CN113828305A - 用于交叉偶联反应的Pd/凹凸棒石催化剂的制备方法 - Google Patents
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Abstract
本发明公开了一种用于交叉偶联反应的Pd/凹凸棒石催化剂的制备方法,该催化剂的制备方法包括以下步骤:首先对凹凸棒石进行制浆提纯、酸活化得到纳米凹凸棒石,然后以纳米凹凸棒石为载体,对Pd盐溶液进行吸附负载,随后经过干燥、退火处理得到Pd/凹凸棒石催化剂。本发明一方面通过退火处理提高了活性金属组分的催化性能和稳定性能,另一方面扩大了凹凸棒石的应用范围和提高了凹凸棒石的附加值;本发明制备的Pd/凹凸棒石催化剂具有制备工艺简单、催化剂与产物容易分离等特点。
Description
技术领域
本发明涉及制备一种用于电化学制氢、赫克反应的凹凸棒石负载有序金属催化剂,属于凹凸棒石的利用以及催化剂制备技术领域。
背景技术
众所周知,交叉偶联反应的效率高、选择性好、反应条件温和,是现代有机合成有效手段。在交叉偶联反应中,金属钯是不可或缺的催化剂,钯作为配位物的作用下,卤代化合物和非过渡金属有机化合物能够高选择性的以形成碳-碳键的方式联接在一起,常用于萘谱生、内皮素拮抗剂等各类有机化合物的合成。
催化是重要的化学反应过程,在催化反应过程中,催化剂与反应物发生化学作用,改变了反应途径,从而降低了反应的活化能和极大的提高反应速率。催化剂是催化反应的核心,催化剂的性能对反应物的转化率和产物的得率及选择性有具有重要的影响。
通常,催化剂分为均相催化剂和非均相催化剂。均相催化剂具有活性中心均一、高活性和高选择性,但均相体系下催化剂不易回收,催化剂成本较高。为了提高催化的经济性,常将催化剂活性金属组分负载到固态载体中制备成非均相催化剂。然而,由于活性组分粒子团聚、活性组分流失、积炭等各种因素的影响,与均相催化剂相比,非均相催化剂的催化活性较低,在一些催化反应中难以达到理想的效果。大量的研究表明退火处理可改变催化剂表面的原子粒径和排布,从而提高其催化活性。
凹凸棒石是一种多孔性链层状含水富镁铝硅酸盐矿物,具有独特的棒晶状结构,是一种天然的一维纳米材料。凹凸棒石具有较大的比表面积和吸附容量,良好的热稳定性和化学稳定性。凹凸棒石晶体结构单元中所含有的Mg2 +、Al3 +离子很容易被其他金属离子交换,层结构中的结构羟基基团可形成Bronst酸位点,而暴露的Al3+离子则形成Lewis酸位点,因此凹凸棒石是一种优良的催化剂载体。凹凸棒石经过适当的退火处理能够在保持结构稳定的情况下,选择性的脱去吸附水和沸石水。
发明内容
本发明的目的是:提供一种用于交叉偶联反应的Pd/凹凸棒石催化剂的制备方法,该制备方法中通过退火处理提高活性金属组分的催化性能和稳定性能,扩大凹凸棒石的应用范围和提高凹凸棒石的附加值,制备所得的Pd/凹凸棒石催化剂具有制备工艺简单、催化剂与产物容易分离等特点。
本发明的技术解决方案是:用于交叉偶联反应的Pd/凹凸棒石催化剂的制备方法,该催化剂的制备方法包括以下步骤:首先对凹凸棒石进行制浆提纯、酸活化得到纳米凹凸棒石,然后以纳米凹凸棒石为载体,对Pd盐溶液进行吸附负载,随后经过干燥、退火处理,得到Pd/凹凸棒石催化剂。
其中,所述的纳米凹凸棒石的制备方法是:
(1)制浆提纯:将100重量份凹凸棒石原矿,300~500重量份水混合均匀,高速剪切机剪切30~180 min,浆料过15~80目筛,溶液依次经过过滤、烘干、粉碎、过200目筛得纯化凹凸棒石;
(2)酸活化:将50重量份纯化凹凸棒石,150~300重量份水和10~50重量份酸混合均匀,50~90℃恒温搅拌30~180 min,然后过滤、烘干、粉碎、过200目筛,得纳米凹凸棒石。
其中,所述的酸为硫酸、盐酸、硝酸中的一种或几种。
其中,Pd/凹凸棒石催化剂的制备方法包括以下具体步骤:
(1)将纳米凹凸棒石在100℃真空干燥24 h,然后按液固比1:1~2:1(v/g)加入质量分数为2%的Pd盐溶液,搅拌6~24 h,抽滤、洗涤、干燥、粉碎、过100 目筛,得到Pd/凹凸棒石粉末;
(2)将Pd/凹凸棒石粉末置于真空管式退火炉中,氩气或氮气保护300~600℃退火0.5~3h,得到Pd/凹凸棒石催化剂。
其中,所述的钯盐为硝酸钯、氯钯酸、氯钯酸铵中的一种或几种。
其中,本发明所制备的Pd/凹凸棒石催化剂用于交叉偶联反应的赫克反应、根岸反应、铃木反应的催化剂。
本发明与现有的技术相比,具有如下优点:
(1)本发明以纳米凹凸棒石作为金属活性组分的载体,催化剂能均匀分散在比表面积较大的纳米凹凸棒石上,从而提高了催化剂的热稳定性和催化活性;
(2)催化剂再生容易,多次重复使用后其催化效率并无明显降低。
(3)通过灵活的退火处理,提高了活性金属组分的催化性能和稳定性能,同时不损坏凹凸棒石独有的棒晶状结构。
具体实施方式
下面结合实施例对本发明作进一步详细的描述,但本发明的保护范围并不仅限于此。
实施例1:依以下具体步骤制备Pd/凹凸棒石催化剂
1、将100 g凹凸棒石原矿和300 g水混合均匀,高速剪切机剪切30min,浆料过15目筛,溶液依次经过过滤、烘干、粉碎、过200目筛,得纯化凹凸棒石;
2、将50 g上述纯化凹凸棒石、10 g盐酸和150 ml水混匀,80℃恒温搅拌120 min,然后过滤、烘干、粉碎、过200目筛,制得纳米凹凸棒石;
3、将0.3 g氯钯酸和15g水混合均匀,然后加入纳米凹凸棒石20g,磁力搅拌12 h后,过滤,干燥,粉碎,过200目筛网,得到的粉末100℃真空干燥24 h;
4、将步骤3得到的粉末置于真空管式退火炉中,在氩气保护下300℃退火3h,得到Pd/凹凸棒石催化剂。
该催化剂对氯化苯和苯乙烯的叉偶联反应的具有较好的催化效果,二苯乙烯的产率为94.2%。
实施例2:依以下具体步骤制备Pd/凹凸棒石催化剂
1、将100 g凹凸棒石原矿和500 g水混合均匀,高速剪切机剪切180min,浆料过80目筛,溶液依次经过过滤、烘干、粉碎、过200目筛,得到纯化凹凸棒石;
2、将50 g上述纯化凹凸棒石、50g硫酸和300 ml水混匀,50℃恒温搅拌180 min,然后过滤、烘干、粉碎、过200目筛,制得纳米凹凸棒石;
3、将0.3 g硝酸钯和15g水混合均匀,然后加入纳米凹凸棒石10g,磁力搅拌6 h后,过滤,干燥,粉碎,过200目筛网,得到的粉末100℃真空干燥24 h;
4、将步骤3得到的粉末置于真空管式退火炉中,在氮气保护下500℃退火0.5 h,得到Pd/凹凸棒石催化剂。
该催化剂对氯化苯和4-乙烯基苯硼酸的交叉偶联反应的具有较好的催化效果,4-乙烯基联苯的产率为78.9%。
实施例3:依以下具体步骤制备Pd/凹凸棒石催化剂
1、将100 g凹凸棒石原矿和450 g水混合均匀,高速剪切机剪切90min,浆料过40目筛,溶液依次经过过滤、烘干、粉碎、过200目筛,得到纯化凹凸棒石;
2、将50 g上述纯化凹凸棒石、30 g硝酸和200 ml水混匀,60℃恒温搅拌30 min,然后过滤、烘干、粉碎、过200目筛,制得纳米凹凸棒石;
3、将0.2 g氯钯酸铵和10g水混合均匀,然后加入纳米凹凸棒石8g,磁力搅拌12 h后,过滤,干燥,粉碎,过200目筛网,得到的粉末100℃真空干燥24 h;
4、将步骤3得到的粉末置于真空管式退火炉中,在氩气保护下400℃退火1h,得到Pd/凹凸棒石催化剂。
该催化剂对氯化苯和苯乙烯的交叉偶联反应的具有较好的催化效果,二苯乙烯的产率为87.6%。
Claims (6)
1.用于交叉偶联反应的Pd/凹凸棒石催化剂的制备方法,其特征是该催化剂的制备方法包括以下步骤:首先对凹凸棒石进行制浆提纯、酸活化得到纳米凹凸棒石,然后以纳米凹凸棒石为载体,对Pd盐溶液进行吸附负载,随后经过干燥、退火处理得到Pd/凹凸棒石催化剂。
2.根据权利要求1 所述的用于交叉偶联反应的Pd/凹凸棒石催化剂的制备方法,其特征是:所述的纳米凹凸棒石的制备方法是:
(1)制浆提纯:将100重量份凹凸棒石原矿,300~500重量份水混合均匀,高速剪切机剪切30~180 min,浆料过15~80目筛,溶液依次经过过滤、烘干、粉碎、过200目筛即得纯化凹凸棒石;
(2)酸活化:将50重量份纯化凹凸棒石,150~300重量份水和10~50重量份酸混合均匀,于50~90℃恒温搅拌30~180 min,然后过滤、烘干、粉碎、过200目筛,得纳米凹凸棒石。
3.根据权利要求2所述的用于交叉偶联反应的Pd/凹凸棒石催化剂的制备方法,其特征是:所述的酸为硫酸、盐酸、硝酸中的一种或几种。
4.根据权利要求1 所述的用于交叉偶联反应的Pd/凹凸棒石催化剂的制备方法,其特征是:所述Pd/凹凸棒石催化剂制备方法的具体步骤如下:
(1)称取20重量份纳米凹凸棒石,然后按液固比1:1~2:1(v/g)加入质量分数为2%的Pd盐溶液,搅拌6~24 h,抽滤、洗涤、干燥、粉碎、过100 目筛,得Pd/凹凸棒石粉末;
(2)将Pd/凹凸棒石粉末置于真空管式退火炉中,在氩气或氮气保护下300~600℃退火0.5~3h,即得到Pd/凹凸棒石催化剂。
5.根据权利要求4 所述的用于交叉偶联反应的Pd/凹凸棒石催化剂的制备方法,其特征是:所述的钯盐为硝酸钯、氯钯酸、氯钯酸铵中的一种或几种。
6.根据权利要求1 所述的用于交叉偶联反应的Pd/凹凸棒石催化剂的制备方法,其特征是:所制备的Pd/凹凸棒石催化剂用于交叉偶联反应的赫克反应、根岸反应、铃木反应的催化剂。
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