CN115304733A - 一种超低温硬质聚氨酯泡沫及其制备方法 - Google Patents
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Abstract
本发明涉及一种超低温硬质聚氨酯泡沫及其制备方法,由组分A和组分B反应制得,其中组分A按照重量份数计组成如下:聚醚多元醇0‑50份、聚酯多元醇50‑100份、有机硅表面活性剂1‑5份、催化剂0.5‑3份、交联剂1‑5份、水0.5‑3份、物理发泡剂10‑30份、阻燃剂10‑20份,组分B为多苯基多亚甲基多异氰酸酯;组分A与组分B的混合质量比例为100:140‑200。将组分A与组分B经高压机枪头充分混合,浇注到模具中发泡成型。本发明制得的材料工作温度范围为‑196℃到‑140℃,产品密度35‑45kg/m3,同时具有良好的尺寸稳定性和机械性能,阻燃性能达到DIN4102B2级。
Description
技术领域
本发明涉及一种超低温硬质聚氨酯泡沫及其制备方法,属于材料合成技术领域。
背景技术
液化天然气(Liquefied Natural Gas,简称LNG)主要成分是甲烷,具有无色、无味、无毒且无腐蚀性,其燃烧过程中产生的能影响人类呼吸系统健康的物质极少,二氧化碳仅为煤的40%左右,在温室气体减排方面具有显著的优势,粉尘排放量降低近100%,燃烧后无废渣、废水产生,是公认的最清洁的能源。近年来LNG的需求量迅速增长,尤其是中国的需求量每年约50%的幅度增长,LNG运输和存储行业迎来了发展良机。LNG的沸点为-163℃,因此,需要将温度控制在-163℃以下的超低温来减少运输和存储过程中LNG的挥发损耗,这就需要对运输船舶和储存基站的LNG罐体和管路做保温处理。
LNG保温材料需要具有良好的保温性能,同时具备耐超低温、线性尺寸变化率小、阻燃等性能;硬质聚氨酯泡沫是一种性能优异的有机材料,具有密度低、强度高、保温性能优异等优点,通过配方设计可以达到阻燃要求。在日本和韩国LNG运输船舶制造业硬质聚氨酯泡沫得到广泛应用,根据具体要求密度从40-500kg/m3各有不同。专利CN 107090074A公开了一种玻纤增强硬质聚氨酯保温材料密度为115kg/m3,阻燃性能B2或者B3级别;专利CN108264625A公开了一种LNG硬质聚氨酯保材料密度也为115kg/m3。在中国,暂时还没有一种密度低至40kg/m3的用于LNG超低温保冷领域的硬质聚氨酯保温材料。
发明内容
本发明的目的是克服现有技术不足,而提供一种超低温硬质聚氨酯泡沫及其制备方法,这种材料工作温度范围为-196℃到-140℃,产品密度40-42kg/m3,同时具有良好的尺寸稳定性和机械性能,阻燃性能达到DIN 4102 B2级。
本发明采取的技术方案为:
一种超低温硬质聚氨酯泡沫,由组分A和组分B反应制得,其中组分A为以聚醚多元醇和/或聚酯多元醇为主体,添加相应助剂混合而成,按照重量份数计组成如下:聚醚多元醇0-50份、聚酯多元醇50-100份、有机硅表面活性剂1-5份、催化剂0.5-3份、交联剂1-5份、水0.5-3份、物理发泡剂10-30份、阻燃剂10-20份;
组分B为多苯基多亚甲基多异氰酸酯;
组分A与组分B的质量混合比例为100:140-200。
所述的聚醚多元醇粘度为2000-40000mPa.s(25℃),聚醚多元醇羟值为300-800mgKOH/g,聚醚多元醇官能度为3.0-8.0;优选粘度为4000-12000mPa.s(25℃),羟值为380-500mgKOH/g,官能度为4.0-6.0。
所述的聚醚多元醇,其为以蔗糖、山梨醇、季戊四醇、乙二胺、甲苯二胺、甘油、乙二醇、丙二醇、一缩二乙二醇等活性基团至少为2的小分子多元醇中的一种或几种复配物为起始剂,与环氧丙烷或环氧乙烷聚合而成,以环氧丙烷封端;优选山梨醇与环氧丙烷聚合而成。
所述的聚酯多元醇,其为芳香族聚酯多元醇,由邻苯二甲酸酐、对苯二甲酸中的一种或两种与乙二醇、二乙二醇、丙二醇、二丙二醇、1,4-丁二醇中的一种或几种混合物聚合而成。
所述的聚酯多元醇粘度为3000-15000mPa.s(25℃),羟值为150-300mgKOH/g;优选粘度为4000-8000mPa.s(25℃),羟值为200-250mgKOH/g。
所述的物理发泡剂为五氟丙烷(HFC-245fa)、五氟丁烷(HFC-365mfc)中的一种或两种的混合物,优选五氟丙烷与五氟丁烷按质量比为1:1复合的混合物。
所述的催化剂为发泡型催化剂五甲基二乙烯三胺、二吗啉二乙基醚、双(二甲氨基乙基)醚,凝胶型催化剂N,N-二甲基环己胺、三乙烯二胺,三聚型催化剂N,N’N”-三(二甲胺基丙基)-六氢化三嗪、2,4,6-三(二甲胺基甲基)苯酚、季铵盐、可溶性钾盐、可溶性钠盐中的一种或多种,进一步优选发泡型催化剂、凝胶型催化剂、三聚型催化剂三者复配。
所述的有机硅表面活性剂,可以选用上海麦豪化工科技有限公司的S系列产品、赢创集团的B系列产品、迈图高新材料的L系列产品及江苏美思德化学股份有限公司的AK系列产品,进一步优选上海麦豪化工科技有限公司的S-8875。
所述的交联剂为甘油、三羟甲基丙烷的一种或几种。
所述的水优选为去离子水。
所述的阻燃剂为TCPP(三(2-氯丙基)磷酸酯)、TCEP(三(2-氯乙基)磷酸酯)、TEP(磷酸三乙酯)、DMMP(甲基膦酸二甲酯)中的一种或几种,较佳的为TCPP与TEP混合物,优选质量比为2:1。
所述的组分A与组分B的质量混合比例进一步优选100:150-160。
组分A在制备时,只需将各组分在具有安全装置的搅拌速度为500rpm的混合釜中均匀混合,混合时最好在不锈钢混合釜内进行,混合时间0.5-1小时,静置0.5-1小时消泡后,放出即得组分A。
上述的超低温硬质聚氨酯泡沫的制备方法采用常规方法,将组分A和组分B放入高压机中,控制料温20±3℃,枪头压力为120-150bar,将组分A与组分B经高压机枪头充分混合,浇注到模具中发泡成型,即制得硬质聚氨酯泡沫。泡沫常温熟化48小时后测试各项性能。
所述的硬质聚氨酯泡沫可切割成平板、瓦壳或管壳,用于LNG罐体、管道的保温。
本发明优势在于:
1)采用聚酯多元醇为主,聚醚多元醇为辅的设计方案,同时使用过量的多苯基多亚甲基多异氰酸酯;制得泡沫中含大量的苯环结构,同时过量的NCO三聚生成很稳定的异氰酸酯杂环,提高泡沫的机械性能和阻燃性能;
2)采用了零臭氧消耗的环保发泡剂HFCs物质为物理发泡剂;
3)水和物理发泡剂合理搭配,控制HFCs在配方中使用量,使成本最优;
4)采用发泡、凝胶和三聚复合催化剂平衡化学反应,使泡沫成型过程更加平稳,满足复杂的生产工艺状况。
5)本发明制得的材料工作温度范围为-196℃到-140℃,产品密度40-42kg/m3,同时具有良好的尺寸稳定性和机械性能,阻燃性能达到DIN 4102 B2级。
具体实施方式
为了能够详细地理解本发明的技术特征和内容,以下结合实施例对本发明做进一步说明。
以下实施例中所用到的原料来源如下:
聚醚多元醇:INOV R6048,羟值480mgKOH/g,粘度40000mPa.s,购于山东一诺威新材料有限公司;
聚酯多元醇C:PS-2452,羟值240mgKOH/g,粘度10000mPa.s,购于斯泰潘南京化学有限公司;
泡沫稳定剂S-8875购于上海麦豪化工科技有限公司;
聚氨酯复合催化剂五甲基二乙烯三胺(PC5)、三乙烯二胺(A33)和N,N’N”-三(二甲胺基丙基)-六氢化三嗪(PC41)购于EVONIK;
交联剂甘油购于中化集团;
阻燃剂TCPP购于江苏法力克化工有限公司;
阻燃剂TEP购于张家港雅瑞化工有限公司;
物理发泡剂HFC-245fa购于中化蓝天霍尼韦尔新材料有限公司;
多苯基多亚甲基多异氰酸酯:PM200,购于万华化学。
实施例1
一种超低温硬质聚氨酯泡沫,由组分A和组分B反应制得,
其中组分A组成如下:聚醚多元醇、聚酯多元醇、有机硅表面活性剂、催化剂、交联剂、水、物理发泡剂、阻燃剂;
组分B为多苯基多亚甲基多异氰酸酯;具体重量份比组成见表1。
制备方法:将组分A各原料在具有安全装置的搅拌速度为500rpm的混合釜中均匀混合,混合时最好在不锈钢混合釜内进行,混合时间1小时,静置1小时消泡后,放出即得组分A。将组分A和组分B放入高压机中,控制料温20±3℃,枪头压力为140bar,将组分A与组分B经高压机枪头充分混合,浇注到模具中发泡成型,即制得超低温硬质聚氨酯泡沫。泡沫常温熟化48小时后测试各项性能。
实施例2-6
一种超低温硬质聚氨酯泡沫,由组分A和组分B反应制得,具体组成如下表1,制备方法同实施例1。
制备超低温硬质聚氨酯泡沫实施例1-6的配方如下表1。
表1
硬质聚氨酯泡沫的性能测试采用以下标准:
泡沫密度采用ASTM D1622,抗压强度采用ASTM D1621,闭孔率采用ASTM D6226,导热系数采用ASTM C518,尺寸稳定性采用ASTM D2126,线性热膨胀系数采用ASTM E831-14,氧指数采用ASTM D2863,阻燃性能采用DIN 4102。各实施例制得硬质聚氨酯泡沫的性能如下表2。
表2
经测试,本发明所制备的硬质聚氨酯泡沫材料能够满足LNG超低温保冷要求,产品密度40-42kg/m3;抗压强度240kPa以上,大于180kPa;常温导热系数约22.00mW/m.k,小于23.00mW/m.k,且超低温-160℃条件下测得12.00mW/m.k;线性膨胀系数40-60μm/m.℃,小于100μm/m.℃;阻燃性达到DIN 4102 B2级。
上述虽然对本发明的具体实施方式进行了描述,但并非对本发明保护范围的限制,所属领域技术人员应该明白,在本发明的技术方案的基础上,本领域技术人员不需要付出创造性劳动即可做出的各种修改或变形仍在本发明的保护范围以内。
Claims (10)
1.一种超低温硬质聚氨酯泡沫,其特征是,由组分A和组分B反应制得,其中组分A为以聚醚多元醇和/或聚酯多元醇为主体,添加相应助剂混合而成,按照重量份数计组成如下:聚醚多元醇0-50份、聚酯多元醇50-100份、有机硅表面活性剂1-5份、催化剂0.5-3份、交联剂1-5份、水0.5-3份、物理发泡剂10-30份、阻燃剂10-20份;
组分B为多苯基多亚甲基多异氰酸酯;
组分A与组分B的质量混合比例为100:140-200。
2.根据权利要求1所述的一种超低温硬质聚氨酯泡沫,其特征是,所述的聚醚多元醇粘度为2000-40000mPa.s(25℃),聚醚多元醇羟值为300-800mgKOH/g,聚醚多元醇官能度为3.0-8.0。
3.根据权利要求1所述的一种超低温硬质聚氨酯泡沫,其特征是,所述的聚酯多元醇,其为芳香族聚酯多元醇,由邻苯二甲酸酐、对苯二甲酸中的一种或两种与乙二醇、二乙二醇、丙二醇、二丙二醇、1,4-丁二醇中的一种或几种混合物聚合而成。
4.根据权利要求3所述的一种超低温硬质聚氨酯泡沫,其特征是,所述的聚酯多元醇粘度为3000-15000mPa.s(25℃),羟值为150-300mgKOH/g。
5.根据权利要求1所述的一种超低温硬质聚氨酯泡沫,其特征是,所述的组分A与组分B的质量混合比例为100:150-160。
6.根据权利要求1所述的一种超低温硬质聚氨酯泡沫,其特征是,所述的催化剂为发泡型催化剂五甲基二乙烯三胺、二吗啉二乙基醚、双(二甲氨基乙基)醚,凝胶型催化剂N,N-二甲基环己胺、三乙烯二胺,三聚型催化剂N,N’N”-三(二甲胺基丙基)-六氢化三嗪、2,4,6-三(二甲胺基甲基)苯酚、季铵盐、可溶性钾盐、可溶性钠盐中的一种或多种。
7.根据权利要求6所述的一种超低温硬质聚氨酯泡沫,其特征是,所述的催化剂为发泡型催化剂、凝胶型催化剂、三聚型催化剂三者复配。
8.根据权利要求1所述的一种超低温硬质聚氨酯泡沫,其特征是,所述的阻燃剂为TCPP、TCEP、TEP、DMMP中的一种或几种。
9.根据权利要求8所述的一种超低温硬质聚氨酯泡沫,其特征是,所述的阻燃剂为TCPP与TEP的混合物。
10.权利要求1-9任一项所述的超低温硬质聚氨酯泡沫的制备方法,其特征是,包括步骤如下:
(1)将组分A各原料在具有安全装置的混合釜中搅拌均匀混合,混合时间0.5-1小时,静置0.5-1小时消泡后,放出即得组分A;
(2)将组分A和组分B放入高压机中,控制料温20±3℃,枪头压力为120-150bar,将组分A与组分B经高压机枪头充分混合,浇注到模具中发泡成型,即制得硬质聚氨酯泡沫。
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