CN115612245A - 一种酚醛树脂保温材料及其制备方法 - Google Patents
一种酚醛树脂保温材料及其制备方法 Download PDFInfo
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229920001568 phenolic resin Polymers 0.000 title claims abstract description 63
- 239000005011 phenolic resin Substances 0.000 title claims abstract description 63
- 239000012774 insulation material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000011810 insulating material Substances 0.000 claims abstract description 14
- -1 polysiloxane Polymers 0.000 claims abstract description 14
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 13
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 13
- 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 12
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims abstract description 11
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- BZQKBFHEWDPQHD-UHFFFAOYSA-N 1,2,3,4,5-pentabromo-6-[2-(2,3,4,5,6-pentabromophenyl)ethyl]benzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1CCC1=C(Br)C(Br)=C(Br)C(Br)=C1Br BZQKBFHEWDPQHD-UHFFFAOYSA-N 0.000 claims abstract description 9
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 9
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- HLVFKOKELQSXIQ-UHFFFAOYSA-N 1-bromo-2-methylpropane Chemical compound CC(C)CBr HLVFKOKELQSXIQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 3
- ZRSKSQHEOZFGLJ-UHFFFAOYSA-N ammonium adipate Chemical group [NH4+].[NH4+].[O-]C(=O)CCCCC([O-])=O ZRSKSQHEOZFGLJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 3
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 3
- OCJKUQIPRNZDTK-UHFFFAOYSA-N ethyl 4,4,4-trifluoro-3-oxobutanoate Chemical compound CCOC(=O)CC(=O)C(F)(F)F OCJKUQIPRNZDTK-UHFFFAOYSA-N 0.000 claims description 3
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims description 3
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 3
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 3
- 235000019293 ammonium adipate Nutrition 0.000 claims description 2
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
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- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
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- 230000011218 segmentation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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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
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Abstract
本发明提供了一种酚醛树脂保温材料及其制备方法。包括酚醛树脂、聚硅氧烷交联剂、二苯甲烷二异氰酸酯、有机硅油、三羟甲基丙烷、十溴二苯乙烷、正庚烷、发泡剂、阻燃剂、催化剂、固化剂、稳定剂。本发明对酚醛树脂保温材料的组方进行了改进，通过配方成分的优化改良使保温材料的物理性能得到显著改善；同时提供了一种全新的制备方法。该方法首先在氯化钴和硫酸锌催化下制备酚醛树脂，并利用2‑溴异丁酸叔丁酯进行改性；对于所得的改性酚醛树脂，以分段工艺与聚硅氧烷交联剂、二苯甲烷二异氰酸酯、三羟甲基丙烷等成分进行复配。本发明酚醛树脂保温材料有效改善了粘接性能，而且抗压抗折能力得到显著提升，具有突出的技术优势。
Description
技术领域
本发明涉及保温材料技术领域，具体涉及一种酚醛树脂保温材料及其制备方法。
背景技术
酚醛树脂是苯酚和甲醛缩聚而成，其发泡物。酚醛树脂经过发泡固化后，基本没有有害物质。酚醛泡沫材料属高分子有机硬质铝箔泡沫产品，是由热固性酚醛树脂发泡而成，它具有轻质、防火、遇明火不燃烧、无烟、无毒、无滴落，使用温度围广(-196～+200℃)低温环境下不收缩、不脆化，是暖通制冷工程理想的绝热材料，由于酚醛泡沫闭孔率高，则导热系数低，隔热性能好，并具有抗水性和水蒸气渗透性，是理想的保温节能材料。
酚醛树脂保温材料可以有效解决建筑防火保温问题，在高温下不熔滴、不软化、发烟量低，不扩散火焰，耐火焰穿透，防火性能出色，并且具有良好的保温节能效果，将优异的防火性能与良好的节能效果集于一身，适合于外墙外保温；也可以与饰面层复合制作保温装饰一体化板，还可以用于构筑传统EPS/XPS/PU外墙保温系统防火隔离带，用作幕墙内的防火保温隔热材料、防火门内隔热材料，以及低温或高温场合的防火保温隔热材料。尽管在保温性、防火性等方面具有以上优势，但目前常规酚醛树脂保温材料的物理性能不是很好，尤其是粘结性不好，因此只能用于特定的保温工程当中；而且，常规酚醛树脂保温材料质地较脆，容易粉化抗压抗折能力差，因而极大限制了此类材料在建筑保温中的应用。
发明内容
本发明旨在针对现有技术的技术缺陷，提供一种酚醛树脂保温材料及其制备方法，以解决常规酚醛树脂保温材料物理性能有待改善的技术问题。
为实现以上技术目的，本发明采用以下技术方案：
一种酚醛树脂保温材料，包括以下重量份的成分：酚醛树脂80～95份，聚硅氧烷交联剂2～8份，二苯甲烷二异氰酸酯4～8份，有机硅油1～5份，三羟甲基丙烷1～3份，十溴二苯乙烷1～5份，正庚烷2～8份，发泡剂0.5～1份，阻燃剂0.5～1.5份，催化剂0.2～0.8份，固化剂0.1～0.3份，稳定剂0.5～0.8份。
作为优选，所述发泡剂为环氧乙烷或溴代异丁烷。
作为优选，所述阻燃剂为三聚磷酸铝或三聚氰胺氰尿酸盐。
作为优选，所述催化剂为二铵己二酸，三氟乙酰乙酸乙酯或1,6-己二胺盐酸盐。
作为优选，所述固化剂为脂环胺类固化剂或聚琉醇类固化剂。
作为优选，所述稳定剂为聚磷酸铵或钛酸正丁酯。
在以上技术方案的基础上，本发明进一步提供了上述酚醛树脂保温材料对的制备方法，包括以下步骤：
1)向反应容器中加入氯化钴和硫酸锌，以氮气置换反应容器中的空气，而后在80℃条件下保持20min，向其中加入苯酚，甲醛和盐酸，以120～160℃的温度2～3.5Mpa的压力反应10～20min，而后恢复至常压，再向其中加入2-溴异丁酸叔丁酯继续反应5～10min；
2)收集步骤1)所得产物，在4～6℃环境中保持20min，向其中加入硫酸锌，在搅拌状态下降温至0～1℃，收集析出的固体，清洗后以30～40℃的温度减压干燥，即得到酚醛树脂；
3)取配方量的步骤2)所得的酚醛树脂，在氮气保护下升温至120～130℃直至熔融，而后向其中加入配方量的聚硅氧烷交联剂，二苯甲烷二异氰酸酯，有机硅油，三羟甲基丙烷，十溴二苯乙烷，搅拌使其溶解，降温至100～110℃，再向其中加入配方量的正庚烷，发泡剂，阻燃剂，催化剂，固化剂，稳定剂，过程中保持搅拌且超声震荡状态，而后将体系温度以不高于0.5℃/min的温度降温至常温，即得到所述酚醛树脂保温材料。
作为优选，步骤1)中氯化钴，硫酸锌，苯酚三者的摩尔比为1:0.3:0.875。
作为优选，步骤2)中清洗的水温为30～50℃。
作为优选，步骤3)中超声震荡的频率为20～40KHz。
本发明提供了一种酚醛树脂保温材料及其制备方法。该技术方案对酚醛树脂保温材料的组方进行了改进，通过配方成分的优化改良使保温材料的物理性能得到显著改善；同时提供了一种全新的制备方法。该方法首先在氯化钴和硫酸锌催化下制备酚醛树脂，并利用2-溴异丁酸叔丁酯进行改性；对于所得的改性酚醛树脂，以分段工艺与聚硅氧烷交联剂、二苯甲烷二异氰酸酯、三羟甲基丙烷等成分进行复配。本发明酚醛树脂保温材料有效改善了粘接性能，而且抗压抗折能力得到显著提升，具有突出的技术优势。
具体实施方式
以下将对本发明的具体实施方式进行详细描述。为了避免过多不必要的细节，在以下实施例中对属于公知的结构或功能将不进行详细描述。以下实施例中所使用的近似性语言可用于定量表述，表明在不改变基本功能的情况下可允许数量有一定的变动。除有定义外，以下实施例中所用的技术和科学术语具有与本发明所属领域技术人员普遍理解的相同含义。
实施例1
一种酚醛树脂保温材料，包括以下重量份的成分：酚醛树脂80～95份，聚硅氧烷交联剂2～8份，二苯甲烷二异氰酸酯4～8份，有机硅油1～5份，三羟甲基丙烷1～3份，十溴二苯乙烷1～5份，正庚烷2～8份，发泡剂0.5～1份，阻燃剂0.5～1.5份，催化剂0.2～0.8份，固化剂0.1～0.3份，稳定剂0.5～0.8份。
上述酚醛树脂保温材料对的制备方法，包括以下步骤：
1)向反应容器中加入氯化钴和硫酸锌，以氮气置换反应容器中的空气，而后在80℃条件下保持20min，向其中加入苯酚，甲醛和盐酸，以120～160℃的温度2～3.5Mpa的压力反应10～20min，而后恢复至常压，再向其中加入2-溴异丁酸叔丁酯继续反应5～10min；
2)收集步骤1)所得产物，在4～6℃环境中保持20min，向其中加入硫酸锌，在搅拌状态下降温至0～1℃，收集析出的固体，清洗后以30～40℃的温度减压干燥，即得到酚醛树脂；
3)取配方量的步骤2)所得的酚醛树脂，在氮气保护下升温至120～130℃直至熔融，而后向其中加入配方量的聚硅氧烷交联剂，二苯甲烷二异氰酸酯，有机硅油，三羟甲基丙烷，十溴二苯乙烷，搅拌使其溶解，降温至100～110℃，再向其中加入配方量的正庚烷，发泡剂，阻燃剂，催化剂，固化剂，稳定剂，过程中保持搅拌且超声震荡状态，而后将体系温度以不高于0.5℃/min的温度降温至常温，即得到所述酚醛树脂保温材料。
实施例2
一种酚醛树脂保温材料，包括以下重量份的成分：酚醛树脂80～95份，聚硅氧烷交联剂2～8份，二苯甲烷二异氰酸酯4～8份，有机硅油1～5份，三羟甲基丙烷1～3份，十溴二苯乙烷1～5份，正庚烷2～8份，发泡剂0.5～1份，阻燃剂0.5～1.5份，催化剂0.2～0.8份，固化剂0.1～0.3份，稳定剂0.5～0.8份。
其中，所述发泡剂为环氧乙烷或溴代异丁烷。所述阻燃剂为三聚磷酸铝或三聚氰胺氰尿酸盐。所述催化剂为二铵己二酸，三氟乙酰乙酸乙酯或1,6-己二胺盐酸盐。所述固化剂为脂环胺类固化剂或聚琉醇类固化剂。所述稳定剂为聚磷酸铵或钛酸正丁酯。
上述酚醛树脂保温材料对的制备方法，包括以下步骤：
1)向反应容器中加入氯化钴和硫酸锌，以氮气置换反应容器中的空气，而后在80℃条件下保持20min，向其中加入苯酚，甲醛和盐酸，以120～160℃的温度2～3.5Mpa的压力反应10～20min，而后恢复至常压，再向其中加入2-溴异丁酸叔丁酯继续反应5～10min；
2)收集步骤1)所得产物，在4～6℃环境中保持20min，向其中加入硫酸锌，在搅拌状态下降温至0～1℃，收集析出的固体，清洗后以30～40℃的温度减压干燥，即得到酚醛树脂；
3)取配方量的步骤2)所得的酚醛树脂，在氮气保护下升温至120～130℃直至熔融，而后向其中加入配方量的聚硅氧烷交联剂，二苯甲烷二异氰酸酯，有机硅油，三羟甲基丙烷，十溴二苯乙烷，搅拌使其溶解，降温至100～110℃，再向其中加入配方量的正庚烷，发泡剂，阻燃剂，催化剂，固化剂，稳定剂，过程中保持搅拌且超声震荡状态，而后将体系温度以不高于0.5℃/min的温度降温至常温，即得到所述酚醛树脂保温材料。
步骤1)中氯化钴，硫酸锌，苯酚三者的摩尔比为1:0.3:0.875。步骤2)中清洗的水温为30～50℃。步骤3)中超声震荡的频率为20～40KHz。
以上对本发明的实施例进行了详细说明，但所述内容仅为本发明的较佳实施例，并不用以限制本发明。凡在本发明的申请范围内所做的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.一种酚醛树脂保温材料，其特征在于包括以下重量份的成分：酚醛树脂80～95份，聚硅氧烷交联剂2～8份，二苯甲烷二异氰酸酯4～8份，有机硅油1～5份，三羟甲基丙烷1～3份，十溴二苯乙烷1～5份，正庚烷2～8份，发泡剂0.5～1份，阻燃剂0.5～1.5份，催化剂0.2～0.8份，固化剂0.1～0.3份，稳定剂0.5～0.8份。
2.根据权利要求1所述的一种酚醛树脂保温材料，其特征在于，所述发泡剂为环氧乙烷或溴代异丁烷。
3.根据权利要求1所述的一种酚醛树脂保温材料，其特征在于，所述阻燃剂为三聚磷酸铝或三聚氰胺氰尿酸盐。
4.根据权利要求1所述的一种酚醛树脂保温材料，其特征在于，所述催化剂为二铵己二酸，三氟乙酰乙酸乙酯或1,6-己二胺盐酸盐。
5.根据权利要求1所述的一种酚醛树脂保温材料，其特征在于，所述固化剂为脂环胺类固化剂或聚琉醇类固化剂。
6.根据权利要求1所述的一种酚醛树脂保温材料，其特征在于，所述稳定剂为聚磷酸铵或钛酸正丁酯。
7.权利要求1所述酚醛树脂保温材料对的制备方法，其特征在于包括以下步骤：
1)向反应容器中加入氯化钴和硫酸锌，以氮气置换反应容器中的空气，而后在80℃条件下保持20min，向其中加入苯酚，甲醛和盐酸，以120～160℃的温度2～3.5Mpa的压力反应10～20min，而后恢复至常压，再向其中加入2-溴异丁酸叔丁酯继续反应5～10min；
2)收集步骤1)所得产物，在4～6℃环境中保持20min，向其中加入硫酸锌，在搅拌状态下降温至0～1℃，收集析出的固体，清洗后以30～40℃的温度减压干燥，即得到酚醛树脂；
3)取配方量的步骤2)所得的酚醛树脂，在氮气保护下升温至120～130℃直至熔融，而后向其中加入配方量的聚硅氧烷交联剂，二苯甲烷二异氰酸酯，有机硅油，三羟甲基丙烷，十溴二苯乙烷，搅拌使其溶解，降温至100～110℃，再向其中加入配方量的正庚烷，发泡剂，阻燃剂，催化剂，固化剂，稳定剂，过程中保持搅拌且超声震荡状态，而后将体系温度以不高于0.5℃/min的温度降温至常温，即得到所述酚醛树脂保温材料。
8.根据权利要求7所述的制备方法，其特征在于，步骤1)中氯化钴，硫酸锌，苯酚三者的摩尔比为1:0.3:0.875。
9.根据权利要求7所述的制备方法，其特征在于，步骤2)中清洗的水温为30～50℃。
10.根据权利要求7所述的制备方法，其特征在于，步骤3)中超声震荡的频率为20～40KHz。
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| CN104356591A (zh) * | 2014-11-06 | 2015-02-18 | 聊城大学 | 增韧增强型酚醛泡沫保温材料及其制备方法 |
| CN105601855A (zh) * | 2014-11-25 | 2016-05-25 | 天津市煜辉机械加工有限公司 | 一种发泡酚醛树脂组合物 |
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| CN104356591A (zh) * | 2014-11-06 | 2015-02-18 | 聊城大学 | 增韧增强型酚醛泡沫保温材料及其制备方法 |
| CN105601855A (zh) * | 2014-11-25 | 2016-05-25 | 天津市煜辉机械加工有限公司 | 一种发泡酚醛树脂组合物 |
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