多元醇50份，催化剂0.2-0.4份，泡沫稳定剂3份，无卤阻燃剂10份，石墨阻燃剂10份；
    或所述白料由如下重量份的组分组成：水玻璃10份，聚醚多元醇50-55份，聚酯多元醇50份，催化剂0.2份，泡沫稳定剂3份，无卤阻燃剂10份，石墨阻燃剂10份。
  10. 根据权利要求1所述的阻燃聚氨酯泡沫体，其特征在于，所述阻燃聚氨酯泡沫体由黑料和白料按照质量比1：1.1-1.2发泡制备得到。
  11. 权利要求1-10任一所述阻燃聚氨酯泡沫体的制备方法，其特征在于，在室温下，先将水玻璃、聚醚多元醇、聚酯多元醇、催化剂、泡沫稳定剂、无卤阻燃剂、石墨阻燃剂混合均匀得到聚醚体系，即为白料；再将黑料和白料按比例混合，充分搅拌后，倒入模具中发泡、熟化，脱模，得到聚氨酯泡沫体。
  12. 根据权利要求11所述的制备方法，其特征在于，所述的搅拌时间5-20s；搅拌速度1200-1800r/min。
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