Preparation process of trimethyl idodine silicon hydride

A technology of trimethyliodosilane and preparation process, which is applied in the fields of compounds, chemical instruments and methods, organic chemistry, etc. It is difficult to control and other problems, so as to achieve the effect of improving product conversion rate, good mass transfer and heat transfer effect, and easy control.

Inactive Publication Date: 2012-10-10
XINYAQIANG SILICON CHEM JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The biggest problem of the traditional preparation process is that there are side reactions in the reaction process, and some previous fractions and residues are produced. At the same time, under high pressure conditions, the operation is difficult to control, the operation safety is low, the product yield is greatly reduced, and the by-products and waste residues increase.

Method used

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  • Preparation process of trimethyl idodine silicon hydride
  • Preparation process of trimethyl idodine silicon hydride
  • Preparation process of trimethyl idodine silicon hydride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] As shown in the figure, the preparation process of the preparation process of iodotrimethylsilane is:

[0033] 1. Preparation of hexamethyldisilane: firstly, to a volume of 1.5m 3 Put 550kg of m-xylene and 100kg of metal potassium into the enamel stirred tank, mix and stir; then add 320kg of trimethylchlorosilane dropwise into the stirred tank, and the dropwise addition is completed within two hours, and the reaction is carried out under a slight positive pressure of 0~0.02MPa , the temperature is controlled below 120°C; stop stirring after the reaction is over, and when the temperature drops to 50°C, the materials in the kettle are introduced into the washing kettle; the unreacted hydrogen chloride gas is absorbed by alkaline water through the falling film absorber;

[0034] 2. Water washing: Add 380 kg of production water to the washing kettle, and control the temperature of the washing kettle to 100°C; after the completion of static sedimentation, the supernatant liq...

Embodiment 2

[0038] As shown in the figure, the preparation process of the preparation process of iodotrimethylsilane is:

[0039] 1. Preparation of hexamethyldisilane: firstly, to a volume of 1.5m 3 Put 580kg of m-xylene and 120kg of metal potassium into the enamel stirred tank, mix and stir; then add 340kg of trimethylchlorosilane dropwise into the stirred tank, and the dropwise addition is completed within two hours, and the reaction is carried out under a slight positive pressure of 0~0.02MPa , the temperature is controlled below 120°C; stop stirring after the reaction is over, and when the temperature drops to 50°C, the materials in the kettle are introduced into the washing kettle; the unreacted hydrogen chloride gas is absorbed by alkaline water through the falling film absorber;

[0040] 2. Water washing: add 400 kg of production water to the washing kettle, and control the temperature of the washing kettle to 100°C; after the completion of static sedimentation, the supernatant liq...

Embodiment 3

[0044] As shown in the figure, the preparation process of the preparation process of iodotrimethylsilane is:

[0045] 1. Preparation of hexamethyldisilane: firstly, to a volume of 1.5m 3 Put 600kg of m-xylene and 140kg of metal potassium into the enamel stirred kettle, mix and stir; then add 360kg of trimethylchlorosilane dropwise into the stirred kettle, and the dropwise addition is completed within two hours, and the reaction is carried out under a slight positive pressure of 0~0.02MPa , the temperature is controlled below 120°C; stop stirring after the reaction is over, and when the temperature drops to 50°C, the materials in the kettle are introduced into the washing kettle; the unreacted hydrogen chloride gas is absorbed by alkaline water through the falling film absorber;

[0046] 2. Water washing: add 400 kg of production water to the washing kettle, and control the temperature of the washing kettle to 100°C; after the completion of static sedimentation, the supernatant...

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Abstract

The invention discloses a preparation process of trimethyl idodine silicon hydride, which comprises the following specific steps of: (1) hexamethyldisiloxane preparation: firstly adding m-xylene and metallic potassium into a stirring kettle, mixing and agitating; and then dropwise adding trimethylchlorosilane into the stirring kettle, stop agitating after reaction and leading materials in the kettle into a washing kettle; (2) washing: adding water into the washing kettle, standing and settling, rectifying generated liquid and recovering solid residues; (3) rectification: adding clear liquid into a rectifying tower kettle, intermittently recovering hexamethyldisilane and intermediate fractions and then recovering the m-xylene; and (4) iodine silane synthesis: adding the rectified hexamethyldisiloxane into a reaction kettle, and adding iodine to generate a trimethyl idodine silicon hydride product. The preparation process has the beneficial effects that the reaction is finished in a micro-positive pressure system, so that the mass transfer and heat transfer effects in the reaction are better, the generated residues in the reaction are less, the product conversion rate is greatly improved, the control is easy, and the operating cost is reduced.

Description

technical field [0001] The invention relates to a preparation process of iodotrimethylsilane. Background technique [0002] The traditional preparation process of iodotrimethylsilane is to firstly react aluminum powder, hexamethyldisiloxane and iodine in a reaction kettle, obtain crude trimethyliodosilane after distillation, and then distill trimethyliodosilane Put the crude product in a still, add copper powder and raise the temperature, collect the distillate to obtain refined iodotrimethylsilane, or directly react trimethylchlorosilane and metal potassium in the reaction kettle under high pressure conditions. [0003] The biggest problem of the traditional preparation process is that there are side reactions in the reaction process, which produce some former fractions and residues. At the same time, under high pressure conditions, the operation is difficult to control, the operation safety is low, the product yield is greatly reduced, and the by-products and waste residue...

Claims

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Application Information

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IPC IPC(8): C07F7/12
Inventor 初亚军
Owner XINYAQIANG SILICON CHEM JIANGSU
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