CN107282004A - 一种用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂及其制备方法 - Google Patents

一种用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂及其制备方法 Download PDF

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CN107282004A
CN107282004A CN201710580856.4A CN201710580856A CN107282004A CN 107282004 A CN107282004 A CN 107282004A CN 201710580856 A CN201710580856 A CN 201710580856A CN 107282004 A CN107282004 A CN 107282004A
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安高军
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Pol Research Institute Of Logistics Support Department Of Central Military Commission
China University of Petroleum East China
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Abstract

本发明公开一种用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂及其制备方法，该固体碱脱酸剂能够有效脱除聚甲氧基二烷基醚生产过程中生成的甲酸以及催化剂脱落的酸性活性组分，从而使得聚甲氧基二烷基醚作为一种柴油调合组分，其酸值符合车用柴油国家标准对酸值的要求。此固体碱类脱酸剂具有机械强度大、吸附容量大的优点，在工业生产中，具有较高的活性周期，能够大大满足聚甲氧基二烷基醚的工业化生产要求。

Description

一种用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂及 其制备方法
技术领域
本发明为化工应用领域，涉及一种用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂及其制备方法。
背景技术
聚甲氧基二烷基醚(PODEn)，是一系列高沸点、无色或淡黄色、无刺激性气味的可燃液体，由于丙醇、丁醇和戊醇均存在同分异构体，所以根据原料结构的不同，产物种类众多，所以聚甲氧基二烷基醚产品包括但不限于聚甲氧基二甲醚(PODEn)、聚甲氧基二乙基醚(简称ETPOMn)、聚甲氧基二丙基醚(简称ITPOMn)、聚甲氧基二异丙基醚(简称IITPOMn)、聚甲氧基二丁基醚(简称BTPOMn)、聚甲氧基二异丁基醚(简称IBTPOMn)、聚甲氧基二戊基醚(简称PTPOMn)和聚甲氧基二异戊基醚(简称IPTPOMn)等。聚甲氧基二烷基醚具有氧含量高、闪点高、十六烷值高、凝点低、冷滤点低、密度适中的优点；与现用石化柴油在高温和低温下的互溶性均良好，可与石化柴油按照一定比例调合使用或直接单独使用，更为重要的是，聚甲氧基二烷基醚由于其凝点超低，适合作为高原地区柴油车辆用的柴油燃料。
目前，尚无聚甲氧基二烷基醚脱酸剂的相关报道或者专利。在聚甲氧基二烷基醚的生产过程中产生的酸性物质，一方面来源于原料甲醛发生反应生成的甲酸，另一方面来源于酸性催化剂(例如磺酸基树脂催化剂)酸性基团的脱落，这些酸性物质一方面会对生产装备产生一定程度的腐蚀，对装备的抗腐蚀等级要求高；另一方面作为柴油调合组分，聚甲氧基二烷基醚的酸值必须符合国家车用柴油GB 19147对柴油酸度的要求，所以对于聚甲氧基二烷基醚的脱酸环节是必不可少的。
发明内容
为解决上述问题，本发明具体技术方案如下：
一种用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂，所述的固体碱脱酸剂包括负载型固体碱脱酸剂和混捏型固体碱脱酸剂两者类型，其中负载型固体碱脱酸剂的组分为：以质量百分比计,载体为70％～95％；活性组分为5％～30％；混捏型固体碱脱酸剂的组分为：以质量百分比计,IIA族碱土金属为10％-50％；有机分散剂5％-10％；粘合剂为2％-4％；扩孔剂为田菁粉，用量为固态粉末用量的2％-4％，剩余为拟薄水铝石。
所述的负载型脱酸剂的载体为3A或4A或5A分子筛、硅胶、活性炭、氧化铝、硅藻土中的一种或几种，固体碱类活性组分为氢氧化钠、氢氧化钾、氢氧化镁、碳酸钾、硝酸钾、碳酸镁、硝酸镁、碳酸钙中的一种或几种。
所述的IIA族碱土金属为Mg、Ca、Ba、Sr中的一张或几种；所述的有机分散剂为乙二醇或者乙二胺；所述的粘合剂为稀硝酸；所述的扩孔剂为田菁粉。
用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂的制备方法，其特征在于，包括如下步骤：
(1)负载型固体碱脱酸剂的制备步骤:以质量百分比计,将载体为70％～95％浸渍在含有活性组分为5％～30％的水溶液中，干燥后在200℃～550℃焙烧2h～8h；
(2)混捏型固体碱脱酸剂的制备步骤:
以质量百分比计,IIA族碱土金属为10％-50％；有机分散剂5％-10％；粘合剂为2％-4％；扩孔剂为田菁粉，用量为固态粉末用量的2％-4％，剩余为拟薄水铝石,经混捏、挤条后，在100℃～120℃干燥12h-24h后，于350℃～650℃下焙烧1h～4h而成。
本发明的技术效果：该固体碱脱酸剂能够有效脱除聚甲氧基二烷基醚生产过程中生成的甲酸以及催化剂脱落的酸性活性组分，从而使得聚甲氧基二烷基醚作为一种柴油调合组分，其酸值符合车用柴油国家标准对酸值的要求。此固体碱类脱酸剂具有机械强度大、吸附容量大的优点，在工业生产中，具有较高的活性周期，能够大大满足聚甲氧基二烷基醚的工业化生产要求。
具体实施方式
下面结合本发明的优选实施例进一步说明本发明。
实施例1：
称取质量为10％的氢氧化镁，2％的田菁粉，2％的稀硝酸以及5％的乙二醇，加入拟薄水铝石，充分混合后捏合60min，挤条后于110℃烘干24h，然后于550℃焙烧4h得到混捏型氧化镁脱酸剂.
实施例2：
以活性炭为载体，将载体浸入等体积的质量百分浓度为5％的碳酸钾水溶液中，在110℃干燥12小时，然后于450℃焙烧6小时，得到负载型活性炭-碳酸钾脱酸剂。
实施例3：
称取质量为50％的氢氧化钙，4％的田菁粉，4％的稀硝酸以及10％的乙二醇，加入拟薄水铝石，充分混合后捏合60min，挤条后于110℃烘干24h，然后于550℃焙烧4h得到混捏型氧化钙脱酸剂。
实施例4：
以3A分子筛为载体，将载体浸入等体积的质量百分浓度为40％的硝酸镁水溶液中，在110℃干燥12小时，然后于450℃焙烧6小时，得到负载型活性炭-碳酸钾脱酸剂。
实施例5：
称取质量为30％的氢氧化钡，3％的田菁粉，3％的稀硝酸以及8％的乙二醇，加入拟薄水铝石，充分混合后捏合60min，挤条后于110℃烘干24h，然后于550℃焙烧4h得到混捏型氧化钙脱酸剂。
实施例6：
以硅藻土为载体，将载体浸入等体积的质量百分浓度为30％的氢氧化钾水溶液中，在110℃干燥12小时，然后于450℃焙烧6小时，得到负载型活性炭-碳酸钾脱酸剂。
将上述制备的脱酸剂装填入容量为10mL的脱酸塔，泵入聚甲氧基二烷基醚原料，控制进料空速为1h-1，对聚甲氧基二烷基醚原料和产物进行酸值测定，实施例1到6的脱酸效果如下表所示：
实施例7：
一种用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂，所述的固体碱脱酸剂包括负载型固体碱脱酸剂和混捏型固体碱脱酸剂两者类型，其中负载型固体碱脱酸剂的组分为：以质量百分比计,载体为70％～95％；活性组分为5％～30％；混捏型固体碱脱酸剂的组分为：以质量百分比计,IIA族碱土金属为10％-50％；有机分散剂5％-10％；粘合剂为2％-4％；扩孔剂为田菁粉，用量为固态粉末用量的2％-4％，剩余为拟薄水铝石。
所述的负载型脱酸剂的载体为3A或4A或5A分子筛、硅胶、活性炭、氧化铝、硅藻土中的一种或几种，固体碱类活性组分为氢氧化钠、氢氧化钾、氢氧化镁、碳酸钾、硝酸钾、碳酸镁、硝酸镁、碳酸钙中的一种或几种。
所述的IIA族碱土金属为Mg、Ca、Ba、Sr中的一张或几种；所述的有机分散剂为乙二醇或者乙二胺；所述的粘合剂为稀硝酸；所述的扩孔剂为田菁粉。
用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂的制备方法，其特征在于，包括如下步骤：
(1)负载型固体碱脱酸剂的制备步骤:以质量百分比计,将载体为70％～95％浸渍在含有活性组分为5％～30％的水溶液中，干燥后在200℃～550℃焙烧2h～8h；
(2)混捏型固体碱脱酸剂的制备步骤:
以质量百分比计,IIA族碱土金属为10％-50％；有机分散剂5％-10％；粘合剂为2％-4％；扩孔剂为田菁粉，用量为固态粉末用量的2％-4％，剩余为拟薄水铝石,经混捏、挤条后，在100℃～120℃干燥12h-24h后，于350℃～650℃下焙烧1h～4h而成。
以上所述，仅为本发明较佳实施例而已，故不能依此限定本发明实施的范围，即依本发明专利范围及说明书内容所作的等效变化与修饰，皆应仍属本发明涵盖的范围内。

Claims (4)

1.一种用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂,其特征在于，所述的固体碱脱酸剂包括负载型固体碱脱酸剂和混捏型固体碱脱酸剂两者类型，其中负载型固体碱脱酸剂的组分为：以质量百分比计,载体为70％～95％；活性组分为5％～30％；混捏型固体碱脱酸剂的组分为：以质量百分比计,IIA族碱土金属为10％-50％；有机分散剂5％-10％；粘合剂为2％-4％；扩孔剂为田菁粉，用量为固态粉末用量的2％-4％，剩余为拟薄水铝石。
2.根据权利要求1所述的用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂，其特征在于，所述的负载型脱酸剂的载体为3A或4A或5A分子筛、硅胶、活性炭、氧化铝、硅藻土中的一种或几种，固体碱类活性组分为氢氧化钠、氢氧化钾、氢氧化镁、碳酸钾、硝酸钾、碳酸镁、硝酸镁、碳酸钙中的一种或几种。
3.根据权利要求1所述的用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂，其特征在于，所述的IIA族碱土金属为Mg、Ca、Ba、Sr中的一张或几种；所述的有机分散剂为乙二醇或者乙二胺；所述的粘合剂为稀硝酸；所述的扩孔剂为田菁粉。
4.用于聚甲氧基二烷基醚脱酸精制过程的固体碱脱酸剂的制备方法，其特征在于，包括如下步骤：
(1)负载型固体碱脱酸剂的制备步骤:以质量百分比计,将载体为70％～95％浸渍在含有活性组分为5％～30％的水溶液中，干燥后在200℃～550℃焙烧2h～8h；
(2)混捏型固体碱脱酸剂的制备步骤:
以质量百分比计,IIA族碱土金属为10％-50％；有机分散剂5％-10％；粘合剂为2％-4％；扩孔剂为田菁粉，用量为固态粉末用量的2％-4％，剩余为拟薄水铝石,经混捏、挤条后，在100℃～120℃干燥12h-24h后，于350℃～650℃下焙烧1h～4h而成。
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CN114762775A (zh) * 2021-01-11 2022-07-19 尚鼎环境科技（江苏）有限公司 一种乳酸溶液的脱色处理系统及饱和活性炭的脱酸处理方法
CN114762775B (zh) * 2021-01-11 2023-08-08 尚鼎环境科技（江苏）有限公司 一种乳酸溶液的脱色处理系统及饱和活性炭的脱酸处理方法

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Application publication date: 20171024