CN107118542A - 一种生物质基阻燃的聚氨酯硬质泡沫保温材料及其制备方法 - Google Patents

一种生物质基阻燃的聚氨酯硬质泡沫保温材料及其制备方法 Download PDF

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CN107118542A
CN107118542A CN201710350634.3A CN201710350634A CN107118542A CN 107118542 A CN107118542 A CN 107118542A CN 201710350634 A CN201710350634 A CN 201710350634A CN 107118542 A CN107118542 A CN 107118542A
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解安庆
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Abstract

本发明公开了一种生物质基阻燃的聚氨酯硬质泡沫保温材料及其制备方法，其特征在于，将玉米棒芯粉碎、过筛，得植物纤维粉末，加液化试剂、浓硫酸，微波加热处理，调pH至中性，得液化产物；将三氯氧磷与甲苯等体积混合，滴加到液化产物中反应，加等体积水水解，得磷化改性产物；向氧化石墨中加N,N二甲基甲酰胺、三乙胺、十六烷基三甲氧基硅烷，磁力搅拌，在油浴、氮气氛围中，搅拌回流反应，得改性氧化石墨；向液体石蜡中加蒸馏水、乳化剂，搅拌乳化，加单体丙烯酸、引发剂及改性氧化石墨，反应得耐磨防水剂；向磷化改性产物中加聚醚多元醇、发泡剂及耐磨防水剂，剧烈搅拌，迅速加入MDI，室温下发泡及熟化，得聚氨酯泡沫体。

Description

一种生物质基阻燃的聚氨酯硬质泡沫保温材料及其制备方法
技术领域
本发明涉及聚氨酯泡沫领域，具体涉及一种生物质基阻燃的聚氨酯硬质泡沫保温材料及其制备方法。
背景技术
生物质炭是将农作物秸秆、木屑等生物质材料在限制或隔绝氧气的环境条件下，经热解得到的固体产物。利用农作物秸秆等废弃物制备成的生物质炭由于灰分含量较高，在工业领域应用会受到一定的限制，而在农业领域上却可以广泛应用。
朱俐静在其硕士学位论文《新型生物质基多元醇及聚氨酯保温材料的制备和表征》中，在微波加热条件下，以浓硫酸为催化剂，使甘蔗渣和玉米棒芯在聚乙二醇(PEG400)和丙三醇(甘油)（两者质量比3:7）构成的液化试剂中进行液化反应；然后利用三氯氧磷对液化产物进行磷化改性得到改性产物；由液化产物、改性产物代替部分传统的聚醚多元醇制备出阻燃的聚氨酯硬质泡沫。但是存在耐摩擦抗磨损性能不足。
发明内容
本发明主要解决的技术问题是提供一种生物质基阻燃的聚氨酯硬质泡沫保温材料的制备方法，依照该工艺制备的聚氨酯泡沫具备良好阻燃、保温性能，且防水、减摩抗磨。
本发明所要解决的技术问题采用以下的技术方案来实现：
一种生物质基阻燃的聚氨酯硬质泡沫保温材料的制备方法，其特征在于，按以下步骤进行：
a. 将40-50重量份玉米棒芯用粉碎机粉碎，过60-80目筛，在50-60℃烘箱中烘2-4h，得植物纤维粉末，1:3-5加入液化试剂，加2-4重量份浓硫酸，充分搅拌混合均匀，在微波中加热到150-160℃处理30-40min，冷却至室温，调pH至中性，得液化产物；将10-20重量份三氯氧磷与甲苯等体积混合均匀，滴加到液化产物中，反应6-8h，加等体积水水解1-2h，得磷化改性产物；
b. 向5-10重量份氧化石墨中1:2-3加入N,N二甲基甲酰胺，超声1-2h分散均匀，形成悬浮液，加入0.3-0.5重量份三乙胺、2-3重量份十六烷基三甲氧基硅烷，磁力搅拌20-40min，在105-115℃油浴、氮气氛围中，搅拌回流反应3-5h，过滤、洗涤，得到改性氧化石墨；
c. 向4-8重量份液体石蜡中1:3-5加入蒸馏水，加热至80-90℃，加入3-7重量份OP-10乳化剂，搅拌乳化1-2h，得乳化液体石蜡，加入10-20重量份单体丙烯酸、1-2重量份引发剂K2S2O8、及b中所得物料，反应2-3h得耐磨防水剂；
d. 向a中所得磷化改性产物中加入20-30重量份聚醚多元醇、5-10重量份发泡剂、及c中所得物料，剧烈搅拌10-20s，迅速加入10-20重量份MDI，室温下发泡及熟化，得聚氨酯泡沫体。
其中，步骤a中所述液化试剂为聚乙二醇和甘油以质量比3:5-7混合，微波功率为300-500W；步骤c中所述搅拌乳化速度为1000-1100r/min；步骤d中所述聚醚多元醇为4110或403，发泡剂为一氟二氯乙烷，MDI是二苯甲烷二异氰酸酯。
本发明的反应机理及有益效果如下：
在微波加热条件下，以浓硫酸为催化剂，使玉米棒芯在聚乙二醇和甘油构成的多羟基醇液化试剂中进行液化反应，然后用三氯氧磷对液化产物进行磷化改性得到改性产物，由磷化改性产物代替部分传统的聚醚多元醇制备出阻燃的聚氨酯硬质泡沫。先用乳化剂OP-10对液体石蜡进行乳化，制备得到液体石蜡乳液，再以单体丙烯酸为改性介体、K2S2O8为引发剂，改性液体石蜡制备丙烯酸改性液体石蜡防水剂，结合了石蜡乳液的耐水性和丙烯酸的耐热性；以N,N二甲基甲酰胺为溶剂，以三乙胺为催化剂，用十六烷基三甲氧基硅烷对氧化石墨进行改性，制备得到硅烷改性氧化石墨，提高氧化石墨与液体石蜡的兼容性，将其添加到液体石蜡中，明显提高液体石蜡的减摩能力，具有优异的摩擦性能，对保温材料起到减摩抗磨作用。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐述本发明。
实施例
一种生物质基阻燃的聚氨酯硬质泡沫保温材料的制备方法，其特征在于，按以下步骤进行：
a. 将40kg玉米棒芯用粉碎机粉碎，过60目筛，在50-60℃烘箱中烘3h，得植物纤维粉末，1:3加入液化试剂，加2kg浓硫酸，充分搅拌混合均匀，在微波中加热到150-160℃处理35min，冷却至室温，调pH至中性，得液化产物；将10kg三氯氧磷与甲苯等体积混合均匀，滴加到液化产物中，反应8h，加等体积水水解2h，得磷化改性产物；
b. 向10kg氧化石墨中1:3加入N,N二甲基甲酰胺，超声1h分散均匀，形成悬浮液，加入0.4kg三乙胺、2kg十六烷基三甲氧基硅烷，磁力搅拌40min，在115℃油浴、氮气氛围中，搅拌回流反应5h，过滤、洗涤，得到改性氧化石墨；
c. 向8kg液体石蜡中1:5加入蒸馏水，加热至80-90℃，加入7kg OP-10乳化剂，搅拌乳化1h，得乳化液体石蜡，加入15kg单体丙烯酸、1kg引发剂K2S2O8、及b中所得物料，反应3h得耐磨防水剂；
d. 向a中所得磷化改性产物中加入20kg聚醚多元醇、5kg发泡剂、及c中所得物料，剧烈搅拌10s，迅速加入10kg MDI，室温下发泡及熟化，得聚氨酯泡沫体。
其中，步骤a中所述液化试剂为聚乙二醇和甘油以质量比3:6混合，微波功率为400W；步骤c中所述搅拌乳化速度为1000r/min；步骤d中所述聚醚多元醇为4110，发泡剂为一氟二氯乙烷，MDI是二苯甲烷二异氰酸酯。

Claims (5)

1.一种生物质基阻燃的聚氨酯硬质泡沫保温材料的制备方法，其特征在于：
将玉米棒芯粉碎、过筛，得植物纤维粉末，加液化试剂、浓硫酸，微波加热处理，调pH至中性，得液化产物；将三氯氧磷与甲苯等体积混合，滴加到液化产物中反应，加等体积水水解，得磷化改性产物；向氧化石墨中加N,N二甲基甲酰胺、三乙胺、十六烷基三甲氧基硅烷，在油浴、氮气氛围中，搅拌回流反应，得改性氧化石墨；向液体石蜡中加蒸馏水、乳化剂、单体丙烯酸、引发剂及改性氧化石墨，反应得耐磨防水剂；向磷化改性产物中加聚醚多元醇、发泡剂及耐磨防水剂，剧烈搅拌，迅速加入MDI，室温下发泡及熟化，得聚氨酯泡沫体。
2.一种生物质基阻燃的聚氨酯硬质泡沫保温材料的制备方法，其特征在于：
a. 将40-50重量份玉米棒芯用粉碎机粉碎，过60-80目筛，在50-60℃烘箱中烘2-4h，得植物纤维粉末，1:3-5加入液化试剂，加2-4重量份浓硫酸，充分搅拌混合均匀，在微波中加热到150-160℃处理30-40min，冷却至室温，调pH至中性，得液化产物；将10-20重量份三氯氧磷与甲苯等体积混合均匀，滴加到液化产物中，反应6-8h，加等体积水水解1-2h，得磷化改性产物；
b. 向5-10重量份氧化石墨中1:2-3加入N,N二甲基甲酰胺，超声1-2h分散均匀，形成悬浮液，加入0.3-0.5重量份三乙胺、2-3重量份十六烷基三甲氧基硅烷，磁力搅拌20-40min，在105-115℃油浴、氮气氛围中，搅拌回流反应3-5h，过滤、洗涤，得到改性氧化石墨；
c. 向4-8重量份液体石蜡中1:3-5加入蒸馏水，加热至80-90℃，加入3-7重量份OP-10乳化剂，搅拌乳化1-2h，得乳化液体石蜡，加入10-20重量份单体丙烯酸、1-2重量份引发剂K2S2O8、及b中所得物料，反应2-3h得耐磨防水剂；
d. 向a中所得磷化改性产物中加入20-30重量份聚醚多元醇、5-10重量份发泡剂、及c中所得物料，剧烈搅拌10-20s，迅速加入10-20重量份MDI，室温下发泡及熟化，得聚氨酯泡沫体。
3.根据权利要求2所述的一种生物质基阻燃的聚氨酯硬质泡沫保温材料的制备方法，其特征在于，步骤a中所述液化试剂为聚乙二醇和甘油以质量比3:5-7混合，微波功率为300-500W。
4.根据权利要求2所述的一种生物质基阻燃的聚氨酯硬质泡沫保温材料的制备方法，其特征在于，步骤c中所述搅拌乳化速度为1000-1100r/min。
5.根据权利要求2所述的一种生物质基阻燃的聚氨酯硬质泡沫保温材料的制备方法，其特征在于，步骤d中所述聚醚多元醇为4110或403，发泡剂为一氟二氯乙烷，MDI是二苯甲烷二异氰酸酯。
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