Reaction system and preparation method for nitrous alkyl ester

A technology of alkyl nitrite and reaction system, which is applied in the direction of preparation of nitrite, chemical method for reacting liquid and gaseous medium, chemical instruments and methods, etc., can solve the problem of intensified side reactions and the process of alkyl nitrite Complications and other problems, to achieve the effect of mild operating conditions, convenient continuous production, high conversion rate of raw materials and high product yield

Inactive Publication Date: 2008-12-03
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the above-mentioned patented technologies all need to use a separation system or complicate the process of generating alkyl nitrite due to the aggravation of side reactions.

Method used

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  • Reaction system and preparation method for nitrous alkyl ester
  • Reaction system and preparation method for nitrous alkyl ester
  • Reaction system and preparation method for nitrous alkyl ester

Examples

Experimental program
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Effect test

Embodiment 1

[0016] The trickle bed reactor is a heterogeneous fixed bed reactor in which the gas-liquid two-phase co-current (or countercurrent) contacts the catalyst or packing at the same time. In the trickle bed reactor, the liquid passes through the packed bed layer downwards, and the gas reacts Pass through concurrently (or countercurrently). In the co-current trickle bed reactor, both the gas and liquid phases flow downward, the gas is the continuous phase, the liquid is the dispersed phase, and the liquid flows down along the surface of the catalyst or solid packing in the form of droplets or liquid film; in countercurrent In a trickle bed reactor, the continuous upward flow of gas is opposite to the downward flow of the dispersed liquid phase.

[0017] The main advantages of a trickle bed are:

[0018] (1) The gas-liquid flow is close to the plug flow, and a higher conversion rate can be obtained;

[0019] (2) The liquid flows in the form of a film, so that the resistance of the...

Embodiment 2

[0032] Under the completely identical situation of other conditions and embodiment 1, change liquid phase ethanol and gaseous phase NO, O 2 The feeding mode of the method is a countercurrent mode, and the regeneration reaction of ethyl nitrite is carried out to form the reaction result of Example 2.

[0033] Table 2: Comparison of two gas-liquid phase mixing methods (reaction temperature 60°C)

[0034]

Embodiment 3

[0036] Under the completely identical situation of other conditions and embodiment 1, change NO and O 2 The feed molar ratio, carry out ethyl nitrite regeneration reaction, form the reaction result of embodiment 3 as shown in table 3.

[0037] Table 3: NO and O 2 Comparison of Feed Molar Ratio

[0038]

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Abstract

The invention relates to a reaction system for alkyl nitrite and a preparation method for the alkyl nitrite. The preparation method comprises the following steps that: a trickle-bed reactor is adopted and porcelain ring filler is filled into the trickle-bed reactor; liquid added into the reactor forms liquid membranes on the filler; alkyl alcohol is taken as a liquid-phase raw material and nitric monoxide, oxygen and nitrogen are taken as gas-phase raw materials; and gas and liquid phases are reacted in the trickle-bed reactor by means of co-current flow or countercurrent flow under the condition of nitrogen protection so as to generate the alkyl nitrite. The mol ratio of the alkyl alcohol to NO is between 2 to 1 and 7 to 1, and the mol ratio of the NO to O2 is between 4 to 1 and 8 to 1; the reaction temperature is between 40 and 100 DEG C, and the reaction pressure is between 0.1 and 1.0 MPa; and the retention time of continuous feeding of liquid-phase alkyl alcohol in the trickle-bed reactor is between 10 and 500 minutes, and the retention time of continuous feeding of gas phase in the trickle-bed reactor is between 0.02 and 1 minute. The reaction system and the preparation method have the advantages that: the operating condition is mild; the reaction time is short; the conversion rate of the raw materials, and the selectivity and the yield of products are high; and the whole reaction system is convenient for realizing continuous production, etc.

Description

technical field [0001] The invention relates to a process for synthesizing alkyl nitrite, in particular to a reaction system and a preparation method for alkyl nitrite. Background technique [0002] The synthesis of alkyl nitrite is one of the steps in the process of preparing dialkyl oxalate by gas-phase catalytic coupling of CO. The preparation of dialkyl oxalate by gas-phase catalytic coupling of CO is composed of a coupling-regeneration reaction cycle system, that is, the following two chemical reactions (the alkyl group is exemplified by ethyl) are carried out simultaneously: [0003] 2CO+2C 2 h 5 ONO→2NO+(COOC 2 h 5 ) 2 (1) Coupling reaction [0004] 2C 2 h 5 OH+1 / 2O 2 +2NO→2C 2 h 5 ONO+H 2 O (2) regeneration reaction [0005] [0006] 2CO+2C 2 h 5 OH+1 / 2O 2 →(COOC 2 h 5 ) 2 +H 2 O total response [0007] In this reaction system, the NO produced by the CO coupling reaction (1) is r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/04C07C203/00B01J10/00
Inventor 马新宾李振花王保伟
Owner TIANJIN UNIV
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