A method for continuous production of ethyl trifluoroacetate

A technology of ethyl trifluoroacetate and trifluoroacetyl chloride, which is applied in the field of continuous preparation of ethyl trifluoroacetate, can solve the problems of high equipment requirements, difficult handling, equipment corrosion, etc., and achieve safe and controllable reaction and short reaction time , the effect of high conversion rate

Active Publication Date: 2022-04-19
中化蓝天氟材料有限公司 +2
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Problems solved by technology

[0005] Although these methods use concentrated sulfuric acid as the catalyst, the process is better, the yield is higher, and the equipment corrosion is not serious, but the price of the catalyst is high, there are problems in catalyst treatment, and it needs to be filtered and dried.
[0006] (3) Patent EP1070702 discloses a preparation method of ethyl trifluoroacetate, using trifluoroacetyl chloride and absolute ethanol as main raw materials, and ethyl trifluoroacetate as solvent to prepare ethyl trifluoroacetate; patent US4916256 discloses A preparation method of ethyl trifluoroacetate is proposed, which uses trifluoroacetyl chloride and absolute ethanol as main raw materials, and turns ethanol and trifluoroacetyl chloride into gas to react to prepare ethyl trifluoroacetate; patent EP1070702 discloses a A kind of preparation method of ethyl trifluoroacetate, take trifluoroacetyl chloride and dehydrated alcohol as main raw material, the acid solution of onium salt is as catalyzer, prepares ethyl trifluoroacetate, and reaction product obtains crude product through layering; These technological process Complicated, ethanol is not easy to react completely, the post-processing is complicated, and continuous production is not possible
[0007] In the existing technology for preparing ethyl trifluoroacetate: the preparation of ethyl trifluoroacetate by the reaction of trifluoroacetic acid and ethanol is the mainstream process. Although the process is simple and easy to operate, it needs to use concentrated sulfuric acid, strongly acidic cation exchange resin, and Acidic substances such as toluene sulfonate are used as catalysts, which not only have the problems of high catalyst price, large amount of spent catalysts and difficult disposal, but also easily cause serious corrosion of equipment and require high equipment; the process of preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride with ethanol In the process, although no acidic catalyst is used, the amount of three wastes can be reduced, but the ethanol needs to be converted into a gas and then reacted, and the energy consumption of the reaction is high, and the ethanol cannot be completely reacted at the same time, because ethanol and ethyl trifluoroacetate will form an azeotrope, The product is not easy to purify, and it needs to go through the process of washing to remove ethanol and drying, which regenerates a large amount of waste water, forming new environmental protection problems, and cannot be used for continuous production

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  • A method for continuous production of ethyl trifluoroacetate
  • A method for continuous production of ethyl trifluoroacetate
  • A method for continuous production of ethyl trifluoroacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] optional attachment figure 2 1 piece of corning straight channel module (as premixing preheating module 3), 6 pieces of corning "heart-shaped" microchannel reaction modules, 1 piece of corning straight channel module (as quenching module 10). According to attached image 3 The reaction process shown constitutes a continuous flow microchannel reaction system. Heat transfer oil is used as the reaction heat exchange medium. According to the forced heat transfer principle of the microchannel reactor, only two temperature measuring points are set at the reactor inlet and outlet. Before the reaction, the microchannel reaction system and connecting pipelines were dehydrated and dried, and the air tightness was checked at 1.0MPa. by attaching image 3 1 liquid-phase pump (such as a diaphragm metering pump) in the system continuously and stably adds raw material ethanol to the microchannel reaction system. by attaching image 3 The 2-gas mass flowmeter in the microchannel re...

Embodiment 2

[0038] Use the same Corning microchannel reactor as in Example 1, and follow the same connection and control methods. In this example, the reaction conditions were changed.

[0039] Set the heat exchanger temperature to 60°C, that is, the reaction temperature, and set the reaction pressure to 0 MPa. Raw material ethanol, the feed rate is 0.88g / min, the feed rate of trifluoroacetyl chloride gas is 2.66g / min, the residence time of the reaction is 20s, and the molar ratio of trifluoroacetyl chloride to ethanol is 1.05:1. The reaction raw materials enter the "heart-shaped" micro-channel reaction module 4 after passing through the micro-channel premixing and preheating module 3, and the trifluoroacetyl chloride gas directly enters the "heart-shaped" micro-channel reaction module 4 through the gas mass flow meter. In microchannel reaction modules 4-9, trifluoroacetyl chloride reacts with ethanol. The crude product of the reaction is collected after passing through the quenching mo...

Embodiment 3

[0042] Use the same Corning microchannel reactor as in Example 1, and follow the same connection and control methods. In this example, the reaction conditions were changed.

[0043] Set the heat exchanger temperature to 65°C, that is, the reaction temperature, and set the reaction pressure to 0 MPa. Raw material ethanol, the feed rate is 1.68g / min, the feed rate of trifluoroacetyl chloride gas is 5.31g / min, the residence time of the reaction is 10s, and the molar ratio of trifluoroacetyl chloride to ethanol is 1.1:1. The reaction raw materials enter the "heart-shaped" micro-channel reaction module 4 after passing through the micro-channel premixing and preheating module 3, and the trifluoroacetyl chloride gas directly enters the "heart-shaped" micro-channel reaction module 4 through the gas mass flow meter. In microchannel reaction modules 4-9, trifluoroacetyl chloride reacts with ethanol. The crude product of the reaction is collected after passing through the quenching mod...

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Abstract

The invention discloses a method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride and ethanol. In a microchannel reactor, raw materials such as anhydrous ethanol and trifluoroacetyl chloride are mixed and reacted in a reaction module, and After the quenching module, ethyl trifluoroacetate is obtained, and the ethanol reaction is completed. The method provided by the invention has the advantages of high conversion rate, short reaction time, safe and controllable reaction, easy purification of products and continuous industrial scale-up.

Description

technical field [0001] The invention relates to a method for preparing ethyl trifluoroacetate, in particular to a method for continuously preparing ethyl trifluoroacetate. Background technique [0002] Ethyl trifluoroacetate is an important organic chemical raw material, mainly used to synthesize organic fluorine compounds such as ethyl trifluoroacetoacetate, trifluoroacetylacetone, 2-thienoyl trifluoroacetone, etc. It can also be used to prepare pesticides and medicines , dyes, liquid crystals and industrial chemicals, etc. The industrial preparation route of ethyl trifluoroacetate more commonly used in the world at present mainly contains following several kinds: [0003] (1) "Wenzhou Normal University Newspaper" the 6th phase P69 page of 1996 discloses a kind of preparation method of ethyl trifluoroacetate, take trifluoroacetic acid and dehydrated alcohol as main raw material, make catalyzer with the concentrated sulfuric acid, heat reflux, Obtain crude product; Chinese...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/63C07C67/14B01J19/00
CPCC07C67/14B01J19/0093C07C69/63
Inventor 徐卫国肖恒侨章祺
Owner 中化蓝天氟材料有限公司
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