CN107051426A - 一种1‑丁烯生成异戊二烯用催化剂 - Google Patents
一种1‑丁烯生成异戊二烯用催化剂 Download PDFInfo
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Abstract
本发明公开了一种1‑丁烯生产异戊二烯用催化剂,涉及化工分离与合成技术领域,具体涉及以纳米活性炭为载体,以5‑25份SbF5/SiO2‑ZrO2、ZrO2SO4、WO3ZrO2等为活性成分,以5‑10份膨润土,硅酸盐或锶盐中的一种或几种为助剂,以碳酸钠、碳酸氢铵、氢氧化钠、氨水、醋酸中为沉淀剂,以去离子水、蒸馏水和无水乙醇为洗涤剂。采用反滴加沉淀法制备,经静置沉淀过夜陈化,后用真空泵进行过滤,洗涤,焙烧,成型即可得1‑丁烯生成异戊二烯用催化剂。本催化剂制备方法有助于提高催化剂的负载率和催化活性,有选择性好、催化效率高的特点,可提高1‑丁烯烯醛生成异戊二烯产量。
Description
技术领域:
本发明涉及化工原料制备技术领域,具体涉及一种1-丁烯生产异戊二烯用催化剂。
背景技术:
异戊二烯是合成橡胶的基本组分,异戊二烯的结构与性能基本与天然橡胶相同,主要用于异戊橡胶、苯乙烯-异戊二烯-苯乙烯嵌段共聚物和丁基橡胶等,其还广泛应用于农药、医药、香料、喷雾剂及粘结剂等,但原料来源受到限制。目前国内市场上聚合级异戊二烯的价格一直在高位运行,并且预计国内未来几年可从乙烯获得的异戊二烯增长量有限。目前异戊二烯的生产方法主要有3种,碳馏分的萃取蒸馏法,异戊烷、异戊烯脱氢法,化学合成法等。
近几年,我国橡胶销量一直居于世界第一位,尽管在聚异戊二烯橡胶尤其是稀土聚合异戊二烯橡胶研发开发方面取得很大进展,但仍不能满足天然橡胶资源严重不足。提高合成橡胶比例其关键技术在于开发出高效催化剂已成为天然天然橡胶短缺的最佳选择。
烯醛法合成异戊二烯是异戊二烯获得方法中的重要方法之一。烯醛法是俄罗斯获得异戊二烯的主要方法之一,俄罗斯目前利用该方法已经形成约25万顿/年的生产能力。烯醛法工艺先后形成两步法、一步法工艺。目前工业上未有工业化案例,主要以两步法进行异戊二烯生成。
烯醛法两步法,首先在酸性催化剂的催化作用下,异丁烯与甲醛经缩合反应生成4,4二甲基-1,3二氧六环(dmd),第二步dmd裂解生成异戊二烯、甲醛和水,经精制获得聚合级异戊二烯。
发明内容:
本发明所要解决的技术问题在于提供一种选择性好、催化效率高的1-丁烯经烯醛合成异戊二烯用催化剂。
本发明所要解决的技术问题采用以下技术方案来实现:
一种1-丁烯生产异戊二烯用催化剂:
1-丁烯经烯醛合成法生产异戊二烯用催化剂,以纳米活性炭为载体,以5-25份SbF5/SiO2-ZrO2、ZrO2SO4、WO3ZrO2等为活性成分,以5-10份膨润土,硅酸盐或锶盐中的一种或几种为助剂。采用反滴加沉淀法制备,将Sb、Zr、W的可溶性物溶于200ml 10%的乙醇溶液中,搅拌20-60min,配置成浓度为0.5mol/L的混合溶液,其中Sb、Zr、W比例为0.05:0.05:0.1~0.5:0.5:1,在45-60℃恒温搅拌条件下采用恒流泵将混合溶液逐滴滴加到100ml 2mol/L的沉淀剂溶液中,恒流泵转速为20-60转/min;搅拌0.5-1时,然后再加入一定浓度一定量的NaOH溶液,静置沉淀过夜陈化,后用真空泵进行过滤,洗涤,60-150℃干燥12-24小时,250-500℃焙烧4-6小时,得到用于1-丁烯经烯醛合成法生成异戊二烯用催化剂。
所述Sb的可溶性物为SbF5、SbP3-Pt等中的一种;Zr的可溶性物为ZrO2、ZrO2SO4等中的一种;W的可溶性物为WO3ZrO2等。
所述沉淀剂为碳酸钠、碳酸氢铵、氢氧化钠、氨水、醋酸中的一种。
所述洗涤为去离子水、蒸馏水和无水乙醇分别先后洗3次。
本发明有益效果是:
(1)主活性组分和纳米活性载体的结合,有助于提高催化剂的负载率和催化活性;
(2)该催化剂制备方法有利于杂质的清楚,获得活性组分分散度较高的产品,且多组分催化剂,利于组分间紧密结合,制成事宜的活性结构;
(3)该法制备催化剂活性组分与载体紧密结合,活性组分不易流失;
(4)该催化剂具有选择性好、催化效率高的特点,可提高1-丁烯烯醛生成异戊二烯产量。
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1
一种1-丁烯生产异戊二烯用催化剂:包括如下步骤:
1-丁烯经烯醛合成法生产异戊二烯用催化剂,以纳米活性炭为载体,以6份SbF5/SiO2-ZrO2、ZrO2SO4、WO3ZrO2为活性成分,以5份膨润土为助剂。采用反滴加沉淀法制备,将Sb、Zr、W的可溶性物溶于200ml 10%的乙醇溶液中,搅拌30min,配置成浓度为0.5mol/L的混合溶液,其中Sb、Zr、W比例为0.05-0.05-0.1,在55℃恒温搅拌条件下采用恒流泵将混合溶液逐滴滴加到100ml 2mol/L的沉淀剂溶液中,恒流泵转速为60转/min;搅拌0.6时,然后再加入一定浓度一定量的NaOH溶液,静置沉淀过夜陈化,后用真空泵进行过滤,洗涤,100℃干燥14小时,240℃焙烧3小时,得到用于1-丁烯经烯醛合成法生成异戊二烯用催化剂。
所述Sb的可溶性物为SbP3-Pt;Zr的可溶性物为ZrO2SO4;W的可溶性物为WO3ZrO2等
所述沉淀剂为醋酸。
所述洗涤为用去蒸馏水和无水乙醇分别先后洗3次。
实施例2
一种1-丁烯生产异戊二烯用催化剂:包括如下步骤:
1-丁烯经烯醛合成法生产异戊二烯用催化剂,以纳米活性炭为载体,以8份SbF5/SiO2-ZrO2、ZrO2/ZrO2SO4、WO3ZrO2为活性成分,以6份膨润土为助剂。采用反滴加沉淀法制备,将Sb、Zr、W的可溶性物溶于200ml 10%的乙醇溶液中,搅拌45min,配置成浓度为0.5mol/L的混合溶液,其中Sb、Zr、W比例为0.05-0.05-0.1,在45℃恒温搅拌条件下采用恒流泵将混合溶液逐滴滴加到100ml 2mol/L的沉淀剂溶液中,恒流泵转速为40转/min;搅拌0.5时,然后再加入一定浓度一定量的NaOH溶液,静置沉淀过夜陈化,后用真空泵进行过滤,洗涤,80℃干燥12小时,260℃焙烧4小时,得到用于1-丁烯经烯醛合成法生成异戊二烯用催化剂。
所述Sb的可溶性物为SbF5;Zr的可溶性物为ZrO2;W的可溶性物为WO3ZrO2等
所述沉淀剂为碳酸钠。
所述洗涤为用去离子水和无水乙醇分别先后洗3次。
将实施例1和实施例2所制1-丁烯生产异戊二烯用催化剂中,对其考察指标进行检测,其检测结果如表1所示。
表1 1-丁烯生产异戊二烯用催化剂检测结果
其中:
灼烧减量是指催化剂中所含水分、铵盐及碳粒等挥发组分的含量。生产中控制其减量≤13%。
比表面积测定方法:测定比表面积采用的方法是氮吸附容量法。
孔体积测定方法:孔体积测量采用的方法是水滴法。
磨损指数:磨损指数来评价微球催化剂的耐磨损强度。测定方法是将一定量催化剂放入磨损指数测定装置中,在恒定的气速下吹磨5小时,第一小时吹出的<15μ的试样弃去不计,收集后4小时吹出的试样,计算出每小时平均磨损百分数,(每小时吹出的<15μ的试样占原有试样中>15μ部分的重量百分数),此即为该催化剂的磨损指数,其单位是%h-1。目前采用的催化剂磨损指数分析方法是直管法。
粒度分布:一般要求催化剂颗粒<40μm的不大于25%,40μm、80μm不小于50%、>80μm的不大于30%。目前测定催化剂筛分采用的仪器是激光粒度仪。
表观松密度:分析催化剂表观松密度所用的仪器为一内径为20毫米的25毫升量筒,并恰好在25毫升刻度处割断磨平。测量时将量筒放在漏斗下,把样品倒在漏斗上,使样品在30秒内连续装满量筒并溢出,用刮刀将多余的催化剂刮平,擦净量筒外催化剂并称重。由此计算出催化剂的表观松密度。单位为克/毫升。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (7)
1.一种1-丁烯生产异戊二烯用催化剂,其特征在于,包括如下组成成分:
一种1-丁烯经烯醛合成法生产异戊二烯用催化剂,以纳米活性炭为载体,以5-25份SbF5/SiO2-ZrO2、ZrO2SO4、WO3ZrO2等为活性成分,以5-10份膨润土,硅酸盐或锶盐中的一种或几种为助剂。
2.根据权利要求1所述的1-丁烯生产异戊二烯用催化剂,其特征在于:采用反滴加沉淀法制备,将Sb、Zr、W的可溶性物溶于200ml 10%的乙醇溶液中,搅拌20-60min,配置成浓度为0.5mol/L的混合溶液,其中Sb、Zr、W比例为0.05-0.05-0.1。
3.根据权利要求2所述的1-丁烯生产异戊二烯用催化剂,其特征在于:在45-60℃恒温搅拌条件下采用恒流泵将步骤权利要求2中混合溶液逐滴滴加到100ml 2mol/L的沉淀剂溶液中,恒流泵转速为20-60转/min,搅拌0.5-1时。
4.根据权利要求3所述的1-丁烯生产异戊二烯用催化剂,其特征在于:权利要求3中沉淀溶液中加入一定浓度一定量的NaOH溶液,静置沉淀过夜陈化,后用真空泵进行过滤,洗涤,60-150℃干燥12-24小时,250-500℃焙烧4-6小时,得到用于1-丁烯经烯醛合成法生成异戊二烯用催化剂。
所述Sb的可溶性物为SbF5、SbP3-Pt等中的一种;Zr的可溶性物为ZrO2、ZrO2SO4等中的一种;W的可溶性物为WO3ZrO2等。
5.根据权利要求4所述的1-丁烯生产异戊二烯用催化剂,其特征在于:所述Sb的可溶性物为SbF5、SbP3-Pt等中的一种;Zr的可溶性物为ZrO2、ZrO2SO4等中的一种;W的可溶性物为WO3ZrO2等。
6.根据权利要求5所述的1-丁烯生产异戊二烯用催化剂,其特征在于:所述淀剂为碳酸钠、碳酸氢铵、氢氧化钠、氨水、醋酸中的一种。
7.根据权利要求6所述的1-丁烯生产异戊二烯用催化剂,其特征在于:所述洗涤为用去离子水、蒸馏水(一种)和无水乙醇分别先后洗3次。
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Publication number | Priority date | Publication date | Assignee | Title |
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CN85102885A (zh) * | 1985-04-01 | 1986-09-17 | 吉林化学工业公司研究院 | 生产异戊二烯的新型催化剂 |
CN86108869A (zh) * | 1986-12-31 | 1988-07-20 | 中国科学院兰州化学物理所 | 异丁烯-甲醛气相缩合制异戊二烯催化剂 |
CN103814004A (zh) * | 2011-08-17 | 2014-05-21 | 史波柏·优乐庆有限公司 | 从异丁烯和甲醛合成异戊二烯的液相合成装置 |
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CN85102885A (zh) * | 1985-04-01 | 1986-09-17 | 吉林化学工业公司研究院 | 生产异戊二烯的新型催化剂 |
CN86108869A (zh) * | 1986-12-31 | 1988-07-20 | 中国科学院兰州化学物理所 | 异丁烯-甲醛气相缩合制异戊二烯催化剂 |
CN103814004A (zh) * | 2011-08-17 | 2014-05-21 | 史波柏·优乐庆有限公司 | 从异丁烯和甲醛合成异戊二烯的液相合成装置 |
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