Method for catalyzing liquid-phase nitration of fat paraffin by using carbon-based solid acid catalyst

A solid acid catalyst, carbon-based solid acid technology, applied in the direction of chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of easy decomposition of catalysts, complex experimental operations, Low catalytic activity and other problems, to achieve the effect of separation, cheap and easy to obtain raw materials, low catalytic activity

Active Publication Date: 2014-01-29
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The main purpose of the present invention is to solve the problems of high reaction temperature, complex experimental operation, need to use a large amount of organic solvent, easy decomposition of catalyst, high synthesis difficulty and low catalytic activity in current nitroalkane production technology

Method used

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  • Method for catalyzing liquid-phase nitration of fat paraffin by using carbon-based solid acid catalyst
  • Method for catalyzing liquid-phase nitration of fat paraffin by using carbon-based solid acid catalyst
  • Method for catalyzing liquid-phase nitration of fat paraffin by using carbon-based solid acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Synthetic steps of naphthalenesulfonic acid methylal carbon-based solid acid catalyst:

[0031] The first step, takes by weighing 10g naphthalene and puts into there-necked flask, under N 2 Under protection, heat it in an oil bath at 150°C to melt it;

[0032] In the second step, add 12mL of sulfuric acid with a mass concentration of 98% to the naphthalene melted in the first step, then raise the temperature to 160°C and keep the temperature constant for four hours to obtain a black liquid;

[0033] In the third step, cool the black liquid in the second step to 105°C, add 14 mL of formaldehyde solution with a mass concentration of 37-40%, raise the temperature to 110°C, and react for 12 hours to obtain a black crude product;

[0034] In the fourth step, use hot water higher than 85°C to filter and wash the black crude product obtained in the third step until there is no SO in the filtrate 4 2- Till now, the resulting filter cake was vacuum-dried at 120°C for 24 hours...

Embodiment 2

[0048] The steps are the same as in Example 2, except that in the third step, 10 mL of formaldehyde solution with a mass concentration of 37 to 40% is added, and the catalyst A is prepared in the fourth step 1 . Its specific surface area is 1.67m 2 / g, the average pore diameter is 14.2nm, and the pore volume is 0.00115cm 3 / g, acid density 4.16mmol / g.

Embodiment 3

[0050] The steps are the same as in Example 2, except that in the third step, 12 mL of formaldehyde solution with a mass concentration of 37 to 40% is added, and the catalyst A is prepared in the fourth step 2 . Its specific surface area is 1.75m 2 / g, the average pore diameter is 6.22nm, and the pore volume is 0.00075cm 3 / g, acid density 4.37mmol / g.

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Abstract

The invention discloses a method for catalyzing liquid-phase nitration of fat paraffin by using a carbon-based solid acid catalyst. The method comprises the following steps: feeding the fat paraffin, nitric acid, a solvent and a naphthalene sulfonic acid methylal carbon-based solid acid catalyst to a high-pressure reaction kettle, wherein the reaction temperature is 105-135 DEG C; the reaction time is 6-24 hours; finally obtaining corresponding nitro fat paraffin, wherein the material ratio is that the molar ratio of the fat paraffin to the nitric acid is 1:(1-3); the mass ratio of the fat paraffin to the carbon-based solid acid catalyst is 1:(0.026-0.26); the volume ratio of the nitric acid to the solvent is 1:(2.2-4.7); the mass percent of the nitric acid is 65-68%. The naphthalene sulfonic acid methylal carbon-based solid acid catalyst for liquid-phase nitration of the fat paraffin disclosed by the invention has the advantages of being simple in preparation method, low in raw material price, available in raw materials, high in acid density, high in catalytic activity and the like.

Description

technical field [0001] The invention relates to the synthesis of nitroalkanes, in particular to a method for catalyzing the liquid-phase nitration of aliphatic alkanes by using a naphthalenesulfonic acid methylal carbon-based solid acid catalyst. technical background [0002] Nitroalkane is an important chemical intermediate and organic solvent. Because of its unique reactivity and physicochemical properties, it has become an important raw material in the field of fine chemicals such as pharmaceuticals, surfactants, solvents, lubricants and emulsifiers, and can be produced There are nearly two thousand derivatives. For example, complete hydrogenation of nitrocyclohexane can produce cyclohexylamine, and partial hydrogenation can reduce cyclohexanone oxime. The former is an important raw material for the synthesis of chemical products such as medicine, fuel, and dyes; the latter can be rearranged by Beckmann to generate caprolactam, which can also be used to produce nylon fib...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/02C07C205/05C07C201/08B01J31/02
Inventor 王荷芳王媛媛杨永芳王延吉贾立元刘红涛
Owner HEBEI UNIV OF TECH
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