CN112252026A - 一种环保型磷系低增重阻燃面料生产工艺 - Google Patents
一种环保型磷系低增重阻燃面料生产工艺 Download PDFInfo
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000003063 flame retardant Substances 0.000 title claims abstract description 87
- 239000004744 fabric Substances 0.000 title claims abstract description 42
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 35
- 239000011574 phosphorus Substances 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000011248 coating agent Substances 0.000 claims abstract description 34
- 238000000576 coating method Methods 0.000 claims abstract description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000002195 synergetic effect Effects 0.000 claims abstract description 12
- 229920000587 hyperbranched polymer Polymers 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 7
- 238000004381 surface treatment Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 10
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
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- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 7
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
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- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 4
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- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims description 4
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 4
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- 239000011780 sodium chloride Substances 0.000 claims description 4
- 239000002562 thickening agent Substances 0.000 claims description 4
- AXJAWMUPFHKOHY-UHFFFAOYSA-N trimethyl(octadecyl)silane Chemical compound CCCCCCCCCCCCCCCCCC[Si](C)(C)C AXJAWMUPFHKOHY-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
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- -1 cationic quaternary ammonium salt Chemical class 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
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- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229920000515 polycarbonate Polymers 0.000 claims description 3
- 239000004417 polycarbonate Substances 0.000 claims description 3
- 229940014800 succinic anhydride Drugs 0.000 claims description 3
- 239000002344 surface layer Substances 0.000 claims description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 3
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 claims description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 3
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 claims description 3
- 208000016261 weight loss Diseases 0.000 claims description 3
- 239000013585 weight reducing agent Substances 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000005002 finish coating Substances 0.000 claims 1
- 150000003014 phosphoric acid esters Chemical class 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 7
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- 229910052736 halogen Inorganic materials 0.000 description 6
- 150000002367 halogens Chemical class 0.000 description 6
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
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- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 230000004584 weight gain Effects 0.000 description 2
- 235000019786 weight gain Nutrition 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 208000021017 Weight Gain Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000003763 carbonization Methods 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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Abstract
本发明公开了一种环保型磷系低增重阻燃面料生产工艺,包括如下步骤:(1)超支化二氧化硅改性溶胶的制备、(2)磷‑硅协同阻燃剂制备、(3)对面料进行表面处理、(4)阻燃涂层整理。在每个步骤中均使用了超支化聚合物,所使用的阻燃剂为环保型磷系阻燃剂。本发明所涉及的一种环保型磷系低增重阻燃面料生产工艺,采用经过超支化改性的二氧化硅溶胶与环保磷系阻燃剂进行混合,所制备的含有超支化的环保磷系阻燃涂层,在对织物表面进行涂层时能够具有优异的结合力,使得在经过多次水洗后仍具有良好的阻燃效果。
Description
技术领域
本发明涉及阻燃面料生产技术领域,尤其是一种环保型磷系低增重阻燃面料生产工艺。
背景技术
阻燃涂层因为其在火焰灼烧情况下可以防止火焰续燃并形成致密碳化层,可以有效地隔绝火势传递,在面料行业有广泛使用。市场上的阻燃图层目前有非环保的卤素系阻燃涂层和环保型的磷氮系阻燃涂层。
卤素系涂层具有阻燃效果优良,且涂层厚度薄(60-70克/平方米),曾经广受欢迎,但因为卤素的毒性较大,随着市场对安全环保要求的进一步提高,卤素系列阻燃涂层已逐渐退出主流面料市场。取而代之的是环保的磷氮系阻燃涂层,然而磷氮系阻燃图层因其阻燃性能不如卤素系列,在实际应用中不得不通过增加涂层厚度,即增加涂层干重(磷氮系涂层干重一般需要达到120-130克/平方米),来达到具体要求。因为磷氮系涂层的厚度比较大,所以经涂层的面料经常面临手感偏硬的问题。
另外,为了形成致密的碳化层,涂层胶里经常会加入高分解温度的阻燃粉,使得涂层脆性增大且形成白色不透光涂层,限制了其许多应用范围。
发明内容
本发明的目的是提供一种环保型磷系低增重阻燃面料生产工艺,采用含有超支化聚合物的环保磷系阻燃剂,使得所制备阻燃面料的阻燃涂层透明并且手感软不发脆,并且在低增重的前提下,亦能保持较好的阻燃效果。
为解决上述技术问题,本发明的目的是这样实现的:
本发明所涉及的一种环保型磷系低增重阻燃面料生产工艺,包括如下步骤:
(1)超支化二氧化硅改性溶胶的制备
称取聚碳酸酯二醇于密闭容器中,在120℃真空干燥2h,脱水干燥后,通往氮气排体系中的除氧气,然后再加入甲苯-2,4-二异氰酸酯及二月桂酸二丁基锡,在80℃反应30min,加入2,2-二羟甲基丙酸/N-甲基吡咯烷酮溶液后,在80℃继续反应2.5h,并在反应过程用适量的四氢呋喃调节体系的粘度,冷却至室温,用四氢呋喃/三乙胺混合浆溶液稀释至20%质量分数,加入NOCH2CH3中和;再加入丁二酸酐改性超支化聚合物、含硅单体,快速搅拌下加水分散,然后将溶剂四氢呋喃蒸出去,然后再加入纳米硅溶胶,继续搅拌,使其混合均匀;
(2)磷-硅协同阻燃剂制备
在步骤(1)制备的超支化二氧化硅改性溶胶中加入其重量10-20%的环保型磷系阻燃剂、3-5%的聚酯类超支化聚合物,搅拌至完全均匀分散;然后将此混合物干燥,使其凝胶并除去溶剂,获得磷-硅协同阻燃剂;
(3)对面料进行表面处理
将面料按照浴比1:5-10置于碱减量处理液中,并升温至130-135℃,处理25-30分钟;降温至105-110℃,再加入高效除油剂DK-808、分散剂DN,处理10-15分钟,再降低温至80-85℃,加入适量醋酸中和,并水洗、烘干;
所述碱减量处理液中含有烧碱、氯化钠、促进剂,所述烧碱的用量为35-40g/L,所述促进剂的用量为0.5-1g/L,所述氯化钠的用量为0.2-0.5g/L;所述促进剂为阳离子季铵盐类有机物;所述烧碱的纯度在98%以上;
(4)阻燃涂层整理
将起经过前处理的面料表面涂覆阻燃涂料,并采用紫外光照射,再烘干;所述阻燃涂料的组分及重量比为:丙烯酸酯乳液50-60%,磷-硅协同阻燃剂30-40%,超支化聚酯季铵盐3-5%,三氧化铁0.1-0.5%,增稠剂和水4-10%;织物的上胶量为80-100g/m2。
在上述方案的基础上并作为上述方案的优选方案:所述含硅单体为甲基三甲氧基硅烷、乙基三甲氧基硅烷、十八烷基三甲基硅烷、苯基三甲氧基硅烷中、正硅酸四乙酯、正硅酸甲酯、正硅酸丙酯中的一种或多种。
在上述方案的基础上并作为上述方案的优选方案:所述超支化聚酯季铵盐为GTA-H20或GTA-H30。
在上述方案的基础上并作为上述方案的优选方案:所述纳米硅溶胶的分子式可表示为mSiO2·nH2O,内部结构为硅氧烷键,表层由硅羟基所覆盖。
在上述方案的基础上并作为上述方案的优选方案:所述环保型磷系阻燃剂包含粘合剂、成炭剂、超支化磷酸酯和磷系阻燃剂;按重量份数计,所述各成分的重量份分别为:粘合剂45-55份,成炭剂20-25份,超支化磷酸酯3-5份,磷系阻燃剂15-20份。
本发明的有益效果是:本发明所涉及的一种环保型磷系低增重阻燃面料生产工艺,采用经过超支化改性的二氧化硅溶胶与环保磷系阻燃剂进行混合,所制备的含有超支化的环保磷系阻燃涂层,在对织物表面进行涂层时能够具有优异的结合力,使得在经过多次水洗后仍具有良好的阻燃效果。
具体实施方式
下面结合具体实施例对本发明进一步说明。
实施例
本实施例所涉及的一种环保型磷系低增重阻燃面料生产工艺,包括如下步骤:(1)超支化二氧化硅改性溶胶的制备、(2)磷-硅协同阻燃剂制备、(3)对面料进行表面处理、(4)阻燃涂层整理。所使用的面料为克重为130-150克每平方米的涤纶面料。
在步骤(1)超支化二氧化硅改性溶胶的制备中,是先称取3质量份的聚碳酸酯二醇,置于密闭容器中,在120℃真空干燥2h,脱水干燥后,通往氮气排体系中的除氧气,然后再加入10质量份的甲苯-2,4-二异氰酸酯及5质量份的二月桂酸二丁基锡,在80℃反应30min,加入按20质量份的2,2-二羟甲基丙酸/N-甲基吡咯烷酮溶液后,在80℃继续反应2.5h,并在反应过程用适量的四氢呋喃调节体系的粘度,用二正丁胺法测试体系-NCO的含量,当-NCO的含量达到理论值时,冷却至室温,用四氢呋喃/三乙胺混合浆溶液稀释至20%质量分数,加入NOCH2CH3中和;再加入2质量份的丁二酸酐改性超支化聚合物、6质量份的含硅单体,快速搅拌下加水分散,然后将溶剂四氢呋喃蒸出去,然后再加入3质量份的纳米硅溶胶,并采用超声波分散法继续搅拌,使其混合均匀。
其是,2,2-二羟甲基丙酸、N-甲基吡咯烷酮是按照1:3的比例混合。
含硅单体为甲基三甲氧基硅烷、乙基三甲氧基硅烷、十八烷基三甲基硅烷、苯基三甲氧基硅烷中、正硅酸四乙酯、正硅酸甲酯、正硅酸丙酯中的一种或多种。在本实施例中为甲基三甲氧基硅烷、乙基三甲氧基硅烷、十八烷基三甲基硅烷按照1:1:1的比例混合所得到。
在本步骤中,纳米硅溶胶的分子式可表示为mSiO2·nH2O,内部结构为硅氧烷键(-Si-O-Si-),表层由硅羟基(-SiOH)所覆盖。利用纳米硅溶胶具有良好的耐高温性、水溶性、反应隆和比表面积大、无毒、无味、无卤、阻燃等特点提高环保磷阻燃剂的阻燃性能,并减少涂胶量。
在步骤(2)磷-硅协同阻燃剂制备中,是在步骤(1)制备的超支化二氧化硅改性溶胶中加入其重量10-20%的环保型磷系阻燃剂、3-5%的聚酯类超支化聚合物,搅拌至完全均匀分散;然后将此混合物干燥,使其凝胶并除去溶剂,获得磷-硅协同阻燃剂。具体在,在本实施例中所加入的是15%的环保型磷系阻燃剂、4%的聚酯类超支化聚合物
环保型磷系阻燃剂包含粘合剂、成炭剂、超支化磷酸酯和磷系阻燃剂;按重量份数计,所述各成分的重量份分别为:粘合剂45-55份,成炭剂20-25份,超支化磷酸酯3-5份,磷系阻燃剂15-20份。具体的,粘合剂50份,成炭剂23份,超支化磷酸酯4份,磷系阻燃剂18份。
在步骤(3)对面料进行表面处理中,是将面料按照浴比1:5-10置于碱减量处理液中,并升温至130-135℃,处理25-30分钟;降温至105-110℃,再加入高效除油剂DK-808、分散剂DN,处理10-15分钟,再降低温至80-85℃,加入适量醋酸中和,并水洗、烘干。
碱减量处理液中含有烧碱、氯化钠、促进剂,烧碱的用量为35-40g/L,促进剂的用量为0.5-1g/L,氯化钠的用量为0.2-0.5g/L;促进剂为阳离子季铵盐类有机物;烧碱的纯度在98%以上。具体的,烧碱的用量为38g/L,促进剂的用量为0.8g/L,氯化钠的用量为0.3g/L
在步骤(4)阻燃涂层整理中,是将起经过前处理的面料表面涂覆阻燃涂料,并采用紫外光照射,再烘干;所述阻燃涂料的组分及重量比为:丙烯酸酯乳液50-60%,磷-硅协同阻燃剂30-40%,超支化聚酯季铵盐3-5%,三氧化铁0.1-0.5%,增稠剂和水4-10%;织物的上胶量为80-100g/m2。具体的,丙烯酸酯乳液55%,磷-硅协同阻燃剂35%,超支化聚酯季铵盐4%,三氧化铁0.3%,增稠剂和水7%;织物的上胶量为90g/m2。
所使用的超支化聚酯季铵盐为GTA-H20或GTA-H30,具体为GTA-H20。使用了氯化铁作为光引发剂,可有效的提高其固化的速率,并提高与纤维的结合能力和结合牢度。经过烘干后的增重量为70g/m2。
在本实施例中,步骤1、2、3、4中都使用了超支化聚合物,可有效的提高结合能力提高阻燃效果和耐水洗性。
按照GB/T5455《纺织品燃烧性能试验垂直法》,采用YG(B)815D-1型垂直燃烧仪进行阻燃性能测试,阻燃性国标B1级:损毁长度≦15cm,续燃时间≦5s,阴燃时间≦5s。
对实施例进行测试,其结果为:损毁长度为3.4cm,续燃时间为0s,阴燃时间为0s。由此可见了本实施例所制备的阻燃面料在增重量较小的情况下,具有良好的阻燃效果。
实施例所制备的阻燃面料进行洗涤10次后,测试结果为损毁长度为5.1cm,续燃时间为0s,阴燃时间为0s。
实施例所制备的阻燃面料进行洗涤20次后,测试结果为损毁长度为7.6cm,续燃时间为0s,阴燃时间为0s。
可见在洗涤多次后仍具有良好的阻燃效果。
以上详细描述了本发明的较佳具体实施例。应当理解,本领域的普通技术人员无需创造性劳动就可以根据本发明的构思做出诸多修改和变化。因此,凡本技术领域中技术人员依本发明的构思在现有技术的基础上通过逻辑分析、推理或者有限的实验可以得到的技术方案,皆应在由权利要求书所确定的保护范围内。
Claims (5)
1.一种环保型磷系低增重阻燃面料生产工艺,其特征在于,包括如下步骤:
(1)超支化二氧化硅改性溶胶的制备
称取聚碳酸酯二醇于密闭容器中,在120℃真空干燥2h,脱水干燥后,通往氮气排体系中的除氧气,然后再加入甲苯-2,4-二异氰酸酯及二月桂酸二丁基锡,在80℃反应30min,加入2,2-二羟甲基丙酸/N-甲基吡咯烷酮溶液后,在80℃继续反应2.5h,并在反应过程用适量的四氢呋喃调节体系的粘度,冷却至室温,用四氢呋喃/三乙胺混合浆溶液稀释至20%质量分数,加入NOCH2CH3中和;再加入丁二酸酐改性超支化聚合物、含硅单体,快速搅拌下加水分散,然后将溶剂四氢呋喃蒸出去,然后再加入纳米硅溶胶,继续搅拌,使其混合均匀;
(2)磷-硅协同阻燃剂制备
在步骤(1)制备的超支化二氧化硅改性溶胶中加入其重量10-20%的环保型磷系阻燃剂、3-5%的聚酯类超支化聚合物,搅拌至完全均匀分散;然后将此混合物干燥,使其凝胶并除去溶剂,获得磷-硅协同阻燃剂;
(3)对面料进行表面处理
将面料按照浴比1:5-10置于碱减量处理液中,并升温至130-135℃,处理25-30分钟;降温至105-110℃,再加入高效除油剂DK-808、分散剂DN,处理10-15分钟,再降低温至80-85℃,加入适量醋酸中和,并水洗、烘干;
所述碱减量处理液中含有烧碱、氯化钠、促进剂,所述烧碱的用量为35-40g/L,所述促进剂的用量为0.5-1g/L,所述氯化钠的用量为0.2-0.5g/L;所述促进剂为阳离子季铵盐类有机物;所述烧碱的纯度在98%以上;
(4)阻燃涂层整理
将起经过前处理的面料表面涂覆阻燃涂料,并采用紫外光照射,再烘干;所述阻燃涂料的组分及重量比为:丙烯酸酯乳液50-60%,磷-硅协同阻燃剂30-40%,超支化聚酯季铵盐3-5%,三氧化铁0.1-0.5%,增稠剂和水4-10%;织物的上胶量为80-100/m2。
2.根据权利要求1所述的环保型磷系低增重阻燃面料生产工艺,其特征在于,所述含硅单体为甲基三甲氧基硅烷、乙基三甲氧基硅烷、十八烷基三甲基硅烷、苯基三甲氧基硅烷中、正硅酸四乙酯、正硅酸甲酯、正硅酸丙酯中的一种或多种。
3.根据权利要求1所述的环保型磷系低增重阻燃面料生产工艺,其特征在于,所述超支化聚酯季铵盐为GTA-H20或GTA-H30。
4.根据权利要求1所述的环保型磷系低增重阻燃面料生产工艺,其特征在于,所述纳米硅溶胶的分子式可表示为mSiO2·nH2O,内部结构为硅氧烷键,表层由硅羟基所覆盖。
5.根据权利要求1所述的环保型磷系低增重阻燃面料生产工艺,其特征在于,所述环保型磷系阻燃剂包含粘合剂、成炭剂、超支化磷酸酯和磷系阻燃剂;按重量份数计,所述各成分的重量份分别为:粘合剂45-55份,成炭剂20-25份,超支化磷酸酯3-5份,磷系阻燃剂15-20份。
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