CN108530257A - 苯和异丙醇联产异丙苯和丙烯的方法 - Google Patents
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Abstract
本发明涉及一种苯和异丙醇联产异丙苯和丙烯的方法，包括在有效反应条件下，使苯和异丙醇与分子筛催化剂接触合成异丙苯和丙烯的步骤；所述有效反应条件至少包括：苯与异丙醇的摩尔比为在大于0、小于2的范围内。所述方法可用于联产异丙苯和丙烯的工业生产中。
Description
技术领域
本发明涉及一种苯和异丙醇联产异丙苯和丙烯的方法。
背景技术
异丙苯是重要的基本有机化工原料，工业上异丙苯的生产是以苯和丙烯为原料，在催化剂作用下经烷基化反应制备。异丙醇与苯直接烷基化也可以生产异丙苯。张祚望等(催化学报，2008，29；1015-1020)考察了MCM-22和MCM-36分子筛用于苯和异丙醇烷基化反应的性能。K.S.N.Reddy等报道了Beta分子筛用于苯和异丙醇的烷基化反应(AppliedCatalysis A:General 1993；95:53-6)。文献EP1069099中使用Beta分子筛考察了异丙醇或异丙醇和丙烯的混合物和苯的烷基化反应。文献CN102171167A公开了用于异丙醇或异丙醇和丙烯的混合物和苯进行烷基化反应生产异丙苯的方法，反应条件为：温度150-230℃，压力1-20bar，苯与异丙醇的摩尔比为2-10。它认为用丙烯对苯的烷基化所用的催化剂不能总是容易适用于苯与作为烷基化试剂的异丙醇的烷基化反应，这些催化剂通常对水非常敏感，因此在异丙醇脱水生成的水的存在下其寿命会大大降低。它发现使用MTW构型的沸石分子筛催化剂，例如ZSM-12沸石可以克服这些问题。
发明内容
本发明旨在提供一种新的苯和异丙醇联产异丙苯和丙烯的方法。
为实现上述发明目的，本发明采取的技术方案如下：一种苯和异丙醇联产异丙苯和丙烯的方法，包括在有效反应条件下，使苯和异丙醇与分子筛催化剂接触合成异丙苯和丙烯的步骤；所述有效反应条件至少包括：苯与异丙醇的摩尔比为在大于0、小于2的范围内。
上述技术方案中，苯与异丙醇的摩尔比为0.1～1.8，优选为0.2～1.5。
上述技术方案中，所述分子筛催化剂以重量百分比计，包括以下组份：a)40～90％的沸石分子筛；和b)10～60％的粘结剂；所述沸石分子筛选自具有MFI、MWW、BEA、MOR和FAU拓扑结构分子筛中的至少一种；所述粘结剂选自氧化铝、氧化硅、氧化钛、氧化锌或和氧化锆中的至少一种。
上述技术方案中，所述沸石分子筛具有MWW和BEA拓扑结构分子筛中的至少一种，优选为MCM-22族分子筛和Beta分子筛中的至少一种。
上述技术方案中，所述沸石分子筛的SiO2/Al2O3摩尔比为5～100，优选为10～80。
上述技术方案中，所述有效反应条件还包括：反应温度100～400℃，优选150～350℃；反应压力0.5～5.0MPa，优选1.0～4.0MPa；异丙醇重量空速为0.1～10小时-1，优选0.2～5小时-1。
本发明方法中，产物中丙烯的浓度大于0.5重量％，最大可达到6重量％。
在异丙醇和苯的烷基化反应中，通过调控异丙醇和苯的摩尔比在大于0、小于2的范围内，将会联产异丙苯和丙烯。在异丙醇和苯的烷基化反应体系中，水、异丙醇和异丙醇脱水产生的丙烯在酸性分子筛上竞争吸附，由于丙烯的极性较弱，在生成后便从催化剂上的酸中心脱附，从而避免了生成的丙烯在催化剂上发生聚合反应而造成的催化剂失活，因此在此过程中产生的水不会对常规的用于苯和丙烯烷基化生产异丙苯催化剂产生毒害；相反，会提高催化剂的稳定性。
下面通过实施例对本发明作进一步阐述。
具体实施方式
【实施例1】
合成具有BEA拓扑结构的Beta分子筛。将600g 40wt.％硅溶胶，38.9g铝酸钠(氧化铝含量42wt.％)，70.6g 25wt.％四乙基氢氧化铵(TEAO小时)，5.0g二乙胺(DEA)，168.0g四乙基溴化铵(TEABr)，16.0g氢氧化钠，136.0g25wt.％的氢氧化铵，925.1g水混合，常温下搅拌均匀。然后转入不锈钢高压釜中，晶化温度155℃，反应50小时。反应结束后，过滤、洗涤、干燥结晶产物。经XRD粉末衍射分析所得的结晶产品为Beta沸石。
取50g干燥后的粉末样品，用1M的硝酸铵交换4次，过滤、干燥。之后，与20g氧化铝充分混合，并加入5wt％硝酸捏合、挤条成型为φ1.6×2mm的条状物，120℃干燥12小时，500℃焙烧6小时，生产成需要的催化剂。
【实施例2】
合成具有MWW拓扑结构的MCM-22分子筛。将铝酸纳(Al2O3 35.21wt％，Na2O31.12wt％)14.5g溶于990g水中，加入氢氧化钠6.18g使之溶解，然后在搅拌的情况下加入有机胺模板剂六亚甲基亚胺49.5g，再加入硅溶胶(SiO2 40wt％)150g，待搅拌均匀后装入不锈钢反应釜中，在搅拌情况下于150℃晶化50小时。然后冷却，过滤结晶的固体产物，并回收结晶母液。上述固体结晶产物再经过滤、洗涤、干燥。X射线衍射仪测得所得晶体为MCM-22。经化学分析得SiO2/Al2O3摩尔比为18。
取50g干燥后的粉末样品，用1M的硝酸铵交换4次，过滤、干燥。之后，与20g氧化铝充分混合，并加入5wt％硝酸捏合、挤条成型为φ1.6×2mm的条状物，120℃干燥12小时，500℃焙烧6小时，生产成需要的催化剂。
【实施例3】
合成具有MWW拓扑结构的MCM-56分子筛。将铝酸纳(Al2O3 35.21wt％，Na2O31.12wt％)14.5g溶于990g水中，加入氢氧化钠6.18g使之溶解，然后在搅拌的情况下加入有机胺模板剂六亚甲基亚胺49.5g，再加入硅溶胶(SiO2 40wt％)150g，待搅拌均匀后装入不锈钢反应釜中，在搅拌情况下于140℃晶化50小时。然后冷却，过滤结晶的固体产物，并回收结晶母液。上述固体结晶产物再经过滤、洗涤、干燥。X射线衍射仪测得所得晶体为MCM-56。经化学分析得SiO2/Al2O3摩尔比为20。
取50g干燥后的粉末样品，用1M的硝酸铵交换4次，过滤、干燥。之后，与20g氧化铝充分混合，并加入5wt％硝酸捏合、挤条成型为φ1.6×2mm的条状物，120℃干燥12小时，500℃焙烧6小时，生产成需要的催化剂。
【实施例4】
将【实施例1-3】的催化剂4.0克分别装填在固定床反应器中，然后通入异丙醇和苯的混合物料，混合物中苯醇摩尔比为0.75。反应条件为:异丙醇重量空速为0.4小时-1，反应温度为200℃，反应压力为2.0MPa。
连续运转100小时，反应结果见表1。
表1
【实施例5】
将【实施例1-3】的催化剂4.0克分别装填在固定床反应器中，然后通入异丙醇和苯的混合物料，混合物中苯醇摩尔比为0.5。反应条件为:异丙醇重量空速为0.4小时-1，反应温度为200℃，反应压力为2.0MPa。
连续运转100小时，反应结果见表2。
表2
【对比例1】
同实施例4，只是反应原料中苯/异丙醇摩尔比为4。连续运转100小时，反应结果见表3。
表3
Claims (10)
1.一种苯和异丙醇联产异丙苯和丙烯的方法，包括在有效反应条件下，使苯和异丙醇与分子筛催化剂接触合成异丙苯和丙烯的步骤；所述有效反应条件至少包括：苯与异丙醇的摩尔比为在大于0、小于2的范围内。
2.根据权利要求1所述苯和异丙醇联产异丙苯和丙烯的方法，其特征在于，苯与异丙醇的摩尔比为0.1～1.8。
3.根据权利要求2所述苯和异丙醇联产异丙苯和丙烯的方法，其特征在于，苯与异丙醇的摩尔比为0.2～1.5。
4.根据权利要求1所述苯和异丙醇联产异丙苯和丙烯的方法，其特征在于，所述分子筛催化剂以重量百分比计，包括以下组份：a)40～90％的沸石分子筛；和b)10～60％的粘结剂；所述沸石分子筛选自具有MFI、MWW、BEA、MOR和FAU拓扑结构分子筛中的至少一种；所述粘结剂选自氧化铝、氧化硅、氧化钛、氧化锌或和氧化锆中的至少一种。
5.根据权利要求4所述苯和异丙醇联产异丙苯和丙烯的方法，其特征在于，所述沸石分子筛具有MWW和BEA拓扑结构分子筛中的至少一种。
6.根据权利要求5所述苯和异丙醇联产异丙苯和丙烯的方法，其特征在于，所述沸石分子筛为MCM-22族分子筛和Beta分子筛中的至少一种。
7.根据权利要求4所述苯和异丙醇联产异丙苯和丙烯的方法，其特征在于，所述沸石分子筛的SiO2/Al2O3摩尔比为5～100。
8.根据权利要求7所述苯和异丙醇联产异丙苯和丙烯的方法，其特征在于，所述分子筛的SiO2/Al2O3摩尔比为10～80。
9.根据权利要求1所述苯和异丙醇联产异丙苯和丙烯的方法，其特征在于，所述有效反应条件还包括：反应温度100～400℃，反应压力0.5～5.0MPa，异丙醇重量空速为0.1～10小时-1。
10.根据权利要求9所述苯和异丙醇联产异丙苯和丙烯的方法，其特征在于，反应温度为150～350℃，反应压力为1.0～4.0MPa，异丙醇重量空速为0.2～5小时-1。
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