CN115043439B - 一种特种阴离子插层改性的镍钛双金属氢氧化物及其制备方法和应用 - Google Patents
一种特种阴离子插层改性的镍钛双金属氢氧化物及其制备方法和应用 Download PDFInfo
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- 150000001450 anions Chemical class 0.000 title claims abstract description 42
- 238000009830 intercalation Methods 0.000 title claims abstract description 29
- 230000002687 intercalation Effects 0.000 title claims abstract description 29
- 229910000000 metal hydroxide Inorganic materials 0.000 title claims abstract description 28
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical class [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 239000010936 titanium Substances 0.000 claims abstract description 31
- 239000003063 flame retardant Substances 0.000 claims abstract description 27
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims abstract description 25
- 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 claims abstract description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910000348 titanium sulfate Inorganic materials 0.000 claims abstract description 21
- 150000004692 metal hydroxides Chemical class 0.000 claims abstract description 18
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims abstract description 18
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- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 6
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 6
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 5
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 5
- 238000002485 combustion reaction Methods 0.000 claims description 4
- CGFYHILWFSGVJS-UHFFFAOYSA-N silicic acid;trioxotungsten Chemical compound O[Si](O)(O)O.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 CGFYHILWFSGVJS-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims description 2
- 229940072056 alginate Drugs 0.000 claims description 2
- 235000010443 alginic acid Nutrition 0.000 claims description 2
- 229920000615 alginic acid Polymers 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 claims description 2
- 229940005740 hexametaphosphate Drugs 0.000 claims description 2
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 2
- 125000000129 anionic group Chemical group 0.000 claims 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 3
- HDUMBHAAKGUHAR-UHFFFAOYSA-J titanium(4+);disulfate Chemical compound [Ti+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HDUMBHAAKGUHAR-UHFFFAOYSA-J 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 29
- 239000008367 deionised water Substances 0.000 abstract description 24
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 5
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000003780 insertion Methods 0.000 description 3
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- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
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- 235000010413 sodium alginate Nutrition 0.000 description 3
- 229940005550 sodium alginate Drugs 0.000 description 3
- 239000000661 sodium alginate Substances 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
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- 235000011152 sodium sulphate Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
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- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012761 high-performance material Substances 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 description 1
- QWMFKVNJIYNWII-UHFFFAOYSA-N 5-bromo-2-(2,5-dimethylpyrrol-1-yl)pyridine Chemical compound CC1=CC=C(C)N1C1=CC=C(Br)C=N1 QWMFKVNJIYNWII-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
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- KDQPSPMLNJTZAL-UHFFFAOYSA-L disodium hydrogenphosphate dihydrate Chemical compound O.O.[Na+].[Na+].OP([O-])([O-])=O KDQPSPMLNJTZAL-UHFFFAOYSA-L 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/009—Use of pretreated compounding ingredients
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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
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Abstract
本发明公开了一种特种阴离子插层改性的镍钛双金属氢氧化物([Ni1‑xTix(OH)2]2x+(An‑)2x/n·mH2O])及其制备方法与应用,属于新型特种纳米复合金属氢氧化物制备及应用领域。本发明采用一步共沉淀法,以六水合硝酸镍、硫酸钛为原料,以典型特种阴离子对应的盐或酸为阴离子来源,去离子水为溶剂,氢氧化钠为沉淀剂,经配制溶液、滴定共沉淀、抽滤、洗涤、干燥步骤制备得到一系列特种阴离子插层改性的镍钛双金属氢氧化物。将其作为阻燃组份添加到有机硅弹性体泡沫材料中,有效提升了有机硅弹性体泡沫材料的阻燃性能及抑烟性能。
Description
技术领域:
本发明属于新型特种纳米复合金属氢氧化物制备及应用技术领域,具体涉及一种特种阴离子插层改性的镍钛双金属氢氧化物及其制备方法和在阻燃领域中的应用。
背景技术:
有机硅弹性体泡沫是一种有机-无机杂化的高性能材料,结合了有机硅材料以及泡沫材料的优异性能,主要应用于化学化工、航空航天和电子产品行业等领域。但是由于其侧链具有较多的甲基以及泡沫材料特有的泡孔结构,有机硅泡沫材料本质易燃,且伴随毒性烟气释放,对其进行阻燃和抑烟改性至关重要。目前主要是通过添加阻燃填料对其进行阻燃改性。然而现有的阻燃剂大多存在着阻燃效率低、毒性较大、难降解等问题,因此无卤、高效、低烟、低毒的阻燃剂成为新一代阻燃剂的发展趋势。
层状双金属氢氧化物(LDH)是一种典型的二维层状结构,其层板由带正电荷的金属离子和氢氧化物构成,层间为带负电的阴离子和水分子。根据现有报道,LDH可作为阻燃协效剂在环氧树脂、聚氨酯泡沫等聚合物材料起到阻燃增效和抑烟的作用,目前在有机硅泡沫材料中的应用并不多见。同时,现有报道以Mg、Al、Zn为层板金属,以硝酸根、碳酸根为插层阴离子的LDH用于阻燃材料改性较为多见。一些基于高效催化作用及热性能的特种金属离子及特种功能性阴离子插层的LDH尚待开发。因此,可通过调控LDH的金属种类和层间阴离子进行结构设计,提升阻燃协效作用,以满足有机硅弹性体泡沫的阻燃需求。
发明内容:
本发明旨在提供一种特种阴离子插层改性的镍钛双金属氢氧化物及其制备方法与阻燃应用,以LDH结构的优势为切入点,有效组装NiTi-LDH,发挥Ni、Ti以及特种阴离子的协同作用,同时提高有机硅弹性体泡沫阻燃效率和抑烟性能。
为了实现上述目的,本发明涉及的特种阴离子插层改性的镍钛双金属氢氧化物,其化学简式为[Ni1-xTix(OH)2]2x+(An-)2x/n·mH2O],其中0.2≤x≤0.33,所述特种阴离子An-为硫酸根(SO4 2-)、钨酸根(WO4 2-)、硅钨酸根(SiW12O40 4-)、磷钨酸根(PW12O40 3-)、硼酸根(BO3 3-)、海藻酸根(Alg-)、磷酸二氢根(H2PO4 -)、三聚磷酸根(P3O10 5-)、六偏磷酸根(SHMP)中的一种。
所述特种阴离子插层改性的镍钛双金属氢氧化物的制备方法为:
(1)分别配制定量的六水合硝酸镍与硫酸钛混合盐溶液和特种阴离子对应的盐或酸溶液待用;(2)在室温搅拌下,向容器中同步滴加六水合硝酸镍与硫酸钛混合盐溶液和特种阴离子对应的盐或酸溶液,通过氢氧化钠溶液调节并实时监测整个体系的pH值,待体系pH稳定后于一定温度下继续搅拌或超声反应,当特种阴离子为硫酸根时,硫酸根对应的盐优选为硫酸钛;(3)室温静置陈化后过滤洗涤至中性,纯化干燥后获得特种阴离子插层改性的镍钛双金属氢氧化物。
上述制备方法步骤(1)中,硝酸镍与硫酸钛混合盐溶液中c(Ni2+):c(Ti4+)控制在2:1-6:1,其中c(Ni2+)代表混合盐溶液中硝酸镍的物质的量浓度,c(Ti4+)代表混合盐溶液中硫酸钛的物质的量浓度。
上述制备方法步骤(1)中,反应体系中c(An-):c(Ti4+)控制在0.2:1-3:1,其中c(An-)代表步骤(2)反应溶液中特种阴离子的物质的量浓度。
上述制备方法步骤(2)中,通过1mol/L的氢氧化钠溶液调节pH。
上述制备方法步骤(2)中,通过氢氧化钠溶液调节并实时监测整个体系的pH值范围控制在pH=4.5-10.0。
上述制备方法步骤(2)中,超声功率为100W-300W,超声时间为4-8小时,温度为20-80℃,陈化时间为12-24小时。
上述特种阴离子插层改性的镍钛双金属氢氧化物作为阻燃剂的应用。
上述特种阴离子插层改性的镍钛双金属氢氧化物作为阻燃剂应用在有机硅弹性体泡沫材料,当添加量为0.5%~2.0%,有机硅弹性体泡沫材料可通过垂直燃烧FV-1或FV-0等级。
本发明以具有高效催化和热稳定性的Ni、Ti为层板金属,采用具有阻燃效用的特种功能阴离子插层,制备得到的新型特种纳米复合金属氢氧化物,金属离子Ni、Ti之间以及金属离子与特种功能阴离子之间相互协同,可用于有机硅弹性体泡沫的阻燃抑烟。
本发明所述特种阴离子插层改性的镍钛双金属氢氧化物具有如下有益效果:
(1)本发明通过采用一步共沉淀法制备了特种阴离子插层改性的镍钛双金属氢氧化物,根据其较大的比表面积、二维层状结构的物理阻隔作用以及在燃烧时吸收大量热,释放不可燃气体等特性可作为一种高效绿色的阻燃剂;(2)特种阴离子插层改性的镍钛双金属氢氧化物作为阻燃剂应用在有机硅弹性体泡沫材料,当添加量为0.5%~2.0%,有机硅弹性体泡沫材料可通过垂直燃烧FV-1或FV-0等级。
附图说明:
图1是本发明实施例1制备NiTi-LDH-SO4 2-的红外谱图。
图2是本发明实施例1制备NiTi-LDH-SO4 2-的XRD谱图。
图3是本发明实施例6制备NiTi-LDH-WO4 2-的红外谱图。
图4是本发明实施例6制备NiTi-LDH-WO4 2-的XRD谱图。
图5是本发明实施例13制备的NiTi-LDH-CO3 2-的红外谱图。
图6是本发明实施例13制备的NiTi-LDH-CO3 2-的XRD谱图。
具体实施方式:
下面结合具体实施例对本发明进行详细的描述,以下实施例只用于对本发明的进一步说明,而不是全部的实施例。本领域技术人员根据本发明内容没有做出一些创造性的改进和调整所得到的所有其它实施方式,都属于本发明所保护的范围。
实施例1:
NiTi-LDH-SO4 2-的制备:将六水合硝酸镍(5.82g,0.02mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,向反应容器中滴加混合盐溶液,同时通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在9.5,在室温下搅拌6小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-SO4 2-。(c(Ni2+):c(Ti4+)=2)
图1是本发明实施例1制备NiTi-LDH-SO4 2-的红外谱图。在红外谱图中,3640cm-1处的峰为游离的羟基,3335cm-1和1636cm-1处的峰分别为O-H拉伸振动吸收峰和层间水分子的弯曲振动吸收峰,1111cm-1处的峰为SO4 2-的特征峰,这表明SO4 2-成功的插入了LDH中。图2是本发明实施例1制备NiTi-LDH-SO4 2-的XRD谱图,从图中可以发现制备的样品出现了LDH的特征峰:(006)、(009)、(012)、(015)和(110),这证明了LDH成功合成。
实施例2:
NiTi-LDH-SO4 2-的制备:将六水合硝酸镍(8.72g,0.03mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,向反应容器中滴加混合盐溶液,同时通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在9.5,在室温下搅拌6小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-SO4 2-。(c(Ni2+):c(Ti4+)=3)
实施例3:
NiTi-LDH-SO4 2-的制备:将六水合硝酸镍(11.63g,0.04mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,向反应容器中滴加混合盐溶液,同时通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在9.5,在80℃下超声(200W)6小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-SO4 2-。(c(Ni2+):c(Ti4+)=4)
实施例4:
NiTi-LDH-P3O10 5-的制备:将六水合硝酸镍(5.82g,0.02mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,将三聚磷酸钠(11.04g,0.03mol)溶于20mL去离子水得到三聚磷酸钠溶液,向反应容器中同步滴加混合盐溶液和三聚磷酸钠溶液,通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在10.0,在80℃下搅拌8小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-P3O10 5-。(c(Ni2+):c(Ti4+)=2,c(P3O10 5-):c(Ti4+)=3)
实施例5:
NiTi-LDH-BO3 3-的制备:将六水合硝酸镍(5.82g,0.02mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,将硼酸(1.24g,0.02mol)溶于20mL热去离子水得到饱和硼酸溶液,向反应容器中同步滴加混合盐溶液和热饱和硼酸溶液,通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在9.0,在65℃下超声(100W)8小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-BO3 3-。(c(Ni2+):c(Ti4+)=2,c(BO3 3-):c(Ti4+)=2)
实施例6:
NiTi-LDH-WO4 2-的制备:将六水合硝酸镍(11.63g,0.04mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,将二水合钨酸钠(6.60g,0.02mol)溶于20mL去离子水得到钨酸钠溶液,向反应容器中同步滴加混合盐溶液和钨酸钠溶液,通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在8.0,在80℃下超声(300W)4小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-WO4 2-。(c(Ni2+):c(Ti4+)=4,c(WO4 2-):c(Ti4+)=2)
图3是本发明实施例6制备的NiTi-LDH-WO4 2-的红外谱图。在红外谱图中,3700cm-1到3100cm-1的钝峰为O-H拉伸振动吸收峰,1638cm-1的峰为层间水分子的弯曲振动吸收峰,779cm-1为W-O-W的拉伸振动吸收峰,672cm-1为W-O的拉伸振动吸收峰,这表明WO4 2-成功的插入了LDH中。图4是本发明实施例6制备的NiTi-LDH-WO4 2-的XRD谱图。从图中可以发现制备的样品出现了LDH的特征峰:(003)、(006)、(009)和(110),这证明了LDH成功合成。
实施例7:
NiTi-LDH-Alg-的制备:将六水合硝酸镍(5.82g,0.02mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,将海藻酸钠(6.48g,0.03mol)溶于20mL去离子水得到海藻酸钠溶液,向反应容器中同步滴加混合盐溶液和海藻酸钠溶液,通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在10.0,在60℃下搅拌8小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-Alg-。(c(Ni2+):c(Ti4+)=2,c(Alg-):c(Ti4+)=3)
实施例8:
NiTi-LDH-SiW12O40 4-的制备:将六水合硝酸镍(8.72g,0.03mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,将12-硅钨酸(5.76g,0.002mol)溶于20mL去离子水得到硅钨酸溶液,向反应容器中同步滴加混合盐溶液和硅钨酸溶液,通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在4.5,在80℃下搅拌6小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-SiW12O40 4-。(c(Ni2+):c(Ti4+)=3,c(SiW12O40 4-):c(Ti4+)=0.2)
实施例9:
NiTi-LDH-PW12O40 3-的制备:将六水合硝酸镍(8.72g,0.03mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,将磷钨酸(5.76g,0.002mol)溶于20mL去离子水得到磷钨酸溶液,向反应容器中同步滴加混合盐溶液和磷钨酸溶液,通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在4.5,在80℃下搅拌4小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-PW12O40 3-。(c(Ni2+):c(Ti4+)=3,c(PW12O40 3-):c(Ti4+)=0.2)
实施例10:
NiTi-LDH-H2PO4 -的制备:将六水合硝酸镍(11.63g,0.04mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,将二水合磷酸氢二钠(4.68g,0.03mol)溶于20mL去离子水得到磷酸氢二钠溶液,向反应容器中同步滴加混合盐溶液和磷酸氢二钠溶液,通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在8.5,在60℃下搅拌6小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-H2PO4 -。(c(Ni2+):c(Ti4+)=4,c(H2PO4 -):c(Ti4+)=3)
实施例11:
NiTi-LDH-SHMP的制备:将六水合硝酸镍(11.63g,0.04mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,将六偏磷酸钠(12.24g,0.02mol)溶于20mL去离子水得到六偏磷酸钠溶液,向反应容器中同步滴加混合盐溶液和六偏磷酸钠溶液,通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在8.0,在60℃下搅拌6小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-SHMP。(c(Ni2+):c(Ti4+)=4,c(SHMP):c(Ti4+)=2)
实施例12:
NiAl-LDH-SO4 2-的制备:将六水合硝酸镍(11.62g,0.04mol)和九水合硝酸铝(7.50g,0.02mol)溶于80mL去离子水得到混合盐溶液,将硫酸钠(2.84g,0.02mol)溶于20mL去离子水得到硫酸钠溶液,向反应容器中同步滴加混合盐溶液和硫酸钠溶液,通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在8.8,在室温下搅拌6小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiAl-LDH-SO4 2-。(c(Ni2+):c(Al3+)=2,c(SO4 2-):c(Al3+)=1)
实施例13:
NiTi-LDH-CO3 2-的制备:将六水合硝酸镍(5.82g,0.02mol)和硫酸钛(2.40g,0.01mol)溶于80mL去离子水得到混合盐溶液,将碳酸钠(2.12g,0.02mol)溶于20mL去离子水得到碳酸钠溶液,向反应容器中同步滴加混合盐溶液和碳酸钠溶液,通过1mol/L的氢氧化钠溶液调节并实时监测整个体系的pH值稳定在9.5,在室温下搅拌6小时,室温静置陈化12-24小时后过滤洗涤至中性后干燥获得NiTi-LDH-CO3 2-。(c(Ni2+):c(Ti4+)=2,c(CO3 2-):c(Ti4+)=2)
图5是本发明实施例13制备的NiTi-LDH-CO3 2-的红外谱图。在红外谱图中,3700cm-1到3100cm-1的钝峰为O-H拉伸振动吸收峰,1638cm-1的峰为层间水分子的弯曲振动吸收峰,1377cm-1和1490cm-1为CO3 2-的拉伸振动吸收峰,1100cm-1为CO3 2-的弯曲振动吸收峰,这表明CO3 2-成功的插入了LDH中。图6是本发明实施例13制备的NiTi-LDH-CO3 2-的XRD谱图。从图中可以发现制备的样品出现了LDH的特征峰:(003)、(006)、(009)和(110),这证明了LDH成功合成。
实施例14-26:
有机硅弹性体泡沫是一种高性能材料,主要应用于化学化工、航空航天和电子产品行业等领域。然而未经改性的有机硅弹性体泡沫存在阴燃和释放大量烟雾等问题,用特种阴离子插层改性的镍钛双金属氢氧化物制备高效阻燃抑烟的有机硅弹性体泡沫复合材料。
具体制备方法为:将乙烯基硅油、羟基硅油、Pt催化剂和分别与实施例1-11制备的特种阴离子插层改性的镍钛双金属氢氧化物及实施例12-13所制备的NiAl-LDH-SO4 2-及NiTi-LDH-CO3 2-在机械搅拌作用下搅拌均匀作为组分A,将羟基硅油、含氢硅油、抑制剂和水作为组分B,在机械搅拌作用下将组分B加入组分A中,搅拌均匀后快速倒入模具中,待室温静置发泡交联完毕后放于150℃烘箱中进一步硫化2h,最终得到高效阻燃抑烟的有机硅弹性体泡沫复合材料。未添加特种LDH的有机硅弹性体泡沫作为对比样。
Claims (7)
1.一种特种阴离子插层改性的镍钛双金属氢氧化物作为阻燃剂的应用,其特征在于,其中,所述特种阴离子在硫酸根(SO4 2-)、钨酸根(WO4 2-)、硅钨酸根(SiW12O40 4-)、磷钨酸根(PW12O40 3-)、硼酸根(BO3 3-)、海藻酸根(Alg-)、磷酸二氢根(H2PO4 -)、三聚磷酸根(P3O10 5-)、六偏磷酸根(SHMP)中的一种。
2.根据权利要求1所述的特种阴离子插层改性的镍钛双金属氢氧化物作为阻燃剂的应用,其特征在于,所述特种阴离子插层改性的镍钛双金属氢氧化物的制备方法,包含以下步骤:
(1)分别配制定量的六水合硝酸镍与硫酸钛混合盐溶液和特种阴离子对应的盐或酸溶液待用;(2)在室温搅拌下,向容器中同步滴加六水合硝酸镍与硫酸钛混合盐溶液和特种阴离子对应的盐或酸溶液,通过氢氧化钠溶液调节并实时监测整个体系的pH值,待体系pH稳定后于一定温度下继续搅拌或超声反应;(3)室温静置陈化后过滤洗涤至中性,纯化干燥后获得特种阴离子插层改性的镍钛双金属氢氧化物。
3.根据权利要求2所述的特种阴离子插层改性的镍钛双金属氢氧化物作为阻燃剂的应用,其特征在于,步骤(1)中,将六水合硝酸镍与硫酸钛混合盐溶液中c(Ni2+): c(Ti4+)控制在2:1-6:1,其中c(Ni2+)代表混合盐溶液中硝酸镍的物质的量浓度,c(Ti4+)代表混合盐溶液中硫酸钛的物质的量浓度。
4.根据权利要求2所述的特种阴离子插层改性的镍钛双金属氢氧化物作为阻燃剂的应用,其特征在于:步骤(1)中,将反应体系中c(An-): c(Ti4+)控制在0.2:1-3:1,其中c(An-)代表反应溶液中特种阴离子的物质的量浓度。
5.根据权利要求2所述的特种阴离子插层改性的镍钛双金属氢氧化物作为阻燃剂的应用,其特征在于:步骤(2)中,通过氢氧化钠溶液调节并实时监测整个体系的pH值范围控制在pH=4.5-10.0。
6.根据权利要求2所述的特种阴离子插层改性的镍钛双金属氢氧化物作为阻燃剂的应用,其特征在于:步骤(2)中,超声功率为100 W-300 W,超声时间为6-8小时,超声温度为20-80 oC。
7.根据权利要求1所述的特种阴离子插层改性的镍钛双金属氢氧化物作为阻燃剂的应用,其特征在于,应用于有机硅弹性体泡沫材料,阴离子插层改性的镍钛双金属氢氧化物添加量为0.5%~2.0%,有机硅弹性体泡沫材料可通过垂直燃烧FV-1或FV-0等级。
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