CN110845529A - 一种含磷多乙烯多胺阻燃剂及其制备方法 - Google Patents
一种含磷多乙烯多胺阻燃剂及其制备方法 Download PDFInfo
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- CN110845529A CN110845529A CN201911160773.5A CN201911160773A CN110845529A CN 110845529 A CN110845529 A CN 110845529A CN 201911160773 A CN201911160773 A CN 201911160773A CN 110845529 A CN110845529 A CN 110845529A
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 66
- 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 60
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 52
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000011574 phosphorus Substances 0.000 title claims abstract description 51
- -1 polyethylene Polymers 0.000 title claims abstract description 49
- 239000004698 Polyethylene Substances 0.000 title claims abstract description 48
- 229920000768 polyamine Polymers 0.000 title claims abstract description 48
- 229920000573 polyethylene Polymers 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 29
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000047 product Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000084 colloidal system Substances 0.000 claims abstract description 9
- 150000007529 inorganic bases Chemical class 0.000 claims abstract description 9
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- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 4
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims abstract description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims abstract description 3
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 claims abstract description 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- BHIIGRBMZRSDRI-UHFFFAOYSA-N [chloro(phenoxy)phosphoryl]oxybenzene Chemical compound C=1C=CC=CC=1OP(=O)(Cl)OC1=CC=CC=C1 BHIIGRBMZRSDRI-UHFFFAOYSA-N 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical group CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 claims description 5
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 4
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- 239000002131 composite material Substances 0.000 abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 239000000779 smoke Substances 0.000 abstract description 4
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 3
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- HEDRZPFGACZZDS-MICDWDOJSA-N Trichloro(2H)methane Chemical compound [2H]C(Cl)(Cl)Cl HEDRZPFGACZZDS-MICDWDOJSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- VYGRRCKMMADGBB-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] phosphono hydrogen phosphate Chemical compound OCC(CO)(CO)COP(O)(=O)OP(O)(O)=O VYGRRCKMMADGBB-UHFFFAOYSA-N 0.000 description 2
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- KGENPKAWPRUNIG-UHFFFAOYSA-N 1-[chloro(ethyl)phosphoryl]ethane Chemical compound CCP(Cl)(=O)CC KGENPKAWPRUNIG-UHFFFAOYSA-N 0.000 description 1
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- 238000004679 31P NMR spectroscopy Methods 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- WVPKAWVFTPWPDB-UHFFFAOYSA-M dichlorophosphinate Chemical compound [O-]P(Cl)(Cl)=O WVPKAWVFTPWPDB-UHFFFAOYSA-M 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- ASMQGLCHMVWBQR-UHFFFAOYSA-M diphenyl phosphate Chemical compound C=1C=CC=CC=1OP(=O)([O-])OC1=CC=CC=C1 ASMQGLCHMVWBQR-UHFFFAOYSA-M 0.000 description 1
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- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- CWXPZXBSDSIRCS-UHFFFAOYSA-N tert-butyl piperazine-1-carboxylate Chemical compound CC(C)(C)OC(=O)N1CCNCC1 CWXPZXBSDSIRCS-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
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- 239000002341 toxic gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/22—Amides of acids of phosphorus
- C07F9/24—Esteramides
- C07F9/2454—Esteramides the amide moiety containing a substituent or a structure which is considered as characteristic
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- C07F9/24—Esteramides
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Abstract
Description
技术领域
本发明属于无卤阻燃技术领域,具体是涉及一种含磷多乙烯多胺阻燃剂及其制备方法。
背景技术
随着高分子材料科学与工程的发展,各种高分子复合材料已逐渐取代传统材料,并应用于社会生产和生活的各个领域。然而,绝大多数高分子材料都是可燃的,而且高分子材料在受热或燃烧过程中会产生大量烟尘和有毒气体,给人们的生产和生活带来了一定的安全隐患。目前用于高分子材料的阻燃剂主要为含卤体系,虽然含卤阻燃剂的阻燃效率很高,但由于其在燃烧过程中会产生大量有毒烟气,有的含卤阻燃剂燃烧时还会产生致癌物质,会给环境带来严重的危害,因此无卤阻燃剂的研发和应用已是国内外阻燃领域发展的趋势。
磷系有机阻燃剂是目前研究和应用非常广泛的一类无卤阻燃剂,阻燃效率高,对环境污染较小,具有广阔的发展前景。尽管小分子磷系有机阻燃剂制备简单,阻燃效果较好,但是其热分解温度较低,在聚合物材料中容易破坏高分子的连续性,从而降低其力学性能。因此,近年来聚合型磷系有机阻燃剂受到广泛关注。如中国专利CN 109749088 A采用手性磷酸、对苯二氨、对苯二异氰酸脂等物质进行聚合反应形成三元共聚物,因为其具有非常高的含碳量,从而达到阻燃效果。中国专利CN 108484919 A以三聚氯氰、N-Boc-哌嗪为初始原料,通过控制反应条件得到中间体(I),再通过与磷酸成盐得到中间体(II),最后高温煅烧得到含磷大分子阻燃剂。中国专利CN 108794746 A报道了一种大分子磷氮类阻燃剂及其制备方法,以磷酰二氯类或二氯磷酸酯类物质、哌嗪为初始原料,通过控制反应条件得到中间体的溶液,再通过与三聚氯氰反应得到本发明的大分子磷氮类阻燃剂。中国专利CN105601857 A公开了一种大分子膨胀阻燃剂的制备方法,包括如下步骤:步骤1)三聚氰胺-双氰胺树脂的合成;步骤2)季戊四醇二磷酸酯的合成;步骤3)季戊四醇二磷酸酯三聚氰胺-双氰胺树脂盐的合成。
由此可以看出,目前聚合型磷系有机阻燃剂普遍存在制备工艺复杂这一重大缺陷。此外,目前的大分子磷系阻燃剂含磷量偏低,导致阻燃效率不高,应用受到一定限制。因此,本发明针对现有技术中存在的问题,提出一步法制备磷、氮含量均较高的聚合型磷系有机阻燃剂。
发明内容
本发明要解决的技术问题为克服现有技术中存在的制备工艺复杂、阻燃效率较低等缺陷,提供一种含磷多乙烯多胺阻燃剂及其制备方法。
为了解决上述技术问题,本发明所采用的技术方案为:一种含磷多乙烯多胺阻燃剂,其分子结构式为:
式中,R为乙基、苯基、乙氧基或苯氧基。
一种含磷多乙烯多胺阻燃剂的制备方法,反应原料由多乙烯多胺、磷酰氯、无机碱、有机碱和有机溶剂组成,多乙烯多胺、磷酰氯、无机碱和有机碱的摩尔比为1:3~6:2~6:3~5。
作为本发明含磷多乙烯多胺阻燃剂的制备方法的进一步改进,所述磷酰氯为二乙基次磷酰氯、二苯基次磷酰氯、氯代磷酸二乙酯或氯代磷酸二苯酯。所述无机碱为醋酸钠、碳酸钠或碳酸钾。所述有机碱为三丙胺或N-甲基咪唑。所述有机溶剂为四氢呋喃、1,4-二氧六环或二氯甲烷。
作为本发明含磷多乙烯多胺阻燃剂的制备方法的进一步改进,具体反应步骤为:首先将多乙烯多胺溶于有机溶剂中,然后加入无机碱和有机碱,在0~5℃和氮气保护条件下,逐滴加入磷酰氯,滴加完毕后接着在0~5℃下继续反应1~3小时,然后升温至30~50℃,在氮气条件反应12~36小时,最后将所得产物过滤去沉淀后除溶剂,得到的淡黄色胶体即含磷多乙烯多胺阻燃剂。
本发明的含磷多乙烯多胺阻燃剂及其制备方法,相对于现有技术的有益效果表现在:
1)、本发明的含磷多乙烯多胺阻燃剂与高分子材料有较好的界面相容性,其耐水性良好,能维持或提高复合材料的耐候性和力学性能。
2)、采用本发明的含磷多乙烯多胺阻燃剂改性高分子材料,可以大幅提高高分子材料的阻燃性能。由于本发明的含磷多乙烯多胺阻燃剂的磷、氮元素含量均较高,二者之间存在协同阻燃效应,使得复合材料在受热或燃烧过程中,能快速促进聚合物碳化,隔氧隔热,降低可燃气体和有毒烟气释放。同时,配合少量的阻燃协效剂,可以进一步提高复合材料的阻燃性能。
3)、本发明的含磷多乙烯多胺阻燃剂的制备方法简单,适用于大多数高分子材料,具有广阔的市场应用前景。
附图说明
图1为实施例1制备的目标产物的核磁共振氢谱。
图2为实施例1所用原料多乙烯多胺的核磁共振氢谱。
图3为实施例1制备的目标产物的核磁共振磷谱。
图4为实施例1所用原料氯代磷酸二苯酯的核磁共振磷谱。
具体实施方式
下面结合附图对本发明的优选方式作进一步详细的描述。
实施例1
将4.68克多乙烯多胺、11.75克碳酸钾、9.72克三丙胺和40毫升四氢呋喃置于三口烧瓶中,在0℃和氮气条件下,逐滴加入27.40克氯代磷酸二苯酯,滴加完毕后在0℃和氮气条件下继续反应1小时,然后升温至30℃,在氮气条件反应24小时,最后将所得产物过滤去沉淀后除溶剂,得到的淡黄色胶体即为本发明的含磷多乙烯多胺阻燃剂。
图1和图2分别为实施例1制备的目标产物和所用原料多乙烯多胺的核磁共振氢谱图1H NMR(400MHz,CDCl3)。从图1和图2中可以看出,二者最显著的区别是在图1化学位移7.1-7.3处有十分显著的峰,归属于磷酸二苯酯中苯环上的氢。此外,多乙烯多胺中亚甲基的化学位移为2.17-2.49(见图2),而目标产物中亚甲基的化学位移为2.27-2.63和3.11-3.20,这是由于磷酰基团的引入导致氢原子的化学位移向低场移动。
图3和图4分别为实施例1制备的目标产物和所用原料氯代磷酸二苯酯的核磁共振磷谱图31P NMR(162MHz,CDCl3)。从图3和图4中可以看出,氯代磷酸二苯酯中磷的化学位移为-5.26,目标产物中磷的化学位移在0左右,说明氯代磷酸二苯酯与多乙烯多胺发生了亲核取代反应,磷所处的化学环境发生变化导致磷原子的化学位移向高场移动。
实施例2
将1.38克多乙烯多胺、0.82克醋酸钠、1.23克N-甲基咪唑和10毫升1,4-二氧六环置于三口烧瓶中,在1℃和氮气条件下,逐滴加入2.11克二乙基次磷酰氯,滴加完毕后在1℃和氮气条件下继续反应1.5小时,然后升温至35℃,在氮气条件反应12小时,最后将所得产物过滤去沉淀后除溶剂,得到的淡黄色胶体即为本发明的含磷多乙烯多胺阻燃剂。
实施例3
将13.75克多乙烯多胺、15.90克碳酸钠、16.42克N-甲基咪唑和120毫升二氯甲烷置于三口烧瓶中,在2℃和氮气条件下,逐滴加入47.33克二苯基次磷酰氯,滴加完毕后在2℃和氮气条件下继续反应2小时,然后升温至40℃,在氮气条件反应36小时,最后将所得产物过滤去沉淀后除溶剂,得到的淡黄色胶体即为本发明的含磷多乙烯多胺阻燃剂。
实施例4
将8.25克多乙烯多胺、24.88克碳酸钾、21.49克三丙胺和80毫升四氢呋喃置于三口烧瓶中,在3℃和氮气条件下,逐滴加入25.88克氯代磷酸二乙酯,滴加完毕后在3℃和氮气条件下继续反应2.5小时,然后升温至45℃,在氮气条件反应30小时,最后将所得产物过滤去沉淀后除溶剂,得到的淡黄色胶体即为本发明的含磷多乙烯多胺阻燃剂。
实施例5
将27.50克多乙烯多胺、49.22克醋酸钠、32.84克N-甲基咪唑和300毫升四氢呋喃置于三口烧瓶中,在4℃和氮气条件下,逐滴加入161.18克氯代磷酸二苯酯,滴加完毕后在4℃和氮气条件下继续反应3小时,然后升温至50℃,在氮气条件反应20小时,最后将所得产物过滤去沉淀后除溶剂,得到的淡黄色胶体即为本发明的含磷多乙烯多胺阻燃剂。
实施例6
将55.00克多乙烯多胺、84.79克碳酸钠、100.29克三丙胺和500毫升1,4-二氧六环置于三口烧瓶中,在5℃和氮气条件下,逐滴加入189.30克二苯基次磷酰氯,滴加完毕后在5℃和氮气条件下继续反应2小时,然后升温至40℃,在氮气条件反应28小时,最后将所得产物过滤去沉淀后除溶剂,得到的淡黄色胶体即为本发明的含磷多乙烯多胺阻燃剂。
实施例7-10
将实施例1-4所制备的含磷多乙烯多胺阻燃剂分别应用于热塑性聚氨酯弹性体(TPU)中得到实施例7-10,考查其阻燃和力学性能。TPU(85E85)购买于保定邦泰化学工业有限公司。
作为对比,未改性TPU的氧指数为22.5%,拉伸强度为48.4MPa,断裂伸长率为592%。
从实施例7-10中可以看出,只需添加15%本发明的含磷多乙烯多胺阻燃剂即可以显著提高TPU的氧指数和拉伸强度,同时断裂伸长率基本保持不变,即表明采用本发明的阻燃剂改性TPU可以使得其获得优异的阻燃和力学性能。
事实上,本发明的含磷多乙烯多胺阻燃剂还可以与多种阻燃剂进行复配使用。此外,本发明的含磷多乙烯多胺阻燃剂还可以应用于聚烯烃、聚苯乙烯、聚酰胺、环氧树脂等各种热塑性和热固性塑料等高分子材料的阻燃处理,具有广阔的市场应用前景。
上述各实施例只是为了说明本发明的技术构思及特点,其目的是在于让本领域内的普通技术人员能够了解本发明的内容并据以实施,并不能以此限制本发明的保护范围。凡是根据本发明内容的实质所作出的等效的变化或修饰,都应涵盖在本发明的保护范围内。
Claims (7)
2.一种制备如权利要求1所述含磷多乙烯多胺阻燃剂的方法,其特征在于,反应原料由多乙烯多胺、磷酰氯、无机碱、有机碱和有机溶剂组成,多乙烯多胺、磷酰氯、无机碱和有机碱的摩尔比为1:3~6:2~6:3~5。
3.如权利要求2所述的方法,其特征在于,所述磷酰氯为二乙基次磷酰氯、二苯基次磷酰氯、氯代磷酸二乙酯或氯代磷酸二苯酯。
4.如权利要求2所述的方法,其特征在于,所述无机碱为醋酸钠、碳酸钠或碳酸钾。
5.如权利要求2所述的方法,其特征在于,所述有机碱为三丙胺或N-甲基咪唑。
6.如权利要求2所述的方法,其特征在于,所述有机溶剂为四氢呋喃、1,4-二氧六环或二氯甲烷。
7.如权利要求2~6任一项所述的方法,其特征在于,具体反应步骤为:首先将多乙烯多胺溶于有机溶剂中,然后加入无机碱和有机碱,在0~5℃和氮气保护条件下,逐滴加入磷酰氯,滴加完毕后接着在0~5℃下继续反应1~3小时,然后升温至30~50℃,在氮气条件反应12~36小时,最后将所得产物过滤去沉淀后除溶剂,得到的淡黄色胶体即含磷多乙烯多胺阻燃剂。
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