CN107790187A - 一种含膦配体的催化剂组合物的制备方法 - Google Patents

一种含膦配体的催化剂组合物的制备方法 Download PDF

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CN107790187A
CN107790187A CN201711184613.5A CN201711184613A CN107790187A CN 107790187 A CN107790187 A CN 107790187A CN 201711184613 A CN201711184613 A CN 201711184613A CN 107790187 A CN107790187 A CN 107790187A
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carbon monoxide
olefin polymeric
containing phosphine
rhodium
phosphine ligands
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陈华
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CHENGDU XINHUAYUAN SCIENCE AND TECHNOLOGY Co Ltd
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CHENGDU XINHUAYUAN SCIENCE AND TECHNOLOGY Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
    • B01J31/22—Organic complexes
    • B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
    • B01J31/2208—Oxygen, e.g. acetylacetonates
    • B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
    • B01J31/223—At least two oxygen atoms present in one at least bidentate or bridging ligand
    • B01J31/2234—Beta-dicarbonyl ligands, e.g. acetylacetonates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
    • B01J31/24—Phosphines, i.e. phosphorus bonded to only carbon atoms, or to both carbon and hydrogen atoms, including e.g. sp2-hybridised phosphorus compounds such as phosphabenzene, phosphole or anionic phospholide ligands
    • B01J31/2404—Cyclic ligands, including e.g. non-condensed polycyclic ligands, the phosphine-P atom being a ring member or a substituent on the ring
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
    • B01J31/24—Phosphines, i.e. phosphorus bonded to only carbon atoms, or to both carbon and hydrogen atoms, including e.g. sp2-hybridised phosphorus compounds such as phosphabenzene, phosphole or anionic phospholide ligands
    • B01J31/2495—Ligands comprising a phosphine-P atom and one or more further complexing phosphorus atoms covered by groups B01J31/1845 - B01J31/1885, e.g. phosphine/phosphinate or phospholyl/phosphonate ligands
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/49—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reaction with carbon monoxide
    • C07C45/50—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reaction with carbon monoxide by oxo-reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
    • B01J2231/30—Addition reactions at carbon centres, i.e. to either C-C or C-X multiple bonds
    • B01J2231/32—Addition reactions to C=C or C-C triple bonds
    • B01J2231/321—Hydroformylation, metalformylation, carbonylation or hydroaminomethylation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

本发明公开了一种含膦配体的催化剂组合物的制备方法，其包括以下步骤：（1）将水合六氯铑酸钠与DMF、乙酰丙酮混合制得乙酰丙酮二羰基铑；（2）将乙酰丙酮二羰基铑和双齿亚磷酸酯、2,2‑二（二苯膦甲基）‑1,1，‑联苯反应得到催化剂；（3）将催化剂封装于MCM‑41分子筛中即得到所述含膦配体的催化剂组合物。本发明的催化剂组合物具有高温稳定性，能有效提高烯烃氢甲酰化的反应效率，且易于分离回收。

Description

一种含膦配体的催化剂组合物的制备方法
技术领域
本发明涉及催化剂的技术领域。
背景技术
烯烃氢甲酰化反应是将烯烃反应得到醛类等产物的主要方法，现有技术中用于这一反应的催化剂催化效率较低，反应过程控制困难，催化剂高温稳定性差。
发明内容
本发明的目的在于提出一种具有高温稳定性，能有效提高催化效率，加强反应控制的，且易于分离回收的含膦配体的催化剂组合物的制备方法。
本发明的技术方案如下：
一种含膦配体的催化剂组合物的制备方法，其包括以下过程：
（1）在惰性气体氛围下，将水合六氯铑酸钠与DMF在90~100℃下混合加热0.5~1h，其后加入乙酰丙酮，升温至150~200℃混合加热1.5~2.5h，其后将产物滤出，洗涤，得到乙酰丙酮二羰基铑；
（2）将乙酰丙酮二羰基铑和双齿亚磷酸酯、2,2-二（二苯膦甲基）-1,1，-联苯在惰性气体中混合加热，加热温度为100~200℃，反应完全后，即得到产物含膦配体的催化剂；
（3）将所述含膦配体的催化剂通过封装技术负载于MCM-41分子筛上，即得到所述含膦配体的催化剂组合物。
优选的是：所述催化剂按物质的量的份包括以下原料：0.5~1.5份2,2-二（二苯膦甲基）-1,1，-联苯，0.5~1.5份乙酰丙酮二羰基铑，1~3份双齿亚磷酸酯，0.1~0.3份MCM-41分子筛。
另外优选的是：所述催化剂按物质的量的份包括以下原料：1份三苯甲基膦三间磺酸钠，1.5份乙酰丙酮二羰基铑，2份双齿亚磷酸酯，0.15份MCM-41分子筛。
本发明制得的含膦配体的催化剂组合物具有油溶性，可有效提高烯烃氢甲酰化反应的效率，提高产物的纯度和产率，显著减少副反应，加强对反应过程的控制，且反应完成后易于分离回收。
具体实施方式
一种含膦配体的催化剂组合物的制备方法，其包括以下过程：
（1）在惰性气体氛围下，将水合六氯铑酸钠与DMF在90~100℃下混合加热0.5~1h，其后加入乙酰丙酮，升温至150~200℃混合加热1.5~2.5h，其后将产物滤出，洗涤，得到乙酰丙酮二羰基铑；
（2）将乙酰丙酮二羰基铑和双齿亚磷酸酯、2,2-二（二苯膦甲基）-1,1，-联苯在惰性气体中混合加热，加热温度为100~200℃，反应完全后，即得到产物含膦配体的催化剂组合物。
优选的是：所述催化剂按物质的量的份包括以下原料：0.5~1.5份2,2-二（二苯膦甲基）-1,1，-联苯，0.5~1.5份乙酰丙酮二羰基铑，1~3份双齿亚磷酸酯。
另外优选的是：所述催化剂按物质的量的份包括以下原料：1份三苯甲基膦三间磺酸钠，1.5份乙酰丙酮二羰基铑，2份双齿亚磷酸酯。

Claims (3)

1.一种含膦配体的催化剂组合物的制备方法，其特征在于：包括以下过程：
（1）在惰性气体氛围下，将水合六氯铑酸钠与DMF在90~100℃下混合加热0.5~1h，其后加入乙酰丙酮，升温至150~200℃混合加热1.5~2.5h，其后将产物滤出，洗涤，得到乙酰丙酮二羰基铑；
（2）将乙酰丙酮二羰基铑和双齿亚磷酸酯、2,2-二（二苯膦甲基）-1,1，-联苯在惰性气体中混合加热，加热温度为100~200℃，反应完全后，即得到产物含膦配体的催化剂；
（3）将所述含膦配体的催化剂通过封装技术负载于MCM-41分子筛上，即得到所述含膦配体的催化剂组合物。
2.根据权利要求1所述含膦配体的催化剂组合物的制备方法，其特征在于：所述含膦配体的催化剂组合物按物质的量的份包括以下原料：0.5~1.5份2,2-二（二苯膦甲基）-1,1，-联苯，0.5~1.5份乙酰丙酮二羰基铑，1~3份双齿亚磷酸酯，0.1~0.3份MCM-41分子筛。
3.根据权利要求1所述含膦配体的催化剂组合物的制备方法，其特征在于：所述含膦配体的催化剂组合物按物质的量的份包括以下原料：1份三苯甲基膦三间磺酸钠，1.5份乙酰丙酮二羰基铑，2份双齿亚磷酸酯，0.15份MCM-41分子筛。
CN201711184613.5A 2017-11-23 2017-11-23 一种含膦配体的催化剂组合物的制备方法 Withdrawn CN107790187A (zh)

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