Preparation method for nitrogen-containing activated carbon catalyst

A technology of activated carbon and catalyst, applied in the field of preparation of nitrogen-containing activated carbon catalyst, can solve the problems of lack of direct data to prove the existence and exact role of nitrogen-containing functional groups, lack of pertinence of high-nitrogen-containing activated carbon, waste of nitrogen-containing reagents, etc. The high temperature activation period is short, the cost is low, and the process is safe and controllable.

Active Publication Date: 2012-07-11
中国中化股份有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Pinel only speculates that the active center of the reaction is a specific nitrogen-containing functional group on activated carbon, but there is no direct data to prove the existence and exact role of the nitrogen-containing functional group
At the same time, because the method needs to feed a large amount of high-temperature ammonia gas, the obtained high nitrogen-containing activated carbon lacks pertinence, and only contains a small part of nitrogen-containing functional groups that can promote the oxidation of diglyphosate to glyphosate, which wastes nitrogen-containing reagents; In addition, this method is difficult to produce on a large scale due to defects such as high energy consumption, complicated operation, and long preparation time.

Method used

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  • Preparation method for nitrogen-containing activated carbon catalyst
  • Preparation method for nitrogen-containing activated carbon catalyst

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Experimental program
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Embodiment 1

[0029] 1) Raw material pretreatment: with the coconut core carbonized material as raw material, the carbonized material used in the present invention comes from a certain activated carbon factory in Hebei. Atmospheric pressure, 60°C, with 68% HNO 3 Immerse the carbonized material at a volume ratio of 2:1 for 24 hours, filter to remove the impregnating solution, wash the residue with deionized water until neutral, and dry at 110°C to constant weight to obtain the treated carbonized material;

[0030] 2) Introduction of nitrogen-containing reagents: crush the dried carbonized material, sieve 100-200 meshes after crushing, mix nitrogen-containing reagent urea into a quartz boat at a molar ratio of N / C of 0.64;

[0031] 3) Activation: Continuous N at a flow rate of 10mL / min 2 Under protection, raise the temperature to 200°C and keep it warm for 2 hours; continue to raise the temperature to 700°C, keep it warm for 8 hours, then stop heating and drop to room temperature to get the ...

Embodiment 2-3

[0038] Respectively with hawthorn core (example 2), peach core (example 3) carbonized material as raw material, melamine is nitrogen-containing reagent, prepare nitrogen-containing activated carbon catalyst as follows:

[0039] 1) Raw material pretreatment: under normal pressure and 100°C, use 68% HNO 3 Reflux the carbonized material at a volume ratio of 2:1 for 4 hours, filter, wash the residue with deionized water until neutral, and dry at 110°C to constant weight to obtain the treated carbonized material;

[0040] The 2nd)-4) step operation is the same as embodiment 1. Catalyst number: AC-2 made from hawthorn kernel charred material, and catalyst number: AC-3 made from peach kernel charred material. Its elemental analysis test and reactivity test method are the same as in Example 1, and the test results are listed in Table 1.

Embodiment 4-5

[0042] In order to illustrate the nitrogen-containing carbon prepared when aniline used in the present invention is a nitrogen-containing reagent, this group of embodiments uses apricot stone (example 4) and coal powder (example 5) charring material as raw materials respectively, and aniline is a nitrogen-containing reagent, by following Steps to prepare nitrogen-containing activated carbon:

[0043] 1) Raw material pretreatment: use apricot kernels or pulverized coal carbonization materials as raw materials respectively, under normal pressure, at 80°C, use 68% HNO 3 Immerse the carbonized material at a volume ratio of 2:1 for 12 hours, filter, wash the residue with deionized water until neutral, and dry at 110°C to constant weight to obtain the treated carbonized material;

[0044] 2) Introduction of nitrogen-containing reagent: crush the dried carbonized material, sieve 100-200 meshes after crushing, mix nitrogen-containing reagent aniline with N / C ratio of 0.64, and put it ...

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Abstract

The invention discloses a preparation method for a nitrogen-containing activated carbon catalyst. The method comprises the following steps of: 1) pre-treating a carbonized material; 2) introducing a nitrogen-containing reagent, wherein the nitrogen-containing reagent is selected from carbamide, melamine or phenylamine, and the adding molar ratio of the carbonized material to the nitrogen-containing reagent is 1:(0.1 to 10); 3) activating in one step; and 4) refining. Compared with the traditional nitrogen-containing activated carbon catalyst, the catalyst prepared by the method has the advantages of high activity, long service life, high yield of reaction product, i.e., glyphosate when the catalyst is applied to the oxidization of N-phosphonomethyl aminodiacetic acid, and the like. The preparation method has the advantages of low pollution, safe and controllable process, short high-temperature activation period, low energy consumption, simple process, low cost and the like.

Description

technical field [0001] The invention belongs to the field of catalyst preparation and relates to a preparation method of a nitrogen-containing activated carbon catalyst. Background technique [0002] Glyphosate (chemical name: N-(phosphonomethyl) glycine, English name: glyphosate) was first successfully developed by Monsanto Chemical Company in the United States in 1974. herbicide. With the successful development and large-scale planting of glyphosate transgenic crops, as well as the promotion of biofuel crops caused by the energy crisis, glyphosate has become the largest and fastest growing herbicide variety in the world. [0003] In the international mainstream iminodiacetic acid production route of glyphosate, the key step is the catalytic oxidation of diglyphosate to synthesize glyphosate. Hershman disclosed in US3969398 that commercially available activated carbon (hereinafter referred to as "Norit activated carbon") in the presence of an oxidizing agent can be used a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02
Inventor 闫海生黄瑞尹荃高双飞任树杰赵瑞强张媛孙鸿曼宋扬刘淑杰
Owner 中国中化股份有限公司
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