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Preparation method for methylaluminoxane, titanium dioxide, white carbon black and phosgene and application of carbon tetrachloride and hexachloroethane

A technology of titanium tetrachloride and silicon tetrachloride, applied in the preparation of phosgene or haloformate, carbon-based compounds, organic compounds, etc., to achieve high anhydrous formaldehyde content, reduce costs, and mild reaction conditions Effect

Inactive Publication Date: 2013-05-08
李坚
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

To protect the ozone layer, the production and sale of carbon tetrachloride has been banned by the government [5] However, the carbon tetrachloride by-product in my country still reaches nearly 60,000 tons every year, and there is an increasing trend [6] , the development of downstream products of carbon tetrachloride has become a major and difficult technical task in terms of low carbon emissions. If such a large amount of by-products are consumed industrially according to the past organic synthesis methods, it will be difficult for a long time in the future It is done, according to regulations, tens of thousands of tons of carbon tetrachloride need to be sent to incineration every year

Method used

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  • Preparation method for methylaluminoxane, titanium dioxide, white carbon black and phosgene and application of carbon tetrachloride and hexachloroethane
  • Preparation method for methylaluminoxane, titanium dioxide, white carbon black and phosgene and application of carbon tetrachloride and hexachloroethane
  • Preparation method for methylaluminoxane, titanium dioxide, white carbon black and phosgene and application of carbon tetrachloride and hexachloroethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0200] Embodiment 1, the preparation of methylalumoxane

[0201] Method 1, put in aluminum trichloride (0.2mol), active zinc powder (0.2mol) and anhydrous tetrahydrofuran 40g, start stirring, heat up to reflux, slowly add anhydrous solid sodium methoxide (0.2mol), and keep warm for 8~ After 12 hours, lower the temperature, add 400 g of toluene, add 50 g of water to dissolve NaCl and zinc chloride, separate the water layer, and distill under vacuum to obtain about 10% methylalumoxane in toluene solution product with a yield of 94%.

[0202] Method 2: Add methylaluminum dichloride (0.2mol) and toluene (348g) as solvents, start stirring, control the temperature at 40-105°C, slowly add anhydrous sodium hydroxide solid (0.2mol), and react for 2-18 hours . Cool down, let stand, filter, and filter out the NaCl solid to obtain a toluene solution of about 10% methylaluminoxane, with a yield of 98%.

Embodiment 2

[0203] Embodiment 2, the preparation of titanium dioxide (titanium dioxide)

[0204] Method 1, put in 99% TiCl 4 (0.2mol) and o-dichlorobenzene (120g), start stirring, control the temperature at 20-200°C, add pure water (0.2mol) slowly, and keep the temperature for 2-8 hours. Add anhydrous NaOH solid (0.2mol) slowly, control the temperature at 100-200°C, and keep warm for 4-12 hours. Cool down, stand still, filter, wash with water, and dry to obtain titanium dioxide crystals with a content of 99% and a yield of 94%.

[0205] Method 2, put in 99% TiCl 4 (0.2mol) and o-dichlorobenzene (120g), start stirring, control the temperature at 20-200°C, slowly add dry anhydrous paraformaldehyde or formaldehyde (0.2mol) gas, and continuously release the generated dichlorobenzene The methane is distilled out and recovered through the rectification column, and the heat preservation reaction is carried out for 2 to 18 hours. Then, slowly add anhydrous sodium hydroxide solid (0.2 mol), an...

Embodiment 3

[0206] Embodiment 3, the preparation of white carbon black (silicon dioxide)

[0207] Method 1, put in 99% silicon tetrachloride (0.2mol) and o-dichlorobenzene, start stirring, control the temperature at 20-200°C, slowly add pure water (0.2mol), and keep warm for 4-12 hours. Then slowly add anhydrous NaOH solid, and keep warm for 4 to 12 hours. Cool down, stand still, filter, wash with water, and dry to obtain silicon dioxide crystals with a content of 99% and a yield of 95%.

[0208] Method 2, put in 99% silicon tetrachloride (0.2mol) and o-dichlorobenzene (120g), start stirring, control the temperature at 20-200°C, and slowly add dry anhydrous paraformaldehyde (0.2mol) or formaldehyde Gas (0.2mol), during the process, the dichloromethane that is continuously generated is distilled out in time and recovered for later use. The heat preservation reaction is carried out for 2 to 18 hours, the temperature is lowered, left standing, filtered, washed with water, and dried to obtai...

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Abstract

The invention provides a preparation method for methylaluminoxane, titanium dioxide, white carbon black and phosgene and application of carbon tetrachloride and hexachloroethane, which relates to a universal novel organic synthesis method titled as Tandem Substitution Rearrangement Reaction of Elementary Organic Chemistry, a TSRE reaction for short. With the method, improvement can be made to clean production processes and application of hundreds of chemical products; zero discharge of waste water in the process of production of a product can be realized; and the method has the characteristics that the problem of waste water discharge can be overcome from a source and consumption of energy can be greatly reduced.

Description

[0001] The invention relates to a new universal reaction method for organic synthesis, which is called "tandem substitution rearrangement reaction of elemental organic chemistry", TSRE reaction for short. This method can improve the clean production process and use of hundreds of thousands of chemical products, and the process of preparing products can achieve zero discharge of wastewater. Its characteristic is that it can solve the problem of wastewater discharge from the source of production, and, Can significantly reduce energy consumption. Background technique [0002] The applicant has applied for dozens of patents, has been engaged in the technical service work of enterprises for a long time, and has invented new preparation methods for many different chemical products. Recently, after the applicant calmed down, he summarized the past technical work and found that these new preparation methods seem to have a consistent red line, thus summarizing the tandem substitution r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06C01G23/053C01B33/12C07C69/96C07C68/02C07C19/045C07C17/361C07C47/04C07C45/51C07C43/04C07C41/16C07C11/04C07C1/30C07C53/48C07C51/58C01B31/28C07D295/027C07D295/023C01B32/80
Inventor 李坚
Owner 李坚