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Method for preparing polyether-modified silicone oil in presence of MOFs (metal-organic frameworks) supported catalyst

A technology of supported catalyst and polyether-modified silicone oil, applied in chemical recovery and other directions, can solve problems such as no binding, and achieve the effect of reducing synthesis cost and not reducing catalytic activity

Active Publication Date: 2015-08-05
GUANGZHOU TINCI MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report in the prior art that it is combined with a homogeneous catalyst for hydrosilylation reaction and successfully used in the catalytic synthesis of polyether modified silicone oil

Method used

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  • Method for preparing polyether-modified silicone oil in presence of MOFs (metal-organic frameworks) supported catalyst
  • Method for preparing polyether-modified silicone oil in presence of MOFs (metal-organic frameworks) supported catalyst
  • Method for preparing polyether-modified silicone oil in presence of MOFs (metal-organic frameworks) supported catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] This embodiment has the synthesis of the MOFs supported catalyst of structural formula (II), and its synthetic route is as follows figure 1 shown.

[0050]

[0051] Its synthetic steps are:

[0052] (1) Under the protection of nitrogen, add 1.3g of pyrrole and 3.2g of p-bromobenzaldehyde into a 2L three-necked flask, add 1.5L of dichloromethane after drying and dehydration at room temperature, and add 3.7mL of trifluoroacetic acid after 10min, Stir at room temperature under nitrogen protection for 1.0h, then add 9g DDQ (dichlorodicyanobenzoquinone), continue to stir for 1.0h, then remove the solvent under reduced pressure, and the crude product is separated using a chromatographic column (stationary phase: silica gel; Mobile phase: petroleum ether / dichloromethane with a volume ratio of 1:1) to obtain organic framework monomer compound 1 with a yield of 30%; mass spectrometry test results: (MALDI-TOF): m / z=926.9, calculated value: 926.9;

[0053] (2) Under nitrogen p...

Embodiment 2

[0056] This embodiment has the synthesis of the MOFs supported catalyst of structural formula (III), and its synthetic route is as follows figure 2 shown.

[0057]

[0058] Its synthetic steps are:

[0059] (1) Under the protection of nitrogen, add 1.3g of pyrrole and 4.7g of 2,4-dibromobenzaldehyde into a 2L three-necked flask, add 1.5L of dichloromethane after drying and dehydration at room temperature, and add 3.7mL of tris Fluoroacetic acid, stirred at room temperature under nitrogen protection for 1.0h, then added 9g DDQ (dichlorodicyanobenzoquinone), continued to stir for 1.0h, then removed the solvent under reduced pressure, and the crude product was separated using a chromatographic column (stationary phase : silica gel; Mobile phase: petroleum ether / dichloromethane with a volume ratio of 1:1) to obtain organic framework monomer compound 3 with a yield of 30%; mass spectrometry test results: (MALDI-TOF): m / z=1245.9, Calculated value: 1245.9;

[0060] (2) Under n...

Embodiment 3

[0063] This embodiment has the synthesis of the MOFs supported catalyst of structural formula (IV), and its synthetic route is as follows image 3 shown.

[0064]

[0065] Its synthetic steps are:

[0066] (1) Under nitrogen protection, add 1.3g of pyrrole and 6.2g of 2,4,6-tribromobenzaldehyde into a 2L three-necked flask, add 1.5L of dichloromethane at room temperature, and add 3.7 mL trifluoroacetic acid, stirred at room temperature under nitrogen protection for 1.0h, then added 9g DDQ (dichlorodicyanobenzoquinone), continued to stir for 1.0h, then removed the solvent under reduced pressure, and the crude product was separated using a chromatographic column ( Stationary phase: silica gel; Mobile phase: petroleum ether / dichloromethane with a volume ratio of 1:1) to obtain organic framework monomer compound 5 with a yield of 30%; mass spectrometry test results: (MALDI-TOF): m / z= 1561.5, calculated value: 1561.5;

[0067] (2) Under nitrogen protection, 8.9g of compound 5...

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Abstract

The invention belongs to the technical field of organic silicon synthesis, and particularly relates to a method for preparing polyether-modified silicone oil in presence of an MOFs (metal-organic frameworks) supported catalyst. The preparation method includes the steps: performing hydrosilylation reaction of hydrogen containing silicone oil and allyl polyether without solvents in presence of the MOFs supported catalyst; filtering and separating the catalyst after reaction to obtain the polyether-modified silicone oil. The MOFs supported catalyst has a structural formula indicated in a formula (I), M refers to platinum, rhodium, palladium or ruthenium, and R1 and R2 are same or different H or Br. The hydrosilylation reaction of the hydrogen containing silicone oil and the allyl polyether is catalyzed by the MOFs supported catalyst which can be recycled by a simple method, and the quality of the polyether-modified silicone oil and the use ratio of precious metals can be effectively improved.

Description

technical field [0001] The invention belongs to the technical field of organosilicon synthesis, and in particular relates to a method for preparing polyether-modified silicone oil under a MOFs supported catalyst. Background technique [0002] Silicone surfactant is a new type of surfactant developed with new silicone materials. The Si-O-Si link in the main chain of its structure has a stronger hydrophobic effect than traditional carbon chain surfactants. It thus has an excellent ability to reduce surface tension. Among them, polyether-modified silicone surfactants are the most widely studied and have the most product types, which are widely used in cosmetic additives, polyurethane foam stabilizers, fabric finishing agents, defoamers and coatings. [0003] The main synthesis method of polyether modified silicone oil is to use the Si-H bond and the unsaturated double bond between the hydrosilylation reaction, the catalyst used is mostly complexes of noble metals, such as: pla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46C08G77/08
CPCY02P20/584
Inventor 吴伟张宇张利萍雷秋芬郭守彬
Owner GUANGZHOU TINCI MATERIALS TECH
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