CN112553913B - 一种含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物、制备方法和阻燃织物 - Google Patents
一种含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物、制备方法和阻燃织物 Download PDFInfo
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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
- D06N3/04—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
- D06N3/042—Acrylic polymers
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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
- D06N3/0056—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
- D06N3/0059—Organic ingredients with special effects, e.g. oil- or water-repellent, antimicrobial, flame-resistant, magnetic, bactericidal, odour-influencing agents; perfumes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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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
- D06N3/0061—Organic fillers or organic fibrous fillers, e.g. ground leather waste, wood bark, cork powder, vegetable flour; Other organic compounding ingredients; Post-treatment with organic compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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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
- D06N3/12—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
- D06N3/121—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 polyesters, polycarbonates, alkyds
- D06N3/123—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 polyesters, polycarbonates, alkyds with polyesters
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- D06N2209/00—Properties of the materials
- D06N2209/06—Properties of the materials having thermal properties
- D06N2209/067—Flame resistant, fire resistant
Abstract
本发明公开了一种含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物,所述组合物包含成膜剂、疏水改性乳液、溴化阻燃剂、含磷阻燃剂、超支化成碳剂、水性涂料助剂,所述的溴化阻燃剂为十溴二苯乙烷,所述含磷阻燃剂选自疏水改性包裹的聚磷酸铵,所述疏水改性乳液选自有机硅改性的丙烯酸聚酯乳液和聚氨酯改性的丙烯酸聚酯乳液。该阻燃涂层组合物耐水好,阻燃效果好。
Description
技术领域
本发明涉及一种含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物、其制备方法及用其制作的纺织品织物。
背景技术
纺织品是日常生活中不可或缺的一部分,例如,可以在窗帘、布料、家具和汽车内饰、玩具、包装材料以及其它众多应用中见到纺织品。有火灾事故调查表明:相当一部分的火灾是由纺织品及室内装饰品引起的。中国是世界上最大的纺织品制造商,2013年中国纺织品出口总额就达到2841亿美元。近一些年来,纺织品阻燃,特别是绿色环保新型阻燃纺织品已逐渐成为高层建筑、公共场所、大飞机和高铁等强制标准要求。我国GB20286—2006《公共场所阻燃制品及组件燃烧性能要求及标识》是强制性国家标,其中也包括了对纺织品阻燃要求。国际生态纺织品认证的《Oeko-Tex StandBrd 100通用及特别技术条件》和《Oeko-Tex StandBrd 200检测程序》也对应用到纺织品上的阻燃剂进行了严格的规定。
近年来,在纺织品领域,水性阻燃涂层胶在许多种织物上都实现了对溶剂型阻燃涂层胶的替代。相对于溶剂型阻燃涂层胶,水性阻燃涂层胶在应用中具有易于稀释、易于涂布、无燃烧爆炸危险、加工中VOC低、流变性易于调控、易于清洗等优点,也受到了市场的认可。水性阻燃涂层胶的兴起,符合国家节能减排、清洁生产的发展方向。
目前最常用最有效的阻燃涂层胶仍然是溴锑型体系。溴锑型阻燃体系在气相阻燃方面性能优异,性价比高,而广受欢迎。向溴化阻燃剂中加入锑,如最常用的氧化锑,实现溴锑协效可大幅提高阻燃体系的阻燃效率并减少阻燃剂的使用量。但是,锑,如氧化锑的安全性已经成为严重的安全环保问题,在一些应用中,氧化锑的使用正受到限制。欧盟EN71-3限制的八大重金属也包括锑。许多厂家还是不得不用氧化锑来协效,甚至为了降成本,采用砷和铅含量非常高的低纯度氧化锑。这些含砷和铅低纯度的氧化锑阻燃体系,很容易造成对生产涂层胶和应用涂层胶工人的接触伤害。同时,做成的纺织成品也很难满足中国及欧美各国关于重金属的标准。欧盟EN71-3测试可迁移重金属,要求砷不得超过25ppm,铅不得超过90ppm。美国CPSIA法案要求基材总铅不得超过l00ppm等等。因此,全世界都在试图找到有效的氧化锑替代品,但目前还没有取得商业上的成功。
膨胀型复合阻燃体系替代溴锑型阻燃剂也是近年来我国阻燃领域广为关注的新型复合阻燃剂。膨胀型复合阻燃剂采用酸源、碳源、气源协同增效阻燃,是阻燃领域又一经典的协效组合。膨胀型阻燃体系可以通过凝聚相阻燃实现高效成炭阻燃,在织物表面形成致密的多孔泡沫炭层。既可阻止内层高聚物的进一步降解及可燃物向表面的释放,又可阻止热源向高聚物的传递以及隔绝氧源,从而阻止火焰的蔓延和传播。膨胀型阻燃剂虽然具有无卤、低烟、低毒、防熔滴和无腐蚀性气体的优点,但在阻燃效率和耐水洗性能等方面还不如溴锑阻燃体系。
目前市场上急需一种集合或部分集合溴锑阻燃体系和磷氮阻燃体系优点并克服它们缺点,无重金属的纺织物阻燃涂层体系。
发明内容
本发明的目的是提供一种含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物,其原料组成按重量配比关系包括:
成膜剂15-40份,溴化阻燃剂10-30份,含磷阻燃剂10-30份,成炭剂3-15份,疏水改性乳液5-15份,分散乳化剂、增稠剂、抗冻剂、成膜助剂和pH调节剂组成的水性涂料助剂0.5-10份,水20-50份。
所述的成膜剂为乙烯-醋酸乙烯酯共聚乳液或丙烯酸聚酯共聚乳液或二者任意比例的混合物。
所述成炭剂为不溶于水的超支化成碳剂。
传统成炭剂大多是小分子结构,如季戊四醇、双季戊四醇等,季戊四醇(PER)是一种带有强极性的化合物,溶于水,在使用过程中耐水与耐久性差、易于迁移到基体表面,造成阻燃涂层胶性能劣化。因此,为了改善小分子成炭剂的缺点,本发明引进了一种具有大分子结构的超支化成炭剂。例如,超支化羟基聚酯成炭剂是由多个官能团单体通过聚合反应形成,它的分子量很大,含碳量也大,合成简单且可以实现工业化生产,成本明显低于其他大分子成炭剂,具有良好的成炭效果,并克服了普通成炭剂不耐水、易迁移的缺点,还有分解温度高、相容性好、不渗出和阻燃性能优良等优点,所以用它作为成炭剂具有很大的实用性。
本发明所述超支化成碳剂选自超支化的三嗪成炭剂或具有羟基官能团的、树枝状的、超支化的、3D结构的聚酯树脂或二者任意比例的混合物。
本发明所选用超支化三嗪成炭剂的化学结构如下(其合成方法采用申请公布号CN103333336 A专利的方法):
本发明所述具有羟基官能团的、树枝状的、超支化的、3D结构的聚酯树脂选自第一代超支化羟基聚酯(Boltorn H10)、第二代超支化羟基聚酯(Boltorn H20)、第三代超支化羟基聚酯(Boltorn H30)和第四代超支化羟基聚酯(Boltorn H40)中的一种或两种以上任意比例的混合。第一代超支化羟基聚酯(Boltorn H10)、第二代超支化羟基聚酯(BoltornH20)、第三代超支化羟基聚酯(Boltorn H30)和第四代超支化羟基聚酯(Boltorn H40)的化学结构分别如下(1)、(2)、(3)和(4)所示:
在纺织品水性阻燃涂层中,传统使用的大多数是水性丙烯酸乳液,其具有透明性、光泽度、初粘性、耐候性、低成本的优势,但其固有的缺点,如蠕变性大、耐高低温性差、高温易返粘等又限制了其应用。利用聚有机硅氧烷的独特性质,将其引入水性丙烯酸酯乳液体系中,从而制备兼具二者优异性能的硅丙乳液,可持续显著地改善水性丙烯酸乳液胶黏剂的湿态和干态粘接性能及贮存稳定性,提高水性丙烯酸乳液胶黏剂的撕裂强度和耐持久性,提高拉伸强度并同时保留伸长率性能,同时提高阻燃涂层胶的耐水性能。聚氨酯和聚丙烯酸酯两者在性能上具有很大的互补性,用聚氨酯进行改性后的水性丙烯酸树脂乳液,可以使聚氨酯的高耐磨性和良好的机械性能与丙烯酸良好的耐候型和耐水性两者有机地结合起来,增加水性丙烯酸树脂乳液在纺织品水性涂层中的适用性。本发明所述疏水改性乳液选自有机硅改性的丙烯酸聚酯乳液或聚氨酯改性的丙烯酸聚酯乳液或二者任意比例的混合物。
本发明所述的含磷阻燃剂为磷氮型膨胀型阻燃剂。
所述磷氮型膨胀型阻燃剂为疏水改性包裹的聚磷酸铵,选自蜜胺树脂包裹的改性聚磷酸铵、硅凝胶包裹的改性聚磷酸铵、聚氨酯包裹的改性聚磷酸铵、脲醛树脂包裹的改性聚磷酸铵和环氧树脂包裹的改性聚磷酸铵中的一种或两种以上任意比例的组合。选用的蜜胺改性聚磷酸铵(APP-Ⅱ),是在Ⅱ型聚磷酸铵的基础上使用三聚氰胺改性而成,聚合度高且不含甲醛,可有效减小阻燃剂的吸湿性,减小在溶液中的粘度,提高耐热性,并能增加阻燃体系与聚合物及树脂的相容性,明显提高阻燃效率及耐水性能。
所述溴化阻燃剂为十溴二苯乙烷。
所述分散乳化剂为异构十醇聚氧乙烯醚,所述抗冻剂为丙二醇、成膜助剂为十二醇酯、pH调节剂为AMP-95,所述增稠剂为羟乙基纤维素和缔合型聚氨酯增稠剂任意比例的组合。
纤维素类增稠剂的使用历史较长、品种很多,其优点是增稠效率高,缺点是耐水性不好,容易被微生物降解,发霉发臭,体系增稠后的触发性强,流平性不佳。常用的纤维素类增稠剂有羟乙基纤维素(HEC)等。
聚丙烯酸类增稠剂又叫碱溶胀增稠剂(ASE),一般是由(甲基)丙烯酸和丙烯酸乙酯,经过一定聚合而制备的一种乳液。其优点是涂膜的致密性相对好一些,可以防止涂膜流挂,防止沉降。缺点是对pH值敏感,耐水性差。
聚氨酯增稠剂(HEUR)是一种疏水基团改性的乙氧基聚氨酯水溶性聚合物,属于非离子型缔合增稠剂。HEUR是由疏水基团、亲水链和聚氨酯基团三部分组成。疏水基团起缔合作用,是增稠的决定因素,亲水链能提供化学稳定性和粘度稳定性。HEUR的优点是对PH不敏感,流平性好,耐水性好。
本发明所述的增稠剂为羟乙基纤维素和缔合型聚氨酯增稠剂任意比例的组合。无机含磷阻燃剂,如聚磷酸铵因其较高的水溶性,部分溶解后呈酸性,影响体系pH值的稳定性,所以在采用丙烯酸类碱增稠剂时,水性涂层体系存在对PH值敏感,耐水性差,易分层等缺点。本发明采用缔合型聚氨酯增稠剂和纤维素增稠剂的组合,减少体系对水和pH的敏感性,共同调节水性涂料胶的流变性能。
本发明提供的含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物的制备方法为:在分散釜中加入水、分散乳化剂,搅拌混合后,再加入溴化阻燃剂、含磷阻燃剂、成炭剂、疏水改性乳液、成膜剂、成膜助剂和抗冻剂,充分搅拌进行分散,使分散液粒子直径小于3μm,然后加入增稠剂和pH调节剂调节粘度和PH值并充分搅拌,最后经过过滤得到成品。
本发明提供了一种阻燃的纺织品织物,将含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物涂布在纺织物上,便获得阻燃的纺织品织物。所述纺织物为选自尼龙、棉、聚酯织物及它们的组合。阻燃的纺织品织物不含锑。
本发明提供的含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物耐水好,阻燃效果好。
具体实施方式
本发明申请使用的术语“不含锑”是指这样的组合物,其中没有特别加入锑(作为单质锑或含锑合金、化合物或其它类似物质),使得锑仅作为痕量组分或作为O.lwt%或更少的杂质存在于阻燃剂组合物中。
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
主要原材料:
1、所选用的改性聚磷酸铵(APP-Ⅱ)聚合度大于1000,包括蜜胺树脂包裹的改性聚磷酸铵,硅凝胶包裹的改性聚磷酸铵,聚氨酯包裹的改性聚磷酸铵,脲醛树脂包裹的改性聚磷酸铵,环氧树脂包裹的改性聚磷酸铵;
2、所选用的成碳剂选自:季戊四醇(PER),超支化聚酯成炭剂Boltorn H20、Boltorn H30、Boltorn H40,超支化三嗪成炭剂;
4、硅丙乳液RS-996AD:一种有机硅改性的丙烯酸乳液,用于改善水性涂料的抗水性和抗油性;
5、增稠剂选自:羟乙基纤维素(HEC),丙烯酸类碱增稠剂8201(碱增稠剂),缔合型聚氨酯增稠剂RM8W(罗门哈斯);
6、RDP:间苯二酚一双(磷酸二苯酯),低聚磷酸酯阻燃剂;
7、抗冻剂:丙二醇;
8、成膜助剂:十二醇酯;
9、pH调节剂:AMP-95。
对比实施例1
阻燃涂层组合物的原料组成为:
对比实施例2
阻燃涂层组合物的原料组成为:
对比实施例3
阻燃涂层组合物的原料组成为:
对比实施例4
阻燃涂层组合物的原料组成为:
实施例5
阻燃涂层组合物的原料组成为:
实施例6
阻燃涂层组合物的原料组成为:
实施例7
阻燃涂层组合物的原料组成为:
实施例8
阻燃涂层组合物的原料组成为:
本发明实施例的制备方法如下:
在分散釜中加入水、分散乳化剂,搅拌混合后,再加入溴化阻燃剂、含磷阻燃剂、成炭剂、疏水改性乳液、成膜剂、成膜助剂和抗冻剂,充分搅拌进行分散,使分散液粒子直径小于3μm,然后加入增稠剂和pH调节剂调节粘度和PH值并充分搅拌,最后经过过滤得到成品即含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物。
本发明制得的水性阻燃涂层组合物的物理指标如下:
外观:乳白或微黄色粘稠状液体;
固含量:50±10%;
粘度:80-130KU;
pH值:6.0-9.0。
将上述制备的水性阻燃涂层组合物涂到玻璃片上,在105度的烘箱干燥1小时,称取重量W1。将干燥后的涂层组合物放入40℃温水浴中浸泡60min,然后取出在105度烘箱干燥1小时,称取重量W2。计算水性阻燃涂层组合物泡水前后的重量损失率,即失重率%=100*(W1-W2)/W1。每个水性阻燃涂层组合物配方分别涂到3片玻璃片上,按照以上步骤计算失重率,并取平均值,结果见下表;
泡水后失重率越大,表明水性阻燃涂层组合物越不耐水。对比实施例1无卤P-N体系失重率为18.5%,耐水性最差。对比实施例2-4为Br-P体系,因为部分采用了疏水改性乳液,耐水性提高,失重率降到7-9%。实施例5-8为Br-P体系,除部分采用了疏水改性乳液外,使用不溶于水的超支化成碳剂,取代耐水差且溶于水的季戊四醇成碳剂,阻燃胶失重率下降到2-3%,耐水性进一步提高。
阻燃性:测试依据《GB/T5455—2014纺织品燃烧性能垂直方向损毁长度和续燃时间的测定》的规定进行。选涤纶窗帘布作为基布,用涂层机将阻燃涂层组合物均匀的涂布在织物的背面,用烘箱120-200度,干燥1-10分钟,干膜涂布量控制在40-100g/m2左右。然后用垂直法织物燃烧性能测试仪,将300X80毫米试样放置在规定的燃烧器下点燃,稳定火苗30秒,开始点燃12秒后,移开火焰,测量试样的续燃时间、阴燃时间和损毁长度。Bl级:损毁炭长度≤15cm,续燃时间≤5s,阴燃时间≤5s。测试结果见下表:
由上表结果可以看出:单纯无卤P-N体系的阻燃性能无法达到B1级的阻燃标准。采用本发明的新型Br-P协效体系,采用超支化成碳剂和疏水改性乳液,即可大大提高阻燃胶的耐水性能,又可以达到B1的阻燃标准。
以上所述,仅是本发明的较佳实施例而已,并非对本发明的技术方案作任何形式上的限制。凡是依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均落入本发明的保护范围内。
实施例名称 | 续燃时间(秒) | 阴燃时间(秒) | 损毁长度(厘米) |
对比实施例1 | >15 | 0 | >15 |
实施例5 | 0 | 0 | 9 |
实施例6 | 0 | 0 | 10 |
实施例7 | 0 | 0 | 8 |
实施例8 | 0 | 0 | 7 |
。
Claims (6)
1.一种含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物,其特征在于其原料组成按重量配比关系包括:
成膜剂15-40份,溴化阻燃剂10-30份,含磷阻燃剂10-30份,成炭剂3-15份,疏水改性乳液5-15份,分散乳化剂、增稠剂、抗冻剂、成膜助剂和pH调节剂组成的水性涂料助剂0.5-10份,水20-50份;
所述溴化阻燃剂为十溴二苯乙烷;
所述含磷阻燃剂为磷氮型膨胀型阻燃剂;所述磷氮型膨胀型阻燃剂为疏水改性包裹的聚磷酸铵,选自蜜胺树脂包裹的改性聚磷酸铵、硅凝胶包裹的改性聚磷酸铵、聚氨酯包裹的改性聚磷酸铵、脲醛树脂包裹的改性聚磷酸铵和环氧树脂包裹的改性聚磷酸铵中的一种或两种以上任意比例的组合;
所述成炭剂为不溶于水的超支化成碳剂;所述超支化成碳剂选自超支化的三嗪成炭剂或具有羟基官能团的、树枝状的、超支化的、3D结构的聚酯树脂或二者任意比例的混合物;所述疏水改性乳液选自有机硅改性的丙烯酸聚酯乳液或聚氨酯改性的丙烯酸聚酯乳液或二者任意比例的混合物;
所述增稠剂为羟乙基纤维素和缔合型聚氨酯增稠剂任意比例的组合。
2.如权利要求1所述的含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物,其特征在于:所述的成膜剂为乙烯-醋酸乙烯酯共聚乳液或丙烯酸聚酯共聚乳液或二者任意比例的混合物。
3.如权利要求1所述的含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物,其特征在于:所述具有羟基官能团的、树枝状的、超支化的、3D结构的聚酯树脂选自第一代超支化羟基聚酯、第二代超支化羟基聚酯、第三代超支化羟基聚酯和第四代超支化羟基聚酯中的一种或两种以上任意比例的混合。
4.如权利要求1所述的含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物,其特征在于:所述分散乳化剂为异构十醇聚氧乙烯醚,所述抗冻剂为丙二醇、成膜助剂为十二醇酯、pH调节剂为AMP-95。
5.制备如权利要求1-4任一项所述的含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物的方法,其特征在于:在分散釜中加入水、分散乳化剂,搅拌混合后,再加入溴化阻燃剂、含磷阻燃剂、成炭剂、疏水改性乳液、成膜剂、成膜助剂和抗冻剂,充分搅拌进行分散,使分散液粒子直径小于3μm,然后加入增稠剂和pH调节剂调节粘度和PH值并充分搅拌,最后经过过滤得到成品。
6.一种阻燃纺织品织物,其特征在于:将权利要求1-4任一项所述的含超支化聚合物的无重金属溴磷协效水性纺织阻燃涂层组合物涂布在纺织物上,便获得阻燃的纺织品织物。
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