CN115572183A - 一种高强度耐高温隔热材料及其制备方法 - Google Patents
一种高强度耐高温隔热材料及其制备方法 Download PDFInfo
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- 239000011810 insulating material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 110
- 239000005011 phenolic resin Substances 0.000 claims abstract description 93
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 92
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 91
- 239000000835 fiber Substances 0.000 claims abstract description 87
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000002002 slurry Substances 0.000 claims abstract description 33
- 239000011268 mixed slurry Substances 0.000 claims abstract description 32
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 31
- 239000010452 phosphate Substances 0.000 claims abstract description 31
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 31
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010000 carbonizing Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 12
- 239000002131 composite material Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 39
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 27
- 229920002866 paraformaldehyde Polymers 0.000 claims description 27
- 238000003763 carbonization Methods 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 16
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical group [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 14
- 239000001095 magnesium carbonate Substances 0.000 claims description 13
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 13
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 13
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 13
- 229920002401 polyacrylamide Polymers 0.000 claims description 13
- -1 chromium phosphate-ammonium phosphate Chemical compound 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 description 25
- 239000012774 insulation material Substances 0.000 description 21
- 238000003756 stirring Methods 0.000 description 17
- 238000005303 weighing Methods 0.000 description 16
- 238000009413 insulation Methods 0.000 description 15
- 239000012299 nitrogen atmosphere Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 238000005187 foaming Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 239000004254 Ammonium phosphate Substances 0.000 description 3
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 3
- 235000019289 ammonium phosphates Nutrition 0.000 description 3
- 229910000151 chromium(III) phosphate Inorganic materials 0.000 description 3
- IKZBVTPSNGOVRJ-UHFFFAOYSA-K chromium(iii) phosphate Chemical compound [Cr+3].[O-]P([O-])([O-])=O IKZBVTPSNGOVRJ-UHFFFAOYSA-K 0.000 description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 3
- 239000004966 Carbon aerogel Substances 0.000 description 2
- 238000002679 ablation Methods 0.000 description 2
- 239000004964 aerogel Substances 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 239000013384 organic framework Substances 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
本发明涉及一种高强度耐高温隔热材料及其制备方法。所述方法包括如下步骤:用水将氧化锆纤维与分散助剂分散均匀,得到纤维料浆;往所述纤维料浆中加入镁砂和磷酸盐并分散均匀,得到混合浆料;用醇溶剂将酚醛树脂与固化剂混合均匀,得到酚醛树脂溶液;将所述混合浆料和所述酚醛树脂溶液混合均匀并进行反应,经干燥,得到复合隔热材料;将所述复合隔热材料进行碳化,制得高强度耐高温隔热材料。本发明制备的是一种有机无机杂化的新型高强度耐高温隔热材料,具有耐高温性能好且兼具有高温隔热性能优异以及高温力学性能优异的特点。
Description
技术领域
本发明属于隔热材料技术领域,尤其涉及一种高强度耐高温隔热材料及其制备方法。
背景技术
随着我国飞行器朝着长航时、高马赫数发展,对隔热材料耐温性能提出了新的要求。当飞行器以高马赫的速度在大气层中飞行时其头锥处的温度超过1800℃,为使其内部仪器设备能在合适的温度范围内工作,必须采用高效的热防护系统。
现阶段,各类飞行器的高效防隔热材料主要有非烧蚀隔热材料和烧蚀隔热材料两种。非烧蚀材料主要包括陶瓷气凝胶和隔热瓦,其中,气凝胶超细纳米颗粒组装的三维纳米结构材料,其隔热性能优异,但是耐温性有限,最高使用温度在1200℃以下;隔热瓦耐温性较好,现有报道的隔热瓦的耐温性可以提升至1500℃,但是材料是以微米级纤维为主体的隔热材料,材料隔热性能较差,尤其是高温隔热性能不足。此外,现有的隔热材料还存在维型性能差、高温结构强度不足,尤其是当使用温度超过1500℃,由于隔热材料高温力学性能不足,导致隔热材料高温稳定性较差。目前,现有的隔热材料无法兼具耐高温、高温隔热性能以及高温力学性能优异的特点。
综上,非常有必要提供一种高强度耐高温隔热材料及其制备方法。
发明内容
为了解决现有技术中存在的一个或者多个技术问题,本发明提供了一种高强度耐高温隔热材料及其制备方法。本发明制备的是一种有机无机杂化的新型高强度耐高温隔热材料,是一种磷酸盐镁基杂化的碳基隔热材料,具有耐高温性能好且兼具有高温隔热性能优异以及高温力学性能优异的特点。
本发明在第一方面提供了一种高强度耐高温隔热材料的制备方法,所述方法包括如下步骤:
(1)用水将氧化锆纤维与分散助剂分散均匀,得到纤维料浆;
(2)往所述纤维料浆中加入镁砂和磷酸盐并分散均匀,得到混合浆料;
(3)用醇溶剂将酚醛树脂与固化剂混合均匀,得到酚醛树脂溶液;
(4)将所述混合浆料和所述酚醛树脂溶液混合均匀并进行反应,经干燥,得到复合隔热材料;
(5)将所述复合隔热材料进行碳化,制得高强度耐高温隔热材料。
优选地,所述氧化锆纤维为超细氧化锆纤维,所述氧化锆纤维的直径为1~3μm;和/或所述分散助剂为聚丙烯酰胺。
优选地,所述纤维料浆中含有的氧化锆纤维的质量分数为5~15%。
优选地,所述镁砂为超细镁砂,所述镁砂的直径为1~3μm;和/或所述磷酸盐为磷酸二氢铝和/或磷酸铬-磷酸铵。
优选地,所述氧化锆纤维、所述镁砂与所述磷酸盐的质量比为(1~2):(10~15):(1~5)。
优选地,所述醇溶剂为甲醇和/或乙醇;和/或所述固化剂为多聚甲醛;所述酚醛树脂溶液中含有的酚醛树脂的质量分数之和为20~40%。
优选地,所述混合浆料与所述酚醛树脂溶液的体积比为1:(1~3)。
优选地,所述反应的温度为90~120℃,所述反应的时间为12~24h;和/或所述干燥的温度为80~100℃,所述干燥的时间为12~30h。
优选地,所述碳化的温度为400~600℃,所述碳化的时间为12~30h。
本发明在第二方面提供了由本发明在第一方面所述的制备方法制得的高强度耐高温隔热材料。
本发明与现有技术相比至少具有如下有益效果:
(1)本发明以氧化锆纤维为增强体,以耐超高温的镁砂为无机隔热组分,以磷酸盐为发泡剂,通过磷酸盐的发泡以及与镁砂的刚性键联作用,用于隔热材料孔结构和高强度无机网络结构的构建,充分发挥磷酸盐基隔热材料的结构强度大与耐温性突出的优势,对于提升隔热材料的高温力学强度和维形性至关重要;并且,本发明引入酚醛树脂,除了产生的酚醛结构网络经高温碳化之后形成碳气凝胶还具有较好的抗辐射性能和烧蚀隔热的作用之外,更重要的是,本发明发现,通过将包含有氧化锆纤维、镁砂和磷酸盐的混合浆料与酚醛树脂溶液混合的方式引入酚醛树脂,这样可以酚醛树脂为有机骨架定型剂,可以防止磷酸盐的无序发泡,使得磷酸盐基隔热材料受酚醛网络结构束缚,获得了更为规整的孔结构,从而有效解决无机有机杂化材料耐温性能不足,高温难维形以及高温抗辐射性能差的技术问题,为高强度磷酸基杂化碳基隔热材料的工程化应用奠定了基础。
(2)本发明中的高强度耐高温隔热材料可以耐温达到1800℃,1800℃处理0.5h后,收缩率不超过5%,具有耐高温性能优异的特点,且同时兼具高温隔热性能优异以及高温力学性能优异的特点,1500℃导热系数不超过0.17W/(m·K),并且高温压缩强度不小于0.12MPa,具有耐高温高强度高温隔热性能优异的优势。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面将结合本发明实施例,对本发明的技术方案进行清楚、完整地描述。显然,所描述的实施例是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例,都属于本发明保护的范围。
本发明在第一方面提供了一种高强度耐高温隔热材料的制备方法,所述方法包括如下步骤:
(1)用水将氧化锆纤维与分散助剂分散均匀,得到纤维料浆;具体地,例如称取氧化锆纤维(例如超细氧化锆纤维)加入水中,之后加入分散助剂,搅拌分散均匀,获得纤维料浆;在本发明中,所述分散助剂的用量为所述氧化锆纤维的质量的0.8~1.5%优选为1%。
(2)往所述纤维料浆中加入镁砂和磷酸盐并分散均匀,得到混合浆料;具体地,例如称取镁砂(例如超细镁砂)和磷酸盐,加入上述纤维料浆中,搅拌分散均匀,获得具有一定粘度的水系浆料,即获得混合浆料;
(3)用醇溶剂将酚醛树脂与固化剂混合均匀,得到酚醛树脂溶液;在本发明中,所述固化剂的用量例如为所述酚醛树脂的质量的4~6%优选为5%;具体地,例如将酚醛树脂溶于醇溶剂中,同时加入固化剂(例如多聚甲醛),获得醇系酚醛树脂溶液,即获得酚醛树脂溶液;本发明对酚醛树脂不做具体的限定,采用市面上可以直接购买的产品即可或者通过现有方法合成的酚醛树脂均可,所述酚醛树脂的CAS号例如为9003-35-4;
(4)将所述混合浆料和所述酚醛树脂溶液混合均匀并进行反应,经干燥,得到复合隔热材料;具体地,例如将所述混合浆料和所述酚醛树脂溶液,搅拌分散均匀后置于高温反应釜中密闭反应,待反应结束后从反应釜中取出材料进行干燥,例如在90℃烘箱干燥24h,得到所述复合隔热材料;
(5)将所述复合隔热材料进行碳化,制得高强度耐高温隔热材料;具体地,例如将上述复合隔热材料置于碳化炉,在氮气气氛中碳化24h,获得高强度耐高温隔热材料。
本发明以氧化锆纤维为增强体,以耐超高温的镁砂为无机隔热组分,以磷酸盐为发泡剂,通过磷酸盐的发泡以及与镁砂的刚性键联作用,用于隔热材料孔结构和高强度无机网络结构的构建,充分发挥磷酸盐基隔热材料的结构强度大与耐温性突出的优势,对于提升隔热材料的高温力学强度和维形性至关重要;并且,本发明引入酚醛树脂,除了产生的酚醛结构网络经高温碳化之后形成碳气凝胶还具有较好的抗辐射性能和烧蚀隔热的作用之外,更重要的是,本发明发现,通过将包含有氧化锆纤维、镁砂和磷酸盐的混合浆料与酚醛树脂溶液混合的方式引入酚醛树脂,这样可以酚醛树脂为有机骨架定型剂,可以防止磷酸盐的无序发泡,使得磷酸盐基隔热材料受酚醛网络结构束缚,获得了更为规整的孔结构,从而有效解决无机有机杂化材料耐温性能不足,高温难维形以及高温抗辐射性能差的技术问题,为高强度磷酸基杂化碳基隔热材料的工程化应用奠定了基础。
根据一些优选的实施方式,所述氧化锆纤维为超细氧化锆纤维,所述氧化锆纤维的直径为1~3μm;本发明对超细氧化锆纤维不做具体的限定,采用市面上可以购买的产品或者通过现有的方法得到均可,在本发明中,优选为所述氧化锆为超细氧化锆纤维,具体为直径为1~3um的氧化锆纤维;和/或所述分散助剂为聚丙烯酰胺;本发明对所述聚丙烯酰胺不做具体的限定,采用市面上可以直接购买的产品或者通过现有方法合成均可,所述聚丙烯酰胺的CAS号例如为9003-05-8。
根据一些优选的实施方式,所述纤维料浆中含有的氧化锆纤维的质量分数为5~15%(例如5%、6%、7%、8%、9%、10%、11%、12%、13%、14%或15%)。
根据一些优选的实施方式,所述镁砂为超细镁砂,所述镁砂的直径(粒度)为1~3μm;本发明对超细镁砂不做具体的限定,采用市面上可以直接购买的产品,具体地,在本发明中,所述超细镁砂指的是粒度为1~3μm的镁砂;和/或所述磷酸盐为磷酸二氢铝和/或磷酸铬-磷酸铵,在本发明中,磷酸铬-磷酸铵为磷酸铬与磷酸铵的混合物,所述磷酸铵的用量为磷酸铬的质量的10~20%。
根据一些优选的实施方式,所述氧化锆纤维、所述镁砂与所述磷酸盐的质量比为(1~2):(10~15):(1~5)(例如1:10:1、1:11:1、1:12:1、1:13:1、1:14:1、1:15:1、1:10:2、1:11:2、1:12:2、1:13:2、1:14:2、1:15:2、1:10:3、1:11:3、1:12:3、1:13:3、1:14:3、1:15:3、1:10:4、1:11:4、1:12:4、1:13:4、1:14:4、1:15:4、1:10:5、1:11:5、1:12:5、1:13:5、1:14:5、1:15:5、2:10:1、2:11:1、2:12:1、2:13:1、2:14:1、2:15:1、2:10:2、2:11:2、2:12:2、2:13:2、2:14:2、2:15:2、2:10:3、2:11:3、2:12:3、2:13:3、2:14:3、2:15:3、2:10:4、2:11:4、2:12:4、2:13:4、2:14:4、2:15:4、2:10:5、2:11:5、2:12:5、2:13:5、2:14:5或2:15:5),更优选为(1~2):(10~15):(2~5)。在本发明中,优选为所述氧化锆纤维、所述镁砂与所述磷酸盐的质量比为(1~2):(10~15):(1~5),若镁砂过多,材料密度增大,固相导热升高,不利于隔热性能提升;而若磷酸盐过多,无序发泡较难控制,材料孔结构不太可控,影响隔热材料的隔热性能和力学性能;而若镁砂和磷酸盐的用量过少,则会对隔热材料孔结构和高强度无机网络结构的构建不充分,同样对于隔热材料的高温隔热性能和高温力学性能提升作用不明显。
根据一些优选的实施方式,所述醇溶剂为甲醇和/或乙醇;和/或所述固化剂为多聚甲醛;本发明对所述多聚甲醛不做具体的限定,采用市面上可以直接购买的产品即可;所述酚醛树脂溶液中含有的酚醛树脂的质量分数为20~40%(例如20%、25%、30%、35%或40%)。
根据一些优选的实施方式,所述混合浆料与所述酚醛树脂溶液的体积比为1:(1~3)(例如1:1、1:1.5、1:2、1:2.5或1:3)。在本发明中,优选为所述混合浆料与所述酚醛树脂溶液的体积比为1:(1~3),并且优选为所述酚醛树脂溶液中含有的酚醛树脂的质量分数为20~40%,若酚醛树脂含量过大,材料含碳量过多,低气压环境氧化会比较严重,不利于隔热材料的高温隔热性能和高温力学性能的提升,而若酚醛树脂含量过少,则难以抑制磷酸盐的无序发泡,同样不利于隔热材料的高温隔热性能和高温力学性能的提升。
根据一些优选的实施方式,所述反应的温度为90~120℃(例如90℃、100℃、110℃或120℃),所述反应的时间为12~24h(例如12、14、16、18、20、22或24h);和/或所述干燥的温度为80~100℃(例如80℃、90℃或100℃),所述干燥的时间为12~30h(例如12、15、18、20、24或30h)。
根据一些优选的实施方式,所述碳化的温度为400~600℃(例如400℃、450℃、500℃、550℃或600℃),所述碳化的时间为12~30h(例如12、15、18、20、24或30h)。
本发明在第二方面提供了由本发明在第一方面所述的制备方法制得的高强度耐高温隔热材料。
下文将通过举例的方式对本发明进行进一步的说明,但是本发明的保护范围不限于这些实施例。
实施例1
①称取5份超细氧化锆纤维加入95份水中,再加入超细氧化锆纤维的质量的1%的分散助剂聚丙烯酰胺,搅拌分散均匀,获得纤维料浆。
②称取75份超细镁砂和5份磷酸二氢铝,加入上述纤维料浆中,搅拌分散均匀,获得混合浆料。
③将酚醛树脂溶于乙醇中,同时加入固化剂多聚甲醛(多聚甲醛的用量为酚醛树脂质量的5%),获得含有酚醛树脂的质量分数为20%的酚醛树脂溶液。
④将混合浆料与酚醛树脂溶液按体积比1:1混合,搅拌分散均匀后置于反应釜中90℃密闭反应24h,待反应结束后取出材料在90℃烘箱干燥24h。
⑤将上述干燥后的材料置于碳化炉中在氮气气氛中500℃碳化24h,获得高强度耐高温隔热材料。
实施例2
①称取10份超细氧化锆纤维加入90份水中,再加入超细氧化锆纤维的质量的1%的分散助剂聚丙烯酰胺,搅拌分散均匀,获得纤维料浆。
②称取100份超细镁砂和25份磷酸二氢铝,加入上述纤维料浆中,搅拌分散均匀,获得混合浆料。
③将酚醛树脂溶于甲醇中,同时加入固化剂多聚甲醛(多聚甲醛的用量为酚醛树脂质量的5%),获得含有酚醛树脂的质量分数为20%的酚醛树脂溶液。
④将混合浆料与酚醛树脂溶液按体积比1:1混合,搅拌分散均匀后置于反应釜中120℃密闭反应12h,待反应结束后取出材料在90℃烘箱干燥24h。
⑤将上述干燥后的材料置于碳化炉中在氮气气氛中500℃碳化24h,获得高强度耐高温隔热材料。
实施例3
①称取15份超细氧化锆纤维加入85份水中,再加入超细氧化锆纤维的质量的1%的分散助剂聚丙烯酰胺,搅拌分散均匀,获得纤维料浆。
②称取150份超细镁砂和75份磷酸二氢铝,加入上述纤维料浆中,搅拌分散均匀,获得混合浆料。
③将酚醛树脂溶于甲醇中,同时加入固化剂多聚甲醛(多聚甲醛的用量为酚醛树脂质量的5%),获得含有酚醛树脂的质量分数为20%的酚醛树脂溶液。
④将混合浆料与酚醛树脂溶液按体积比1:3混合,搅拌分散均匀后置于反应釜中120℃密闭反应12h,待反应结束后取出材料在90℃烘箱干燥24h。
⑤将上述干燥后的材料置于碳化炉中在氮气气氛中500℃碳化24h,获得高强度耐高温隔热材料。
实施例4
①称取10份超细氧化锆纤维加入90份水中,再加入超细氧化锆纤维的质量的1%的分散助剂聚丙烯酰胺,搅拌分散均匀,获得纤维料浆。
②称取100份超细镁砂和25份磷酸二氢铝,加入上述纤维料浆中,搅拌分散均匀,获得混合浆料。
③将酚醛树脂溶于甲醇中,同时加入固化剂多聚甲醛(多聚甲醛的用量为酚醛树脂质量的5%),获得含有酚醛树脂的质量分数为20%的酚醛树脂溶液。
④将混合浆料与酚醛树脂溶液按体积比1:2混合,搅拌分散均匀后置于反应釜中110℃密闭反应15h,待反应结束后取出材料在90℃烘箱干燥24h。
⑤将上述干燥后的材料置于碳化炉中在氮气气氛中500℃碳化24h,获得高强度耐高温隔热材料。
实施例5
①称取10份超细氧化锆纤维加入90份水中,再加入超细氧化锆纤维的质量的1%的分散助剂聚丙烯酰胺,搅拌分散均匀,获得纤维料浆。
②称取100份超细镁砂和30份磷酸二氢铝,加入上述纤维料浆中,搅拌分散均匀,获得混合浆料。
③将酚醛树脂溶于甲醇中,同时加入固化剂多聚甲醛(多聚甲醛的用量为酚醛树脂质量的5%),获得含有酚醛树脂的质量分数为30%的酚醛树脂溶液。
④将混合浆料与酚醛树脂溶液按体积比1:1混合,搅拌分散均匀后置于反应釜中120℃密闭反应12h,待反应结束后取出材料在90℃烘箱干燥24h。
⑤将上述干燥后的材料置于碳化炉中在氮气气氛中500℃碳化24h,获得高强度耐高温隔热材料。
实施例6
①称取10份超细氧化锆纤维加入90份水中,再加入超细氧化锆纤维的质量的1%的分散助剂聚丙烯酰胺,搅拌分散均匀,获得纤维料浆。
②称取100份超细镁砂和30份磷酸铬-磷酸铵(磷酸铵的用量为磷酸铬的质量的15%),加入上述纤维料浆中,搅拌分散均匀,获得混合浆料。
③将酚醛树脂溶于甲醇中,同时加入固化剂多聚甲醛(多聚甲醛的用量为酚醛树脂质量的5%),获得含有酚醛树脂的质量分数为30%的酚醛树脂溶液。
④将混合浆料与酚醛树脂溶液按体积比1:1混合,搅拌分散均匀后置于反应釜中120℃密闭反应12h,待反应结束后取出材料在90℃烘箱干燥24h。
⑤将上述干燥后的材料置于碳化炉中在氮气气氛中500℃碳化24h,获得高强度耐高温隔热材料。
实施例7
实施例7与实施例5基本相同,不同之处在于:
步骤②为:称取90份超细镁砂和8份磷酸二氢铝,加入上述纤维料浆中,搅拌分散均匀,获得混合浆料。
实施例8
实施例8与实施例5基本相同,不同之处在于:
步骤②为:称取160份超细镁砂和60份磷酸二氢铝,加入上述纤维料浆中,搅拌分散均匀,获得混合浆料。
实施例9
实施例9与实施例5基本相同,不同之处在于:
步骤③为:将酚醛树脂溶于甲醇中,同时加入固化剂多聚甲醛(多聚甲醛的用量为酚醛树脂质量的5%),获得含有酚醛树脂的质量分数为15%的酚醛树脂溶液。
步骤④为:将混合浆料与酚醛树脂溶液按体积比1:0.8混合,搅拌分散均匀后置于反应釜中120℃密闭反应12h,待反应结束后取出材料在90℃烘箱干燥24h。
实施例10
实施例10与实施例5基本相同,不同之处在于:
步骤③为:将酚醛树脂溶于甲醇中,同时加入固化剂多聚甲醛(多聚甲醛的用量为酚醛树脂质量的5%),获得含有酚醛树脂的质量分数为40%的酚醛树脂溶液。
步骤④为:将混合浆料与酚醛树脂溶液按体积比1:3.5混合,搅拌分散均匀后置于反应釜中120℃密闭反应12h,待反应结束后取出材料在90℃烘箱干燥24h。
对比例1
①称取10份超细氧化锆纤维加入90份水中,再加入超细氧化锆纤维的质量的1%的分散助剂聚丙烯酰胺,搅拌分散均匀,获得纤维料浆。
②称取100份超细镁砂和30份磷酸二氢铝,加入上述纤维料浆中,搅拌分散均匀,置于反应釜中120℃密闭反应24h,获得隔热材料。
对比例2
①将酚醛树脂溶于甲醇中,同时加入固化剂多聚甲醛(多聚甲醛的用量为酚醛树脂质量的5%),获得含有酚醛树脂的质量分数为30%的酚醛树脂溶液,搅拌分散均匀后置于反应釜中120℃密闭反应12h,待反应结束后取出材料在90℃烘箱干燥24h。
②将上述干燥后的材料置于碳化炉中在氮气气氛中500℃碳化24h,获得隔热材料。
对比例3
①称取100份超细镁砂、30份磷酸二氢铝和30份酚醛树脂分散于65份甲醇中,同时加入固化剂多聚甲醛(多聚甲醛的用量为酚醛树脂质量的5%),搅拌分散均匀后置于反应釜中120℃密闭反应12h,待反应结束后取出材料在90℃烘箱干燥24h。
②将上述干燥后的材料置于碳化炉中在氮气气氛中500℃碳化24h,获得隔热材料。
对比例4
①称取10份超细氧化锆纤维加入90份水中,再加入超细氧化锆纤维的质量的1%的分散助剂聚丙烯酰胺,搅拌分散均匀,获得纤维料浆。
②将酚醛树脂溶于甲醇中,同时加入固化剂多聚甲醛(多聚甲醛的用量为酚醛树脂质量的5%),获得含有酚醛树脂的质量分数为30%的酚醛树脂溶液。
③将纤维料浆与酚醛树脂溶液按体积比1:1混合,搅拌分散均匀后置于反应釜中120℃密闭反应12h,待反应结束后取出材料在90℃烘箱干燥24h。
④将上述干燥后的材料置于碳化炉中在氮气气氛中500℃碳化24h,获得隔热材料。
本发明对各实施例和各对比例最终制备的隔热材料进行1500℃导热系数的测定以及1500℃压缩强度的测定,并且还对各实施例以及各对比例最终制备的材料进行了1800℃收缩率的测定,结果如表1所示;其中,收缩率的测定为:将各实施例和各对比例最终制备的材料在10kPa气压空气气氛条件下1800℃处理0.5h,测得材料热面(朝向1800℃热源的一面)相比未经过1800℃处理0.5h前在长度方向上的收缩率。
表1:各实施例以及各对比例最终制得的隔热材料的性能。
本发明各实施例以及各对比例中涉及的“份”,均指的是“重量份”,单位例如可以统一取“g”或“kg”等重量单位。
本发明未详细说明部分为本领域技术人员公知技术。
最后应说明的是:以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (10)
1.一种高强度耐高温隔热材料的制备方法,其特征在于,所述方法包括如下步骤:
(1)用水将氧化锆纤维与分散助剂分散均匀,得到纤维料浆;
(2)往所述纤维料浆中加入镁砂和磷酸盐并分散均匀,得到混合浆料;
(3)用醇溶剂将酚醛树脂与固化剂混合均匀,得到酚醛树脂溶液;
(4)将所述混合浆料和所述酚醛树脂溶液混合均匀并进行反应,经干燥,得到复合隔热材料;
(5)将所述复合隔热材料进行碳化,制得高强度耐高温隔热材料。
2.根据权利要求1所述的制备方法,其特征在于:
所述氧化锆纤维为超细氧化锆纤维,所述氧化锆纤维的直径为1~3μm;和/或
所述分散助剂为聚丙烯酰胺。
3.根据权利要求1所述的制备方法,其特征在于:
所述纤维料浆中含有的氧化锆纤维的质量分数为5~15%。
4.根据权利要求1所述的制备方法,其特征在于:
所述镁砂为超细镁砂,所述镁砂的直径为1~3μm;和/或
所述磷酸盐为磷酸二氢铝和/或磷酸铬-磷酸铵。
5.根据权利要求1所述的制备方法,其特征在于:
所述氧化锆纤维、所述镁砂与所述磷酸盐的质量比为(1~2):(10~15):(1~5)。
6.根据权利要求1所述的制备方法,其特征在于:
所述醇溶剂为甲醇和/或乙醇;和/或
所述固化剂为多聚甲醛;
所述酚醛树脂溶液中含有的酚醛树脂的质量分数为20~40%。
7.根据权利要求1所述的制备方法,其特征在于:
所述混合浆料与所述酚醛树脂溶液的体积比为1:(1~3)。
8.根据权利要求1所述的制备方法,其特征在于:
所述反应的温度为90~120℃,所述反应的时间为12~24h;和/或
所述干燥的温度为80~100℃,所述干燥的时间为12~30h。
9.根据权利要求1所述的制备方法,其特征在于:
所述碳化的温度为400~600℃,所述碳化的时间为12~30h。
10.由权利要求1至9中任一项所述的制备方法制得的高强度耐高温隔热材料。
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