Poly ethyelen glycol two-phase system and application

A polyethylene glycol, system technology, applied in the direction of carbon monoxide reaction preparation, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc.

Inactive Publication Date: 2005-01-05
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present inventor Jin Zilin etc. reported the synthetic method of the phosphine ligand B-F that contains PEG chain and the application in the hydroformylation reaction of higher carbon olefins of water / organic two-phase temperature control phase transfer catalysis (J.Mol.Catal. 1997, 116, 55; ZL97119429.7, J.Mol.Catal.2001, 171, 85; J.Mol.Catal.1999, 147, 131; ZL, 001261185), but these ligands containing PEG chains have not been Applied in water-liquid / liquid two-phase system

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Phosphine ligand (A)P[O(CH 2 CH 2 O)nCH 3 ] 3 Synthesis

[0023] 44.7mmol average molecular weight of 150, 350, 750, 1150 polyethylene glycol monomethyl ether CH 3 (OCH 2 CH 2 ) m OH, 47.85mmol of triethylamine and 100ml of toluene were placed in a 250ml three-necked flask equipped with mechanical stirring, and 14.5mmol of PCl was dissolved under stirring after cooling to 0°C. 3 40ml of toluene solution was slowly dripped from the dropping funnel within 120 minutes, and the ice-water bath was removed after dripping, and stirring was continued for 9 hours at room temperature.

[0024] in N 2 Under protection, the reaction mixture was filtered, triethylamine hydrochloride was filtered off, and the filtrate was 2 The solvent toluene was vacuumed off under protection to obtain a colorless viscous liquid. NMR analysis data is H 1 NMR (δ, C 6 D. 6 ), δ3.904-3.859(m, 6H), 3.412-3.378(m, 24H), 3.052(S, 9H); 13 CNMR (δ, C 6 D. 6 ), 72.912, 71.971, 71.926, 71.561,...

Embodiment 2

[0026] RhCl 3 / P[O(CH2 CH 2 O)nCH 3 ] 3 (Phosphine Ligand A) Catalyzed Hydroformylation of PEG Two-phase Isobutyl Styrene

[0027] In a 100ml stainless steel autoclave, place 4.0g PEG-4000, 3.0g n-heptane, 3.5g toluene, 1.7g (10mmol) p-isobutylstyrene, internal standard decane and a certain amount of RhCl 3 and Phosphine Ligand A (M=150). Tighten the autoclave, use 2.0MPa synthesis gas (CO / H 2 =1:1) to replace three times and fill to the required reaction pressure. Under the reaction conditions that the temperature is 120°C, the pressure is 5.0MPa, the substrate: rhodium = 1000: 1, and P / Rh = 13, after 2 hours of reaction, after cooling to room temperature, the pressure is released, the lid of the kettle is opened, and the upper layer is separated According to GC analysis of the reaction solution, the conversion rate of p-isobutylstyrene is 100%, and the yield of aldehyde is 95-97%.

Embodiment 3

[0029] Catalyst Separation and Recycling Activity Investigation

[0030] The method is shown in Example 2, the difference is that "re-add 1.7g p-isobutylstyrene" (IBS), 3.5g toluene, 3.0g n-heptane and internal standard decane for each cycle. The experimental results are shown in Table 1.

[0031] Cycles

[0032] As can be seen from Table 1, the catalyst was recycled 7 times, and its activity was basically unchanged, but the aldehyde yield had a certain decline. After 8 cycles, the activity and aldehyde yield had a certain decline. After 8 cycles, the activity and aldehyde yield rates have a downward trend.

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Abstract

A two-phase system is composed of polyethylene glycol (PEG), phosphine ligand containing PEG chain and non-polar organic solvent. It features that when the reaction is taking place at high temp, all reactants are mixed to become one phase, and when the reaction is finished, the PEG phase is automatically separated from the resultant.

Description

technical field [0001] The invention relates to a polyethylene glycol two-phase system and its application, which has the function of temperature-controlled phase change and is used for easy separation and recovery of homogeneous complex catalysts. Background technique [0002] The effective separation and recovery of transition metal homogeneous catalysts through "homogeneous reaction and two-phase separation" is a method of "reaction-separation integration". The reaction system of "homogeneous reaction, two-phase separation" implemented by regulating temperature has fluorine two-phase (Flourous biphasis system, FBS) (Science, 1994,266,72) and other ethylene (propylene) carbonate (Chem .Eng.Technol.2000, 23(2), 122) and polyethylene glycol (Chem.Commun, 1998.787) is a liquid / liquid two-phase system composed of a polar phase and a non-polar organic phase. The report that polyethylene glycol can be combined with certain mixed organic solvents to form a system with "miscibili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/24C07C45/50
Inventor 蒋景阳杨玉川王艳华冯翠兰于凤丽金子林
Owner DALIAN UNIV OF TECH
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