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CN110272346A - A kind of method of continuous production Trifluoroacetic Acid Ethyl Ester - Google Patents

A kind of method of continuous production Trifluoroacetic Acid Ethyl Ester Download PDF

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Publication number
CN110272346A
CN110272346A CN201810203029.8A CN201810203029A CN110272346A CN 110272346 A CN110272346 A CN 110272346A CN 201810203029 A CN201810203029 A CN 201810203029A CN 110272346 A CN110272346 A CN 110272346A
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reaction
raw material
trifluoro
trifluoroacetic acid
ethyl ester
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CN110272346B (en
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徐卫国
肖恒侨
章祺
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Zhejiang Lantian Environmental Protection Hi Tech Co Ltd
Sinochem Lantian Co Ltd
Sinochem Lantian Fluorine Materials Co Ltd
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Zhejiang Lantian Environmental Protection Hi Tech Co Ltd
Sinochem Lantian Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093Microreactors, e.g. miniaturised or microfabricated reactors
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/14Preparation of carboxylic acid esters from carboxylic acid halides

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of methods that trifluoro-acetyl chloride and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester, in micro passage reaction, Materials Absolute ethanol is mixed and is reacted in reaction module with trifluoro-acetyl chloride, and Trifluoroacetic Acid Ethyl Ester is obtained after quenching module, and ethanol synthesis finishes.The method that invention provides has that high conversion rate, reaction time are short, reaction is safely controllable, product be easy purifying and can continuous chemical industry amplify.

Description

A kind of method of continuous production Trifluoroacetic Acid Ethyl Ester
Technical field
The present invention relates to a kind of preparation methods of Trifluoroacetic Acid Ethyl Ester, prepare trifluoroacetic acid more particularly, to a kind of serialization The method of ethyl ester.
Background technique
Trifluoroacetic Acid Ethyl Ester is a kind of important Organic Chemicals, is mainly used to synthesize trifluoroacetic ethyl acetoacetate, three The organofluorine compounds such as acetyl fluoride acetone, 2- thioyl trifluoroacetone, it can also be used to prepare pesticide, medicine, dyestuff, liquid crystal With industrial chemical etc..At present in the world more commonly used Trifluoroacetic Acid Ethyl Ester industrially prepared route mainly include the following types:
(1) P69 pages of the phase of " Wenzhou normal academy's report " 1996 the 6th discloses a kind of preparation method of Trifluoroacetic Acid Ethyl Ester, Using trifluoroacetic acid and dehydrated alcohol as primary raw material, catalyst is made with the concentrated sulfuric acid, is heated to reflux, crude product is obtained;Chinese patent CN102276463 is disclosed, and using trifluoroacetic acid and dehydrated alcohol as primary raw material, makees catalyst preparation crude product with the concentrated sulfuric acid, Sulfur trioxide is added inside rectifying Liquid Residue, dilute sulfuric acid is made to become the concentrated sulfuric acid, thus realize recycling, save the cost, but this Method concentrated sulfuric acid usage amount is bigger, and equipment corrosion is more serious;
(2) P4 pages of the phase of volume 48 the 4th of " Zhejiang chemical industry " discloses a kind of preparation method of Trifluoroacetic Acid Ethyl Ester, with trifluoro second Acid and dehydrated alcohol are that primary raw material is heated to reflux with solid super strong acid as catalyst, obtain crude product;" Hebei chemical industry " the 35th Roll up the 6th P24 pages of the phase disclose a kind of preparation method of Trifluoroacetic Acid Ethyl Ester, using trifluoroacetic acid and dehydrated alcohol as primary raw material, Make catalyst with p-methyl benzenesulfonic acid, be heated to reflux, obtains crude product;CN101397249 discloses a kind of system of Trifluoroacetic Acid Ethyl Ester Preparation Method makees catalyst using trifluoroacetic acid and dehydrated alcohol as primary raw material with storng-acid cation exchange resin, is being lower than 50 DEG C and normal pressure under dehydrated alcohol be added dropwise and kept for a period of time make fully reacting.Catalyst is filtered out, solid particle is being filled with Dry in the drying tower of silica gel to remove surplus moisture, air-distillation, the fraction for collecting 58~64 DEG C is finished product.Production process is complete close It is carried out under envelope state, catalyst recycling, tails can be recycled after harvest product.
Although it is catalyst that these methods, which relatively use the concentrated sulfuric acid, technique is more preferable, and yield is higher, and equipment corrosion is not serious, It is that catalyst price is high, there are problems that catalyst treatment, need filtration drying etc..
(3) patent EP1070702 discloses a kind of preparation method of Trifluoroacetic Acid Ethyl Ester, with trifluoro-acetyl chloride and anhydrous second Alcohol is primary raw material, and Trifluoroacetic Acid Ethyl Ester is solvent, to prepare Trifluoroacetic Acid Ethyl Ester;Patent US4916256 discloses one kind three The preparation method of ethyl fluoroacetate becomes ethyl alcohol and trifluoro-acetyl chloride using trifluoro-acetyl chloride and dehydrated alcohol as primary raw material Gas reaction, to prepare Trifluoroacetic Acid Ethyl Ester;Patent EP1070702 discloses a kind of preparation method of Trifluoroacetic Acid Ethyl Ester, with Trifluoro-acetyl chloride and dehydrated alcohol are primary raw material, and the acid solution of salt is catalyst, and to prepare Trifluoroacetic Acid Ethyl Ester, reaction is produced Object is layered to obtain crude product;These complex technical process, ethyl alcohol are not easy fully reacting, and post-processing is complicated, is unable to continuous production.
In the existing technique for preparing Trifluoroacetic Acid Ethyl Ester: preparing Trifluoroacetic Acid Ethyl Ester with ethanol synthesis with trifluoroacetic acid is Prevailing technology needs to use the concentrated sulfuric acid, storng-acid cation exchange resin, to toluene although simple process is easily operated The acidic materials such as sulphur are as catalyst, and there is only catalyst price height, the big and intractable problem of dead catalyst amount, Er Qieyi So that equipment seriously corroded, the high requirements on the equipment;It is prepared in Trifluoroacetic Acid Ethyl Ester technique with trifluoro-acetyl chloride and ethanol synthesis, though Acidic catalyst is not used so, and quantity of three wastes can be reduced, but be reacted again after needing to convert ethyl alcohol to gas, energy consumption of reaction It is higher, while ethyl alcohol cannot react completely, since ethyl alcohol and Trifluoroacetic Acid Ethyl Ester will form azeotropic mixture, product not easy purification, also It needs to remove ethyl alcohol and dry process by washing, regenerates a large amount of waste water, form new environmental issue, and cannot Carry out continuous production.
Therefore, it is necessary to which the preparation process to Trifluoroacetic Acid Ethyl Ester is improved further.
Summary of the invention
The purpose of the present invention is to provide a kind of trifluoro-acetyl chlorides and ethanol synthesis serialization to prepare Trifluoroacetic Acid Ethyl Ester Method enables ethyl alcohol in reaction process fully reacting, to reduce purifying products problem, and enables technique continuous production.
Synthesis route of the invention are as follows:
The invention provides the following technical scheme:
A kind of method that trifluoro-acetyl chloride prepares Trifluoroacetic Acid Ethyl Ester with ethanol synthesis serialization, the method is in microchannel It is carried out in reactor, comprising the following steps:
(1) raw material 1 is made to enter warm-up block 3, preheating temperature is 0~100 DEG C, and the raw material 1 includes dehydrated alcohol;
(2) raw material 1 and raw material 2 after step (1) preheats is made to enter microchannel reaction module 4, the raw material 2 includes three Fluoracyl chloride, raw material 2 are mixed and are reacted in the microchannel reaction module with raw material 1, mole of the raw material 2 and raw material 1 Proportion be 1.5:1~1.0:1,1 flow of raw material be 0.1~10g/min, reaction temperature be 0~100 DEG C, reaction pressure be 0~ 1.0MPa;
(3) reaction module 9 exit in step (2) microchannel obtains compound after quenching module 10 to get to product three Ethyl fluoroacetate.
Trifluoro-acetyl chloride provided by the invention and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester, will be micro- logical before preparation Reactor each module in road is assembled to obtain micro passage reaction.As an example, one piece can be preheated according to shown in attached drawing 3 3, six pieces of microchannel reaction modules 4~9 of module and one piece of quenching module 10 carry out tandem installation, in which: with 3 phase of warm-up block 1 even is liquid phase pump, the feed inlet as raw material 1;1 to be connected with microchannel reaction module 4 is gas mass flow meter, as 2 feed inlet of raw material.
After micro passage reaction connects, conduction oil can be used and conduct heat.Connect in trifluoro-acetyl chloride and ethanol synthesis During continuousization prepares Trifluoroacetic Acid Ethyl Ester, it can according to need and increase or decrease microchannel reaction module, can according to need 2 pieces or 2 pieces of selection or more microchannel reaction module participates in reaction.
Trifluoro-acetyl chloride provided by the invention and ethanol synthesis serialization are prepared in Trifluoroacetic Acid Ethyl Ester method, as preferred Mode, the mass tranfer coefficient of the micro passage reaction is 1~30Ka, exchange capability of heat 1700KW/m2K or more.
Trifluoro-acetyl chloride provided by the invention and ethanol synthesis serialization are prepared in Trifluoroacetic Acid Ethyl Ester method, as preferred Mode, the micro passage reaction is that healthy and free from worry G2 microreactor, microwell array decline channel reactor, finned microchannel plate Answer device, capillary microchannels reactor or multiply parallel type microreactor.
Trifluoro-acetyl chloride provided by the invention and ethanol synthesis serialization are prepared in Trifluoroacetic Acid Ethyl Ester method, described micro- logical Microchannel structure in the reaction module of road reactor includes once-through type channel design and enhancing mixed type channel design.Preferably It is that the once-through type channel design is tubular structure, the enhancing mixed type channel design is T-type structure, spherical structure, spherical shape Band baffle arrangement, drops structure or heart-shaped structure, and channel diameter is 0.5mm~10mm.
Trifluoro-acetyl chloride provided by the invention and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester method, the microchannel The material of reaction module is selected from silicon carbide, breathes out C alloy or manganese Nai Er alloy.
Trifluoro-acetyl chloride provided by the invention and ethanol synthesis serialization are prepared in Trifluoroacetic Acid Ethyl Ester method, raw material 1 into It before entering warm-up block 3, is preheated, preheating temperature is 0~100 DEG C.Preferably, the preheating temperature is 20~80 ℃。
Trifluoro-acetyl chloride provided by the invention and ethanol synthesis serialization are prepared in Trifluoroacetic Acid Ethyl Ester method, raw material 1 with The mol ratio satisfaction of raw material 2 goes on smoothly reaction.As a preferred mode, the raw material 2 and raw material 1 rub Your proportion is 1.5:1~1.0:1.As further preferred mode, the mol ratio of the raw material 2 and raw material 1 be 1.2:1~ 1.05:1。
Trifluoro-acetyl chloride provided by the invention and ethanol synthesis serialization are prepared in Trifluoroacetic Acid Ethyl Ester method, raw material 2 Flow enough goes on smoothly reaction.As a preferred mode, 1 flow of raw material is 0.1~10g/min.
Trifluoro-acetyl chloride provided by the invention and ethanol synthesis serialization are prepared in Trifluoroacetic Acid Ethyl Ester method, step (2) Middle reaction temperature is 0~100 DEG C.As a preferred mode, the reaction temperature is 20~80 DEG C.
Trifluoro-acetyl chloride provided by the invention and ethanol synthesis serialization are prepared in Trifluoroacetic Acid Ethyl Ester method, step (2) Middle reaction pressure is 0~1.0MPa.As a preferred mode, the reaction pressure is 0~0.5MPa.
Trifluoro-acetyl chloride provided by the invention and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester method, with the prior art Compare, have that high conversion rate, the reaction time is short, reaction is safely controllable, product be easy purifying and can continuous chemical industry amplify Characteristic advantage.
Detailed description of the invention
Fig. 1 is the typical structure unit figure of micro passage reaction module used in the present invention;
Fig. 2 is institute of the invention to module map for Corning micro passage reaction;
Fig. 3 is institute of the invention to micro channel reactor system device figure for Corning microchannel module, and in Fig. 3: 1 it is liquid phase pump (1 feed inlet of raw material), 2 be gas mass flow meter (2 feed inlet of raw material), 3 be warm-up block, 4~9 is micro- logical Road reaction module, 10 are quenching module.
Specific embodiment
Next combined with specific embodiments below invention is further explained, but does not limit the invention to these tools Body embodiment.One skilled in the art would recognize that present invention encompasses may include in Claims scope All alternatives, improvement project and equivalent scheme.
Embodiment 1
Select 1 piece of corning straight channel module in attached drawing 2 (as premix warm-up block 3), corning " heart " micro- logical 6 pieces of road reaction module, 1 piece of corning straight channel module (as quenching module 10).It is formed according to reaction process shown in attached drawing 3 Continuous flow microchannel reaction system.Reacting replacing heat medium uses conduction oil.Heat transfer theory is forced according to micro passage reaction, is only existed Two temperature measuring points are arranged in the reactor feed mouth and discharge port.Microchannel reaction system and connecting line are carried out respectively before reaction Water removal is dried, and carries out 1.0MPa airtight test.By 1 liquid phase pump (such as diaphragm metering pump) in attached drawing 3, to microchannel Feed ethanol is added in reaction system continuous-stable.By 2 gas mass flow meters in attached drawing 3, connect to microchannel reaction system It is continuous to be quantitatively adding trifluoroacetyl chlorine body.
55 DEG C of heat exchange temperature of setting, i.e. reaction temperature set reaction pressure 0MPa.Feed ethanol, charging rate are 0.67g/min, trifluoro-acetyl chloride gas feed speed are 2.12g/min, and residence time of reaction is 25s, trifluoro-acetyl chloride with The mol ratio of ethyl alcohol is 1.1:1.Reaction raw materials enter " heart " microchannel reaction module after microchannel premixes warm-up block 3 4, trifluoroacetyl chlorine body is directly entered " heart " microchannel reaction module 4 by gas mass flow meter, micro- logical in " heart " In road reaction module 4-9, trifluoro-acetyl chloride and ethanol synthesis.Crude reaction collects after quenching module 10 and obtains trifluoroacetic acid second Ester crude product.
GC analysis is carried out to the mixed liquor of reaction, the results showed that, the residual quantity of ethyl alcohol is 0, and the conversion ratio of ethyl alcohol is 100%.
Embodiment 2
Using healthy and free from worry micro passage reaction similarly to Example 1, and according to same connection type and control method.This Embodiment changes reaction condition.
60 DEG C of heat exchange temperature of setting, i.e. reaction temperature set reaction pressure 0MPa.Feed ethanol, charging rate are 0.88g/min, trifluoro-acetyl chloride gas feed speed are 2.66g/min, and residence time of reaction is 20s, trifluoro-acetyl chloride with The mol ratio of ethyl alcohol is 1.05:1.Reaction raw materials enter " heart " microchannel plate Ying Mo after microchannel premixes warm-up block 3 Block 4, trifluoroacetyl chlorine body is directly entered " heart " microchannel reaction module 4 by gas mass flow meter, micro- in " heart " In pathway reaction module 4-9, trifluoro-acetyl chloride and ethanol synthesis.Crude reaction collects after quenching module 10 and obtains trifluoroacetic acid Ethyl ester.
GC analysis is carried out to reaction mixture, the results showed that, the residual quantity of ethyl alcohol is 0, and the conversion ratio of ethyl alcohol is 100%.
Embodiment 3
Using healthy and free from worry micro passage reaction similarly to Example 1, and according to same connection type and control method.This Embodiment changes reaction condition.
65 DEG C of heat exchange temperature of setting, i.e. reaction temperature set reaction pressure 0MPa.Feed ethanol, charging rate are 1.68g/min, trifluoro-acetyl chloride gas feed speed are 5.31g/min, and residence time of reaction is 10s, trifluoro-acetyl chloride with The mol ratio of ethyl alcohol is 1.1:1.Reaction raw materials enter " heart " microchannel reaction module after microchannel premixes warm-up block 3 4, trifluoroacetyl chlorine body is directly entered " heart " microchannel reaction module 4 by gas mass flow meter, micro- logical in " heart " In road reaction module 4-9, trifluoro-acetyl chloride and ethanol synthesis.Crude reaction collects after quenching module 10 and obtains trifluoroacetic acid second Ester crude product.
GC analysis is carried out to reaction mixture, the results showed that, the residual quantity of ethyl alcohol is 0, and the conversion ratio of ethyl alcohol is 100%.
Embodiment 4
Using healthy and free from worry micro passage reaction similarly to Example 1, and according to same connection type and control method.This Embodiment changes reaction condition.
80 DEG C of heat exchange temperature of setting, i.e. reaction temperature set reaction pressure 0MPa.Feed ethanol, charging rate are 0.88g/min, trifluoro-acetyl chloride gas feed speed are 2.66g/min, and residence time of reaction is 20s, trifluoro-acetyl chloride with The mol ratio of ethyl alcohol is 1.05:1.Reaction raw materials enter " heart " microchannel plate Ying Mo after microchannel premixes warm-up block 3 Block 4, trifluoroacetyl chlorine body is directly entered " heart " microchannel reaction module 4 by gas mass flow meter, micro- in " heart " In pathway reaction module 4-9, trifluoro-acetyl chloride and ethanol synthesis.Crude reaction collects after quenching module 10 and obtains trifluoroacetic acid Ethyl ester.
GC analysis is carried out to reaction mixture, the results showed that, the residual quantity of ethyl alcohol is 0, and the conversion ratio of ethyl alcohol is 100%.
Embodiment 5
Using healthy and free from worry micro passage reaction similarly to Example 1, and according to same connection type and control method.This Embodiment changes reaction condition.
50 DEG C of heat exchange temperature of setting, i.e. reaction temperature set reaction pressure 0MPa.Feed ethanol, charging rate are 0.56g/min, trifluoro-acetyl chloride gas feed speed are 1.77g/min, and residence time of reaction is 30s, trifluoro-acetyl chloride with The mol ratio of ethyl alcohol is 1.1:1.Reaction raw materials enter " heart " microchannel reaction module after microchannel premixes warm-up block 3 4, trifluoroacetyl chlorine body is directly entered " heart " microchannel reaction module 4 by gas mass flow meter, micro- logical in " heart " In road reaction module 4-9, trifluoro-acetyl chloride and ethanol synthesis.Crude reaction collects after quenching module 10 and obtains trifluoroacetic acid second Ester crude product.
GC analysis is carried out to reaction mixture, the results showed that, the residual quantity of ethyl alcohol is 0, and the conversion ratio of ethyl alcohol is 100%.
Embodiment 6
Using healthy and free from worry micro passage reaction similarly to Example 1, and according to same connection type and control method.This Embodiment changes reaction condition.
30 DEG C of heat exchange temperature of setting, i.e. reaction temperature set reaction pressure 0.1MPa.Feed ethanol, charging rate are 0.26g/min, trifluoro-acetyl chloride gas feed speed are 0.89g/min, and residence time of reaction is 30s, trifluoro-acetyl chloride with The mol ratio of ethyl alcohol is 1.2:1.Reaction raw materials enter " heart " microchannel reaction module after microchannel premixes warm-up block 3 4, trifluoroacetyl chlorine body is directly entered " heart " microchannel reaction module 4 by gas mass flow meter, micro- logical in " heart " In road reaction module 4-9, trifluoro-acetyl chloride and ethanol synthesis.Crude reaction collects after quenching module 10 and obtains trifluoroacetic acid second Ester crude product.
GC analysis is carried out to reaction mixture, the results showed that, the residual quantity of ethyl alcohol is 0, and the conversion ratio of ethyl alcohol is 100%.
Embodiment 7
Using healthy and free from worry micro passage reaction similarly to Example 1, and according to same connection type and control method.This Embodiment changes reaction condition.
40 DEG C of heat exchange temperature of setting, i.e. reaction temperature set reaction pressure 0.1MPa.Feed ethanol, charging rate are 0.32g/min, trifluoro-acetyl chloride gas feed speed are 1.06g/min, and residence time of reaction is 25s, trifluoro-acetyl chloride with The mol ratio of ethyl alcohol is 1.15:1.Reaction raw materials enter " heart " microchannel plate Ying Mo after microchannel premixes warm-up block 3 Block 4, trifluoroacetyl chlorine body is directly entered " heart " microchannel reaction module 4 by gas mass flow meter, micro- in " heart " In pathway reaction module 4-9, trifluoro-acetyl chloride and ethanol synthesis.Crude reaction collects after quenching module 10 and obtains trifluoroacetic acid Ethyl ester.
GC analysis is carried out to reaction mixture, the results showed that, the residual quantity of ethyl alcohol is 0, and the conversion ratio of ethyl alcohol is 100%.
Embodiment 8
Using healthy and free from worry micro passage reaction similarly to Example 1, and according to same connection type and control method.This Embodiment changes reaction condition.
70 DEG C of heat exchange temperature of setting, i.e. reaction temperature set reaction pressure 0.1MPa.Feed ethanol, charging rate are 0.59g/min, trifluoro-acetyl chloride gas feed speed are 1.77g/min, and residence time of reaction is 15s, trifluoro-acetyl chloride with The mol ratio of ethyl alcohol is 1.05:1.Reaction raw materials enter " heart " microchannel plate Ying Mo after microchannel premixes warm-up block 3 Block 4, trifluoroacetyl chlorine body is directly entered " heart " microchannel reaction module 4 by gas mass flow meter, micro- in " heart " In pathway reaction module 4-9, trifluoro-acetyl chloride and ethanol synthesis.Crude reaction collects after quenching module 10 and obtains trifluoroacetic acid Ethyl ester.
GC analysis is carried out to reaction mixture, the results showed that, the residual quantity of ethyl alcohol is 0, and the conversion ratio of ethyl alcohol is 100%.

Claims (8)

1. a kind of method that trifluoro-acetyl chloride and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester, it is characterised in that the method It is carried out in micro passage reaction, comprising the following steps:
(1) raw material 1 is made to enter warm-up block 3, preheating temperature is 0~100 DEG C, and the raw material 1 includes dehydrated alcohol;
(2) raw material 1 and raw material 2 after step (1) preheats is made to enter microchannel reaction module 4, the raw material 2 includes trifluoro second Acyl chlorides, raw material 2 are mixed and are reacted in the microchannel reaction module with raw material 1, the mol ratio of the raw material 2 and raw material 1 For 1.5:1~1.0:1,1 flow of raw material is 0.1~10g/min, and reaction temperature is 0~100 DEG C, reaction pressure is 0~ 1.0MPa;
(3) reaction module 9 exit in step (2) microchannel obtains compound after quenching module 10 to get to product trifluoro second Acetoacetic ester.
2. the method that trifluoro-acetyl chloride described in accordance with the claim 1 and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester, The mol ratio for being characterized in that the raw material 2 and raw material 1 is 1.2:1~1.05:1, and preheating temperature is 20~80 in step (1) ℃。
3. the method that trifluoro-acetyl chloride and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester according to claim 2, It is characterized in that in the step (2) that reaction temperature is 20~80 DEG C.
4. the method that trifluoro-acetyl chloride described in accordance with the claim 1 and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester, It is characterized in that in the step (2) that reaction pressure is 0~0.5MPa.
5. the method that trifluoro-acetyl chloride described in accordance with the claim 1 and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester, In step described in feature (2), raw material 2 is mixed and is reacted in two or more microchannel reaction modules with raw material 1.
6. the method that trifluoro-acetyl chloride described in accordance with the claim 1 and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester, Be characterized in that: microchannel reaction module described in step (2), material are selected from silicon carbide, breathe out C alloy or manganese Nai Er alloy, institute The mass tranfer coefficient for stating micro passage reaction is 1~30Ka, exchange capability of heat 1700KW/m2K or more.
7. the method that trifluoro-acetyl chloride described in accordance with the claim 1 and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester, Be characterized in that: the reaction module of the micro passage reaction, internal microchannel structure includes once-through type channel design and increasing Strong mixed type channel design, the once-through type channel design are tubular structure, and the enhancing mixed type channel design is T junction Structure, spherical structure, spherical band baffle arrangement, drops structure or heart-shaped structure, and channel diameter is 0.5mm~10mm.
8. the method that trifluoro-acetyl chloride described in accordance with the claim 1 and ethanol synthesis serialization prepare Trifluoroacetic Acid Ethyl Ester, Be characterized in that: the micro passage reaction is that healthy and free from worry G2 microreactor, microwell array decline channel reactor, finned microchannel Reactor, capillary microchannels reactor or multiply parallel type microreactor.
CN201810203029.8A 2018-03-13 2018-03-13 Method for continuously producing ethyl trifluoroacetate Active CN110272346B (en)

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CN114160067A (en) * 2021-12-09 2022-03-11 扬州大学 Combined baffle type microreactor
CN115043728A (en) * 2022-06-23 2022-09-13 福建省龙德新能源有限公司 Synthesis method of ethyl trifluoroacetate

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CN103864615A (en) * 2012-12-07 2014-06-18 中化蓝天集团有限公司 Method for preparing ethyl trifluoroacetate through continuous non-catalytic method
CN104418746A (en) * 2013-08-20 2015-03-18 中国石油化工股份有限公司 Method for preparing diphenyl m-phthalate through micro-channel reaction apparatus

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114160067A (en) * 2021-12-09 2022-03-11 扬州大学 Combined baffle type microreactor
CN115043728A (en) * 2022-06-23 2022-09-13 福建省龙德新能源有限公司 Synthesis method of ethyl trifluoroacetate
CN115043728B (en) * 2022-06-23 2023-04-21 福建省龙德新能源有限公司 Synthesis method of ethyl trifluoroacetate

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