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Novel process for catalytic conversion of tetrachloromethane on non-hydrogen condition

A technology for catalyzing carbon tetrachloride and carbon tetrachloride, which is applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, organic chemistry, etc., can solve resource waste and use of tetrachloride Carbon and other issues to achieve the effect of reducing loss

Active Publication Date: 2013-01-16
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But its disadvantage is: carbon tetrachloride is converted into HCl and CO in the reaction 2 , only use HCl and methanol to react to produce monochloromethane, while CO 2 is emitted, and the carbon atoms in carbon tetrachloride are not utilized, resulting in a waste of resources

Method used

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  • Novel process for catalytic conversion of tetrachloromethane on non-hydrogen condition
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  • Novel process for catalytic conversion of tetrachloromethane on non-hydrogen condition

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Embodiment 1

[0021] Weigh the dried Al 2 o 3 3.00g, 2.63g nickel nitrate, dissolve nickel nitrate with 3.9g distilled water to make a solution, add nickel nitrate solution evenly to Al 2 o 3 In, soak for 24 hours. Then put it in air at 120°C for 5 hours, bake at 450°C for 3 hours under the protection of nitrogen, and reduce at 450°C for 3 hours in the presence of hydrogen. The prepared catalyst containing Ni mass percent is 15%, denoted as 15%Ni / Al 2 o 3 .

[0022] In a stainless steel autoclave, 0.3 g of the catalyst prepared above was added, 2 mL of carbon tetrachloride and 28 mL of methanol were added. Close the reactor, replace the air in the reactor with nitrogen for three times, then feed nitrogen and maintain the pressure in the reactor, heat up to 200°C, the reaction pressure is 4.0MPa, start stirring, react at constant temperature for 9 hours, and analyze the product with gas chromatography The results are shown in Table 1.

Embodiment 2

[0024] Weigh the dried SiO 2 4.00g, copper chloride 0.18g, fully dissolve copper chloride with 8.8g distilled water to form a solution, and add copper chloride solution evenly to SiO 2 In, soak for 24 hours. Then put it in the air to dry at 120°C for 5 hours, bake at 300°C for 2 hours under the protection of nitrogen, and reduce at 400°C for 3 hours in the presence of hydrogen. The prepared catalyst contains 2% by mass of Cu, denoted as 2%Cu / SiO 2 .

[0025] In a stainless steel autoclave, 0.8 g of the catalyst prepared above was added, 5 mL of carbon tetrachloride and 25 mL of methanol were added. Close the reactor, replace the air in the reactor with nitrogen for three times, then feed nitrogen and maintain the pressure in the reactor, raise the temperature to 150°C, the reaction pressure is 2.0MPa, start stirring, react at constant temperature for 9 hours, and analyze the product with gas chromatography The results are shown in Table 1.

Embodiment 3

[0027] Replace SiO in Example 2 with mesoporous carbon 2 , using the same catalyst preparation method as in Example 2, the prepared catalyst contains 2% by mass of Cu, which is denoted as 2%Cu / MC.

[0028] In a stainless steel autoclave, add 0.8 g of the catalyst prepared above, add 10 mL of carbon tetrachloride and 20 mL of methanol. Close the reactor, replace the air in the reactor with nitrogen for three times, then feed nitrogen and maintain the pressure in the reactor, heat up to 130°C, the reaction pressure is 2.0MPa, start stirring, react at constant temperature for 9 hours, and analyze the product with gas chromatography The results are shown in Table 1.

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Abstract

The invention relates to a novel process for catalytic conversion of tetrachloromethane on a non-hydrogen condition, which performs reaction in a high-pressure autoclave and includes steps of reacting mixture of the tetrachloromethane and methyl alcohol under protection of inert gas and action of catalyst and transforming the tetrachloromethane into mixture of trichloromethane, dichloromethane and methane chloride, wherein mole ratio of the tetrachloromethane and the methyl alcohol is 1:1-35, usage of the catalyst is 0.8-10% of mass of the tetrachloromethane, operation pressure is 1.0-4.0MPa,and reaction temperature is 130-250 DEG C. The catalyst is prepared by following steps: loading nitrate of active components Ag, Cu and Ni or one or two mixtures in water-soluble chloride on a catalyst carrier which is dried and roasted, drying prepared catalyst precursor in air at a temperature of 80-150 DEG C, and roasting the dried catalyst for 1-6 hours at a temperature of 30-650 DEG C under protection of nitrogen. Further, the roasted catalyst needs to be reduced for 1-5 hours in the presence of hydrogen at a temperature of 200-500 DEG C.

Description

technical field [0001] The invention relates to a new process for converting carbon tetrachloride into a mixture of chloroform, dichloromethane and monochloromethane in the presence of methanol, a catalyst for the reaction and a preparation method. Background technique [0002] Carbon tetrachloride has high stability and is a chemical with a high oxygen consumption index, which is extremely destructive to the ozone layer. Therefore, the use of carbon tetrachloride is strictly limited and is about to be phased out. However, in the industrial production of methane chloride, carbon tetrachloride will be produced as a by-product. Therefore, with the development of technology, some methods of dealing with carbon tetrachloride have emerged, such as thermodynamic incineration, catalytic incineration and catalytic hydrogenation. Since the first two methods will produce secondary pollution, the catalytic hydrogenation method to treat carbon tetrachloride is the main research direct...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/23C07C19/03C07C17/16B01J23/755B01J23/72B01J23/50
Inventor 石小玉李明时鲁墨弘朱建军单玉华
Owner 溧阳常大技术转移中心有限公司
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