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Organofunctional surface-modified metal oxides

A modification, silica technology, applied in the fields of organic chemistry, dyeing organosilicon compound treatment, organic chemistry methods, etc., can solve the problem of accelerating the binding reaction of modifying reagents, etc.

Inactive Publication Date: 2009-07-08
WACKER CHEM GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantage is that while the catalyst accelerates the incorporation reaction of the modifying reagent, it often also catalyzes the decomposition reaction of the functional group

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0318] at a temperature of 25°C with N 2 Under inert gas, 1.5 grams of fully deionized (DI) water was added by atomization in very finely divided form to 100 grams of pyrogenic hydrophilic silica having a moisture content of less than 1% and an HCl content of less than 100 ppm and With a specific surface area of ​​130 m2 / g (determined by the BET method according to D1N 66131 and 66132) (trade name WACKER HDK S13, Waker-Chemie GmbH, Munich, D) and atomization via a single-fluid nozzle (pressure: 5 bar) 8.5 g of methacryloxymethyltrimethoxysilane was added. Therefore the loaded silica is subsequently in N 2 React at a temperature of 25°C for 3.0 hours and then purify at 80°C for 1 hour in a 100 L dry box to remove water and MeOH. This gives a white hydrophobic silica powder with a homogeneous layer of silanizing agent.

[0319] Analytical data are shown in Table 1.

Embodiment 2

[0321] at a temperature of 25°C with N 2 Under inert gas, 1.5 g of DI (DI = fully deionized) water was added in very finely divided form by atomization to 100 g of pyrogenic hydrophilic silica having a moisture content of less than 1% and an HCl content of less than 100 Ppm and have a specific surface area of ​​130 m2 / g (determined by the BET method in accordance with DIN 66131 and 66132) (trade name WACKER HDKS13, available from Waker-Chemie GmbH, Munich, D) and atomization via a single-fluid nozzle (pressure: 5 bar) 10.0 g of methacryloxymethyltriethoxysilane was added. Therefore the loaded silica is subsequently in N 2 React at a temperature of 25°C for 3.0 hours and then purify at 80°C for 1 hour in a 100 L dry box to remove water and MeOH. This gives a white hydrophobic silica powder with a homogeneous layer of silanizing agent.

[0322] Analytical data are shown in Table 1.

Embodiment 3

[0324] at a temperature of 25°C with N 2 Under inert gas, 1.5 g of D1 water is added by atomization in very finely divided form to 100 g of pyrogenic hydrophilic silica having a moisture content of less than 1% and an HCl content of less than 100 ppm and a specific surface area of ​​130 square meters / g (determined by the BET method in accordance with DIN 66131 and 66132) (trade name WACKER HDK S13, purchased from Waker-Chemie GmbH, Munich, D) and atomization (pressure: 5 bar) via a single-fluid nozzle was added to 5.0 g Aminomethyldimethylmethoxysilane. Therefore the loaded silica is subsequently in N 2 React at a temperature of 25°C for 3.0 hours and then purify at 80°C for 1 hour in a 100 L dry box to remove water and MeOH. This gives a white hydrophobic silica powder with a homogeneous layer of silanizing agent.

[0325] Analytical data are shown in Table 1.

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Abstract

A method of preparing metal oxides having groups of the following formula I: -O 1+n -SiR 1 2-n -CH 2 - Y(I), the process comprising reacting a solid having OH groups on the surface with a silane of the following formula II: RO 1+n -SiR 1 2-n -CH 2 -Y(II), where R is C-O bonded C 1 -C 15 Hydrocarbyl, R 1 C is a hydrogen atom or a Si-C bond 1 -C 20 Hydrocarbyl, the C 1 -C 20 Hydrocarbyl is unsubstituted or substituted, or C 1 -C 15 Hydrocarbyloxy, wherein one or more non-consecutive methylene units can be formed by the group -O-, -CO-, -COO-, -OCO- or -OCOO-, -S- or -NR X 2 - replacement, and one or more non-consecutive methine units may be replaced by the group -N=, -N=N- or -P=, each R 1 Can be the same or different, Y is a functional group -NR x 2 , -OC(O)C(R)=CH 2 (R=H, C 1 -C 15 Hydrocarbyl), -halogen, -NCO or (R 1 O) 2 (O)P-, R x is a hydrogen atom or C 1 -C 15 Hydrocarbyl or aryl, each R x are the same or different, and n is 0, 1 or 2.

Description

technical field [0001] The present invention relates to a method for preparing organofunctionalized metal oxides and to a metal oxide. Background technique [0002] Surface modification of solids, whether they are powdery or bulky (bulky) solids, often suffers from the problem that the surface modification is not durable, i.e. the surface modifier is not sufficiently immobilized on the surface and is thus absorbed by the solvent or the surrounding medium or matrix. separation and elution. This problem can be overcome by obtaining a firm chemical attachment involving the formation of chemical bonds, as described in EP896029B1. However, the latter approach has the disadvantages of known methods requiring high temperatures and long reaction times, especially when modifiers carrying reactive organic groups such as methacryloyl, epoxy or isocyanate groups can lead to decomposition reactions case. This leads to an undesired decrease in the amount of functional groups and to the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C04B41/00C09D201/02G03G9/08C01B13/14C01B33/18C01F7/02C08K9/06C08L101/00C09C1/00C09C1/30C09C1/56C09C3/12G03G9/097
CPCC09C1/3081C07F7/1844C07B2200/11C01P2006/10C09C3/12C09C1/56C07F7/1804
Inventor 托尔斯滕·戈特沙尔克-高迪希赫伯特·巴特尔于尔根·普法伊费尔
Owner WACKER CHEM GMBH