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Hybrid inorganic/organic polymer catalytic membrane material including immobilized molecular catalyst and its preparation

A technology of molecular catalysts and catalytic materials, applied in the field of new catalytic hybrid inorganic/polymer materials, can solve the problem of no reactor, no method of manufacturing polymer catalytic membranes, and unsuccessful development of polymer catalytic membranes And other issues

Inactive Publication Date: 2016-08-03
NIPPON KODOSHI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] The current state of the art clearly shows that polymer-based catalytic membranes for highly (stereo)selective chemical reactions have not yet been successfully developed, and likewise neither reactors based on these polymer-based catalytic membranes nor based on These polymer-based catalytic membrane methods

Method used

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  • Hybrid inorganic/organic polymer catalytic membrane material including immobilized molecular catalyst and its preparation
  • Hybrid inorganic/organic polymer catalytic membrane material including immobilized molecular catalyst and its preparation
  • Hybrid inorganic/organic polymer catalytic membrane material including immobilized molecular catalyst and its preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment I

[0048] This example illustrates the general procedure for preparing immobilized hybrid inorganic / polymeric materials, especially membranes, for preformed molecular catalysts. The raw material aqueous solution is passed through a predetermined amount of sodium silicate and / or sodium tungstate dihydrate (Na 2 WO 6 2H 2 O) obtained by mixing into 100 ml of 10% by weight polyvinyl alcohol solution. PVA has an average degree of polymerization of 3100-3900 and a degree of saponification of 86-90%. A hydrochloric acid solution having a concentration of 2.4 M was added dropwise to the raw material aqueous solution under stirring for co-existing neutralization, which induced a hybridization reaction.

[0049] The precursor solution was cast on the polyester film of the coating device with the plate heated to a temperature of 60-80°C. The coating equipment was an RK Print Coat Instruments Ltd. electric coater (Kcontrolcoater) having a doctor blade for adjusting the gap with a microm...

Embodiment II

[0053] This example illustrates the general procedure for preparing a catalytic membrane by immobilizing a pre-formed metal catalyst on a hybrid inorganic / polymer membrane prepared as described in Example I according to the method of the invention as described above.

[0054] will be in 2 1cm clamped between windows 2 Hybrid inorganic / PVA membrane support samples were introduced into round bottom glass flasks equipped with lateral stopcocks. Methanol (10 mL) was introduced into the flask degassed with three vacuum / nitrogen cycles. The pre-formed metal complex catalyst (3.10 -3 mmol) of nitrogen degassed solution was passed under nitrogen flow Capillary transfer to flask. The flask was stirred at room temperature for 24 h by means of an orbital shaker. Afterwards, the methanol solution was removed from the flask by decantation under a nitrogen flow, the membrane was carefully washed with sequential addition / removal of degassed MeOH portions (3×15 mL) and dried under a ni...

Embodiment III

[0057] This example illustrates: according to the method of the invention as described in the preceding examples, based on the immobilization of a pre-formed rhodium catalyst [((-)-BINAP)Rh( NBD)]PF 6 Steps to prepare the catalytic membrane.

[0058] will be in 2 1cm clamped between windows 2 (6.76 mg) hybrid inorganic / PVA membrane carrier type NK-1 was introduced into a round bottom glass flask fitted with a side stopper. Methanol (10 mL) was introduced into the flask degassed with three vacuum / nitrogen cycles. The preformed rhodium catalyst [((-)-BINAP)Rh(NBD)]PF in methanol (5 mL) was then 6 (3.00mg, 3.1·10 -3 mmol) of nitrogen degassed solution was passed under nitrogen flow Capillary transfer to flask. The flask was stirred at room temperature for 24 h by means of an orbital shaker. Afterwards, the methanol solution was removed from the flask by decantation under a nitrogen flow, the membrane was carefully washed with sequential addition / removal of degassed MeOH...

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Abstract

A low-cost, feasible and modular method for the preparation of new, highly selective "catalytic membranes" and their use in various types of reactors is disclosed. The membranes are versatile and reusable with negligible catalyst leaching, especially in the asymmetric hydrogenation of substituted α,β-unsaturated acids or esters. The membrane comprises a hybrid inorganic / polymer carrier material (i) and a molecular catalyst (ii) immobilized on the hybrid inorganic / polymer carrier material (i), wherein -(i) consists of an inorganic compound and an organic The hybrid inorganic / macromolecular compound composed of polymer chemical combination; -The inorganic compound is at least one selected from silicic acid compound, tungstic acid compound, molybdic acid compound and stannic acid compound; -The organic polymer Has a hydroxyl group, preferably polyvinyl alcohol (PVA); -(ii) is a pre-formed metal catalyst comprising at least one selected from Ru, Rh, Pd, Ir, Ni, Pt, Au A transition metal and at least one chiral ligand selected from phosphinos, aminos and / or amino-phosphines, preferably DIOP, BINAP monophosphorus or TMBTP.

Description

technical field [0001] The present invention relates to novel catalytic hybrid inorganic / polymer materials, especially catalytic hybrid inorganic / polymer membranes, which exhibit high selectivity, activity, stability, reusability and Low metal leaching. More specifically, the present invention relates to the manufacture of low-cost hybrid materials of the polyvinyl alcohol type, especially membranes, and to the immobilization of selective catalysts on said materials, to the production of catalytic materials exhibiting the above specific properties, their reactors Assemblies in and their use in chemical processes. The use of such materials is particularly useful for, but not limited to, the asymmetric hydrogenation of prochiral, unsaturated organic substrates. Background technique [0002] Sustainable, ie cost-effective and environmentally friendly, highly selective process development for the production of fine chemicals (pharmaceuticals, agrochemicals, fragrances, etc.) i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/16B01J31/24B01J35/06B01J37/03C07C5/03C07B53/00B01J31/06B01J21/08B01J23/28B01J23/30B01J23/14
CPCB01J31/069B01J31/1683B01J31/1691B01J31/2226B01J31/2295B01J31/2414B01J31/2447B01J31/2466B01J2231/645B01J2531/0266B01J2531/0272B01J2531/18B01J2531/821B01J2531/822B01J2531/824B01J2531/827B01J2531/828B01J2531/847C07B53/00C07B2200/07C07C231/18C07C233/47B01J31/24B01J37/03
Inventor P·巴巴洛C·比安奇尼F·利果里泽春夫F·维扎
Owner NIPPON KODOSHI
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