Preparation method of catalyst used in dilute nitric acid treating and alkyl nitrite generating

A technology of alkyl nitrite and catalyst, which is applied in the preparation of nitrite, physical/chemical process catalyst, molecular sieve catalyst, etc., can solve the problems of high content of by-product nitric acid and low selectivity of alkyl nitrite, etc. Low cost, high selectivity, easy to achieve effects

Active Publication Date: 2015-02-11
TONGLIAO GOLD COAL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by this invention is that there is low selectivity of alkyl nitrite esters of C1~C4 chain in the past literature, in O 2 Under the existing situation, the technical problem of high content of by-product nitric acid is proposed, and a preparation method of a catalyst capable of processing dilute nitric acid and generating alkyl nitrite is proposed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Take 10g columnar coal-based activated carbon, pickle it with 50g concentration of 20% hydrochloric acid for 1h, then wash it 4 times with deionized water, carry out oxidation treatment with 50g concentration of 20% nitric acid, then dry it at 120°C Dry and cool in a desiccator for later use.

[0032] (2) with water glass (Na 2 SiO 3 ) is silicon source, sodium metaaluminate (NaAlO 2 ) is aluminum source, sodium hydroxide is raw material, according to the molar composition ratio SiO of molecular sieve synthesis liquid 2 :Al 2 o 3 :TPaOH:EtOH:NaOH:H 2 O=1:0.5:0:0:0:50, mixed and stirred to form a gel.

[0033] (3) Weigh 10 g of the activated carbon obtained in step (1), immerse in 20 g of molecular sieve synthetic liquid, stir at room temperature for 2 h, and continue stirring at 50° C. until dry.

[0034] (4) The activated carbon of 10g coated molecular sieve membrane obtained in step (3) is impregnated in 15g rich in ferric nitrate (Fe(NO 3 ) 3 Mass fraction...

Embodiment 2

[0037] (1) Take 10g columnar coal-based activated carbon, pickle it with 50g concentration of 20% hydrochloric acid for 1h, then wash it 4 times with deionized water, carry out oxidation treatment with 50g concentration of 20% nitric acid, then dry it at 120°C Dry and cool in a desiccator for later use.

[0038] (2) with water glass (Na 2 SiO 3 ) is silicon source, sodium metaaluminate (NaAlO 2 ) is aluminum source, sodium hydroxide is raw material, according to the molar composition ratio SiO of molecular sieve synthesis liquid 2 :Al 2 o 3 :TPaOH:EtOH:NaOH:H 2 O=1:1:1:2:2:100, mixed and stirred to form a gel.

[0039] (3) Weigh 10 g of the activated carbon obtained in step (1), immerse in 20 g of molecular sieve synthetic liquid, stir at room temperature for 2 h, and continue stirring at 50° C. until dry.

[0040] (4) The activated carbon of 10g coated molecular sieve membrane obtained in step (3) is impregnated in 15g rich in ferric nitrate (Fe(NO 3 ) 3 Mass fractio...

Embodiment 3

[0043] (1) Take 10g columnar coal-based activated carbon, pickle it with 50g concentration of 20% hydrochloric acid for 1h, then wash it 4 times with deionized water, carry out oxidation treatment with 50g concentration of 20% nitric acid, then dry it at 120°C Dry and cool in a desiccator for later use.

[0044] (2) With water glass (Na2SiO3) as silicon source, sodium metaaluminate (NaAlO2) as aluminum source, sodium hydroxide as raw material, according to the molar composition ratio of molecular sieve synthetic liquid SiO2: Al2O3: TPaOH: EtOH: NaOH: H2O= 1:1.5:2:4:4:300, mix and stir to form a gel.

[0045] (3) Weigh 10 g of the activated carbon obtained in step (1), immerse in 20 g of molecular sieve synthetic liquid, stir at room temperature for 2 h, and continue stirring at 50° C. until dry.

[0046] (4) The activated carbon of 10g coated molecular sieve membrane obtained in step (3) is impregnated in 15g rich in ferric nitrate (Fe(NO 3 ) 3 Mass fraction 30%) and copper...

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Abstract

The invention relates to a preparation method of a catalyst used in dilute nitric acid treating and alkyl nitrite generating and mainly aims at solving the disadvantages of introducing O2 in the nitrate regeneration process and a series of problems of easy generation of nitric acid, failure in dilute nitric acid treatment, low reaction efficiency, and low nitrite selectivity, and the like in the regeneration process in the prior art. The following technical scheme is adopted: in the presence of an activated carbon coated molecular sieve membrane catalyst, NO reacts with an aqueous solution of alkyl alcohol and nitric acid in a manner of being contacted with the catalyst under the re-circulating conditions in which the reaction temperature is within the range of 60-100 DEG C, a reaction pressure is within the range of 0.28-0.35Mpa, the synthetic gas flow is within the range of 800-1000L/h, the mass fraction of the NO is 8-20%, the mass fraction of the alkyl alcohol is 30-60% in the liquid phase solution and the content of the dilute nitric acid is 1%-10%, due to the reaction, the dilute nitric acid can be completely decomposed into nitrous acid, and the nitrous acid is capable of further reacting with the alkyl alcohol to generate the alkyl nitrite. The catalyst is capable of well being used for catalyzing in the reaction of the dilute nitric acid decomposing and the alkyl nitrite generating with high efficiency, and therefore, the series of problems can be solved. The catalyst can be applied to the regeneration production of the alkyl nitrite in the industry of producing ethylene glycol from coal.

Description

technical field [0001] The invention relates to a method for preparing a catalyst for treating dilute nitric acid and generating alkyl nitrite. The catalyst can be used for the catalytic reduction of dilute nitric acid to generate alkyl nitrite with high efficiency, and is mainly used for coal production In the production of alkyl nitrite regeneration in the glycol industry. Background technique [0002] Oxalate is an important organic chemical raw material, which is widely used in the fine chemical industry. It is mainly used as a solvent or raw material to produce various medicines, dyes, extraction agents and intermediates of chemical raw materials. It is hydrolyzed to prepare oxalic acid and normal pressure Ammonolysis to prepare oxamide; in addition, hydrogenation of oxalate can produce ethylene glycol, a very important chemical raw material, but currently ethylene glycol is mainly prepared through petroleum routes, which has high cost and high energy consumption; since...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/072C07C201/04C07C203/00
Inventor 吴晓金孔国杰梁鹏张学岭吴维果
Owner TONGLIAO GOLD COAL CHEM
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