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Removal of dissolved silicates from alcohol-silicon direct synthesis solvents

A silicate and solvent technology, which is applied to the preparation and separation methods of organic silicon compounds and organic compounds, can solve the problems of no disclosure of specific methods for solvent or slurry treatment or recovery, and limitation of long-term use of solvents, and achieves a feasible solution. The effect of good performance and environmental requirements

Inactive Publication Date: 2002-09-11
GENERAL ELECTRIC CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These effects limit the long-term use of the solvent and require treatment or remediation
R.J.Ayen et al. in "Better Ceramics Through Chemistry II" (C.J.Brinker, D.E.Clark and D.R.Ulrich, Editors, Materials Research Society Pittsburgh, PA, 1986, PP, 801-808) demonstrated that this A problem exists, but they do not disclose specific methods for the disposal or recovery of solvents or slurries

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] This example illustrates silicon, dissolved silicate and total solids content in spent solvent for direct synthesis of trimethoxysilane from laboratory and commercial slurry phases.

[0053] table 3

[0054]

Embodiment 2

[0056] This example demonstrates that the rate of solid / liquid separation is effectively increased by adding filter aids to the reaction solvent used. For several polyacrylates (GOOD-RITE  7058, CARBOPOL  980, PEMULEN  ), cellulose based (SOLKAFLOC  ), sorbitol base (MILLITHIX  925) and polyethylene oxide filter aids were tested. The data listed in Table 3 all refer to the direct synthesis of HSi (OCH 3 ) 3 THERMINOL  59 is added with 0.5 (weight)% filter aid.

[0057] In each experiment, 200 g of the solvent used was stirred at 21°C with the appropriate filter aid. Filtration was performed under a nitrogen pressure of 20 psig (137.9 kPa) using stainless steel filters and 142 mm diameter filter pads made of 0.7 micron borosilicate microfibers. The collected filtrate was weighed at time intervals and the weight was plotted against time. The filtration rates (grams per minute) listed in Table 4 are the slopes of the straight line on the rising portion of the curv...

Embodiment 3

[0065] In a 4 liter round bottom four neck flask, 600.25 grams of used solvent A, 150.49 grams of methanol and 30.33 grams of water were mixed together at room temperature. The flask was equipped with a distillation head, a thermometer, an addition funnel and a mechanical stirrer. The used THERMINOL had the properties described in the general reaction procedure. The mixture was heated to reflux temperature for 3 hours. Excess water and methanol were stripped by gradually heating to 120°C and bubbling an appropriate amount of nitrogen. About 188 grams of light stripped material was collected. The flask was cooled to 70°C and the contents of the flask were transferred to a pressure filter using #4 filter paper. The amount of the filtrate is 381.7 grams, which is a golden clear liquid. After analysis and determination, the silicon content is 421ppm. The solids were 189.5 grams and were a wet, lumpy and granular dark gray material. Filtration was easy and quick, followed by ...

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PUM

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Abstract

By adding a compatibilizing agent and water to produce a filterable precipitate, the dissolved silane, siloxane and silicate in the solvent used for the direct synthesis of alkoxysilane in the slurry phase can be removed and a reusable solvent can be obtained. This allows solvent salvage and makes the solvent suitable for reuse in direct synthesis. After remedial treatment, the solvent foam is less and the silicon conversion rate is higher. The precipitate is easy to filter, and the amount of solvent contained in the precipitate is negligible.

Description

field of invention [0001] The present invention relates to the removal of dissolved silanes, siloxanes and silicates from solvents used in the slurry phase direct synthesis of alkoxysilanes. This allows the solvent to be salvaged and made suitable for reuse in the direct synthesis. More specifically, the present invention discloses the use of compatible solvents and water to react dissolved silanes, siloxanes and silicates to form filterable precipitates and reusable solvents. Background of the invention [0002] Trialkoxysilanes, especially trimethoxysilane and triethoxysilane, are commonly used to prepare silane coupling agents. One method of synthesizing trialkoxysilanes is directly from silicon and alcohols. This method is technically known as direct synthesis, direct reaction, direct process or Rochow reaction. [0003] For trialkoxysilanes, the direct synthesis is most conveniently carried out in slurry reactors. In the slurry reactor for the direct synthesis of tr...

Claims

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Application Information

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IPC IPC(8): C07C7/148B01D19/04C07C7/10C07C7/12C07C15/00C07C41/58C07C43/02C07F7/02C07F7/04
CPCB01D19/0404C07F7/025Y02P30/40
Inventor T·L·斯曼丹F·D·曼狄西诺
Owner GENERAL ELECTRIC CO
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