CN110272346B - Method for continuously producing ethyl trifluoroacetate - Google Patents
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Abstract
The invention discloses a method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride and ethanol. 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 amplification.
Description
Technical Field
The invention relates to a preparation method of ethyl trifluoroacetate, in particular to a method for continuously preparing ethyl trifluoroacetate.
Background
Ethyl trifluoroacetate is an important organic chemical raw material, is mainly used for synthesizing organic fluorine compounds such as ethyl trifluoroacetoacetate, trifluoroacetylacetone, 2-thenoyltrifluoroacetone and the like, and can also be used for preparing pesticides, medicines, dyes, liquid crystals, industrial chemicals and the like. The industrial preparation routes of the ethyl trifluoroacetate which are commonly used internationally at present mainly comprise the following steps:
(1) a preparation method of ethyl trifluoroacetate is disclosed in the report of Wenzhou academy of academic sciences at No. 6P 69 of 1996, trifluoroacetic acid and absolute ethyl alcohol are used as main raw materials, concentrated sulfuric acid is used as a catalyst, and heating reflux is carried out to obtain a crude product; chinese patent CN102276463 discloses that trifluoroacetic acid and absolute ethyl alcohol are used as main raw materials, concentrated sulfuric acid is used as a catalyst to prepare a crude product, sulfur trioxide is added into a rectification residual liquid to change dilute sulfuric acid into concentrated sulfuric acid, so that recycling is realized, and cost is saved;
(2) zhejiang chemical engineering, volume 48, No. 4, P4, discloses a preparation method of ethyl trifluoroacetate, which comprises the steps of taking trifluoroacetic acid and absolute ethyl alcohol as main raw materials, taking solid superacid as a catalyst, heating and refluxing to obtain a crude product; the Hebei chemical engineering, 35 th volume, 6 th phase P24, discloses a preparation method of ethyl trifluoroacetate, which comprises the steps of taking trifluoroacetic acid and absolute ethyl alcohol as main raw materials, taking P-toluenesulfonic acid as a catalyst, heating and refluxing to obtain a crude product; CN 10139249 discloses a method for preparing ethyl trifluoroacetate, which uses trifluoroacetic acid and absolute ethyl alcohol as main raw materials, uses strong acid cation exchange resin as a catalyst, and adds absolute ethyl alcohol dropwise at a temperature lower than 50 ℃ and under normal pressure for a period of time to complete the reaction. And filtering out the catalyst, drying in a drying tower filled with solid particle silica gel to remove residual moisture, distilling at normal pressure, and collecting the distillate at the temperature of 58-64 ℃ as a finished product. The production process is carried out in a fully sealed state, the catalyst is recycled, and the fraction after the finished product is obtained can be recycled.
Although these methods have better process, higher yield and less equipment corrosion than the method using concentrated sulfuric acid as catalyst, the catalyst is expensive, has the problem of catalyst treatment, and needs to be filtered and dried.
(3) Patent EP1070702 discloses a preparation method of ethyl trifluoroacetate, which uses trifluoroacetyl chloride and absolute ethyl alcohol as main raw materials, and ethyl trifluoroacetate as a solvent to prepare ethyl trifluoroacetate; patent US4916256 discloses a method for preparing ethyl trifluoroacetate by using trifluoroacetyl chloride and anhydrous ethanol as main raw materials, and reacting ethanol and trifluoroacetyl chloride into gas to prepare ethyl trifluoroacetate; patent EP1070702 discloses a preparation method of ethyl trifluoroacetate, which uses trifluoroacetyl chloride and absolute ethyl alcohol as main raw materials, uses an acid solution of onium salt as a catalyst to prepare ethyl trifluoroacetate, and layers reaction products to obtain a crude product; the technological processes are complex, the ethanol is not easy to react completely, the post-treatment is complex, and the continuous production cannot be realized.
In the existing process for preparing ethyl trifluoroacetate: the method takes the reaction of trifluoroacetic acid and ethanol to prepare ethyl trifluoroacetate as a mainstream process, although the process is simple and easy to operate, acidic substances such as concentrated sulfuric acid, strong-acid cation exchange resin, p-toluene sulfonic acid and the like are required to be used as catalysts, so that the problems of high catalyst price, large waste catalyst amount and difficulty in treatment exist, equipment is easy to corrode seriously, and the requirement on the equipment is high; in the process of preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride with ethanol, although an acid catalyst is not used, the amount of three wastes can be reduced, ethanol needs to be converted into gas and then reacts, the reaction energy consumption is high, simultaneously, the ethanol cannot be completely reacted, an azeotrope can be formed by the ethanol and the ethyl trifluoroacetate, the product is not easy to purify, the processes of washing to remove the ethanol and drying are also needed, a large amount of wastewater is generated again, a new environment-friendly problem is formed, and continuous production cannot be carried out.
Therefore, there is a need for further improvement of the process for the preparation of ethyl trifluoroacetate.
Disclosure of Invention
The invention aims to provide a method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride with ethanol, so that the ethanol can completely react in the reaction process, the product purification problem is reduced, and the process can be continuously produced.
The synthetic process route of the invention is as follows:
the invention provides the following technical scheme:
a method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride with ethanol, which is carried out in a microchannel reactor, comprises the following steps of:
(1) enabling the raw material 1 to enter a preheating module 3, wherein the preheating temperature is 0-100 ℃, and the raw material 1 comprises absolute ethyl alcohol;
(2) enabling the raw material 1 and the raw material 2 preheated in the step (1) to enter a microchannel reaction module 4, wherein the raw material 2 comprises trifluoroacetyl chloride, the raw material 2 and the raw material 1 are mixed and reacted in the microchannel reaction module, the molar ratio of the raw material 2 to the raw material 1 is 1.5: 1-1.0: 1, the flow of the raw material 1 is 0.1-10 g/min, the reaction temperature is 0-100 ℃, and the reaction pressure is 0-1.0 MPa;
(3) and (3) after a compound obtained at the outlet of the microchannel reaction module 9 in the step (2) passes through a quenching module 10, obtaining a product of ethyl trifluoroacetate.
The trifluoroacetyl chloride and ethanol provided by the invention are reacted to continuously prepare ethyl trifluoroacetate, and modules of the microchannel reactor are assembled before preparation to obtain the microchannel reactor. By way of example, a pre-heat module 3, six microchannel reaction modules 4-9, and a quench module 10 may be mounted in series as shown in FIG. 3, wherein: the liquid phase pump 1 connected with the preheating module 3 is used as a feed inlet of the raw material 1; the 1 connected with the micro-channel reaction module 4 is a gas mass flowmeter which is used as a feed inlet of a raw material 2.
After the microchannel reactor is connected, heat conduction oil can be used for heat transfer. In the continuous reaction process of preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride and ethanol, the number of microchannel reaction modules can be increased or decreased according to needs, and 2 or more than 2 microchannel reaction modules can be selected to participate in the reaction according to needs.
In the method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride with ethanol, the preferable mode is that the mass transfer coefficient of the microchannel reactor is 1-30 Ka, and the heat exchange capacity is 1700KW/m2K or more.
In the method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride with ethanol, the microchannel reactor is a corning G2 microreactor, a micropore array microchannel reactor, a fin type microchannel reactor, a capillary microchannel reactor or a multi-strand parallel flow microreactor as a preferable mode.
In the method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride and ethanol, provided by the invention, the micro-channel structure in the reaction module of the micro-channel reactor comprises a direct-current channel structure and an enhanced mixed channel structure. Preferably, the straight-flow channel structure is a tubular structure, the reinforced mixed channel structure is a T-shaped structure, a spherical baffle structure, a water-drop structure or a heart-shaped structure, and the diameter of the channel is 0.5 mm-10 mm.
According to the method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride with ethanol, the material of the microchannel reaction module is selected from silicon carbide, a Hash alloy or a manganese-Nael alloy.
In the method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride with ethanol, the raw material 1 needs to be preheated before entering the preheating module 3, and the preheating temperature is 0-100 ℃. Preferably, the preheating temperature is 20-80 ℃.
In the method for continuously preparing the ethyl trifluoroacetate by reacting the trifluoroacetyl chloride with the ethanol, the molar ratio of the raw material 1 to the raw material 2 meets the requirement of smoothly carrying out the reaction. In a preferred embodiment, the molar ratio of the raw material 2 to the raw material 1 is 1.5:1 to 1.0: 1. More preferably, the molar ratio of the raw material 2 to the raw material 1 is 1.2:1 to 1.05: 1.
In the method for continuously preparing the ethyl trifluoroacetate by reacting the trifluoroacetyl chloride with the ethanol, the flow of the raw material 2 is enough to ensure that the reaction is smoothly carried out. As a preferable mode, the flow rate of the raw material 1 is 0.1-10 g/min.
In the method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride with ethanol, the reaction temperature in the step (2) is 0-100 ℃. As a preferable mode, the reaction temperature is 20-80 ℃.
In the method for continuously preparing the ethyl trifluoroacetate by reacting the trifluoroacetyl chloride with the ethanol, the reaction pressure in the step (2) is 0-1.0 MPa. In a preferred embodiment, the reaction pressure is 0 to 0.5 MPa.
Compared with the prior art, the method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride with ethanol has the advantages of high conversion rate, short reaction time, safe and controllable reaction, easy purification of products and continuous industrial amplification.
Drawings
FIG. 1 is a diagram of a typical structural unit of a microchannel reactor module used in the present invention;
FIG. 2 is a block diagram illustrating a Corning microchannel reactor according to the present invention;
FIG. 3 is a diagram of a microchannel reactor system apparatus, as an example of a Corning microchannel module, according to the present invention, and FIG. 3: the device comprises a liquid phase pump (raw material 1 feed port), a gas mass flowmeter (raw material 2 feed port) 1, a preheating module 3, microchannel reaction modules 4-9 and a quenching module 10.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the invention to these embodiments. It will be appreciated by those skilled in the art that the present invention encompasses all alternatives, modifications and equivalents as may be included within the scope of the claims.
Example 1
The method selects a corning straight channel module 1 block (as a premixing preheating module 3), a corning heart-shaped micro-channel reaction module 6 block and the corning straight channel module 1 block (as a quenching module 10) in the attached figure 2. A continuous flow microchannel reaction system was constructed according to the reaction scheme shown in FIG. 3. The reaction heat exchange medium adopts heat conducting oil. According to the principle of forced heat transfer of the microchannel reactor, only two temperature measuring points are arranged at the feed inlet and the discharge outlet of the reactor. Before the reaction, the microchannel reaction system and the connecting pipeline are respectively subjected to dehydration and drying treatment, and 1.0MPa air tightness inspection is carried out. The raw material ethanol is continuously and stably added into the micro-channel reaction system through a liquid phase pump 1 (such as a diaphragm metering pump) in the attached figure 3. Trifluoroacetyl chloride gas was continuously dosed into the microchannel reaction system by means of a gas mass flow meter 2 in figure 3.
The temperature of the heat exchanger is set to 55 ℃, namely the reaction temperature, and the reaction pressure is set to 0 MPa. The feed rate of raw material ethanol is 0.67g/min, the feed rate of trifluoroacetyl chloride gas is 2.12g/min, the reaction residence time is 25s, and the molar ratio of trifluoroacetyl chloride to ethanol is 1.1: 1. The reaction raw material enters a heart-shaped microchannel reaction module 4 after passing through a microchannel premixing and preheating module 3, the trifluoroacetyl chloride gas directly enters the heart-shaped microchannel reaction module 4 through a gas mass flowmeter, and trifluoroacetyl chloride and ethanol react in the heart-shaped microchannel reaction module 4-9. And collecting the reaction crude product after passing through a quenching module 10 to obtain a trifluoroacetic acid ethyl ester crude product.
GC analysis of the reaction mixture showed that the residual ethanol was 0 and the conversion of ethanol was 100%.
Example 2
The same corning microchannel reactor as in example 1 was used, and the same connection and control method were followed. This example varied the reaction conditions.
The temperature of the heat exchanger is set to be 60 ℃, namely the reaction temperature, and the reaction pressure is set to be 0 MPa. The feed rate of raw material ethanol 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 material enters a heart-shaped microchannel reaction module 4 after passing through a microchannel premixing and preheating module 3, the trifluoroacetyl chloride gas directly enters the heart-shaped microchannel reaction module 4 through a gas mass flowmeter, and trifluoroacetyl chloride and ethanol react in the heart-shaped microchannel reaction module 4-9. And collecting the reaction crude product after passing through a quenching module 10 to obtain a trifluoroacetic acid ethyl ester crude product.
GC analysis of the reaction mixture showed that the residual ethanol was 0 and the conversion of ethanol was 100%.
Example 3
The same corning microchannel reactor as in example 1 was used, and the same connection and control method were followed. This example varied the reaction conditions.
The temperature of the heat exchanger is set to 65 ℃, namely the reaction temperature, and the reaction pressure is set to 0 MPa. The raw material ethanol has the feeding speed of 1.68g/min, the feeding speed of trifluoroacetyl chloride gas is 5.31g/min, the reaction residence time is 10s, and the molar ratio of trifluoroacetyl chloride to ethanol is 1.1: 1. The reaction raw material enters a heart-shaped microchannel reaction module 4 after passing through a microchannel premixing and preheating module 3, the trifluoroacetyl chloride gas directly enters the heart-shaped microchannel reaction module 4 through a gas mass flowmeter, and trifluoroacetyl chloride and ethanol react in the heart-shaped microchannel reaction module 4-9. And collecting the reaction crude product after passing through a quenching module 10 to obtain a trifluoroacetic acid ethyl ester crude product.
GC analysis of the reaction mixture showed that the residual ethanol was 0 and the conversion of ethanol was 100%.
Example 4
The same corning microchannel reactor as in example 1 was used, and the same connection and control method were followed. This example varied the reaction conditions.
The temperature of the heat exchanger is set to 80 ℃, namely the reaction temperature, and the reaction pressure is set to 0 MPa. The feed rate of raw material ethanol 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 material enters a heart-shaped microchannel reaction module 4 after passing through a microchannel premixing and preheating module 3, the trifluoroacetyl chloride gas directly enters the heart-shaped microchannel reaction module 4 through a gas mass flowmeter, and trifluoroacetyl chloride and ethanol react in the heart-shaped microchannel reaction module 4-9. And collecting the reaction crude product after passing through a quenching module 10 to obtain a trifluoroacetic acid ethyl ester crude product.
GC analysis of the reaction mixture showed that the residual ethanol was 0 and the conversion of ethanol was 100%.
Example 5
The same corning microchannel reactor as in example 1 was used, and the same connection and control method were followed. This example varied the reaction conditions.
The temperature of the heat exchanger is set to 50 ℃, namely the reaction temperature, and the reaction pressure is set to 0 MPa. The feed rate of raw material ethanol is 0.56g/min, the feed rate of trifluoroacetyl chloride gas is 1.77g/min, the residence time of the reaction is 30s, and the molar ratio of trifluoroacetyl chloride to ethanol is 1.1: 1. The reaction raw material enters a heart-shaped microchannel reaction module 4 after passing through a microchannel premixing and preheating module 3, the trifluoroacetyl chloride gas directly enters the heart-shaped microchannel reaction module 4 through a gas mass flowmeter, and trifluoroacetyl chloride and ethanol react in the heart-shaped microchannel reaction module 4-9. And collecting the reaction crude product after passing through a quenching module 10 to obtain a trifluoroacetic acid ethyl ester crude product.
GC analysis of the reaction mixture showed that the residual ethanol was 0 and the conversion of ethanol was 100%.
Example 6
The same corning microchannel reactor as in example 1 was used, and the same connection and control method were followed. This example varied the reaction conditions.
The temperature of the heat exchanger is set to 30 ℃, namely the reaction temperature, and the reaction pressure is set to 0.1 MPa. The feed rate of raw material ethanol is 0.26g/min, the feed rate of trifluoroacetyl chloride gas is 0.89g/min, the residence time of the reaction is 30s, and the molar ratio of trifluoroacetyl chloride to ethanol is 1.2: 1. The reaction raw material enters a heart-shaped microchannel reaction module 4 after passing through a microchannel premixing and preheating module 3, the trifluoroacetyl chloride gas directly enters the heart-shaped microchannel reaction module 4 through a gas mass flowmeter, and trifluoroacetyl chloride and ethanol react in the heart-shaped microchannel reaction module 4-9. And collecting the reaction crude product after passing through a quenching module 10 to obtain a trifluoroacetic acid ethyl ester crude product.
GC analysis of the reaction mixture showed that the residual ethanol was 0 and the conversion of ethanol was 100%.
Example 7
The same corning microchannel reactor as in example 1 was used, and the same connection and control method were followed. This example varied the reaction conditions.
The temperature of the heat exchanger is set to 40 ℃, namely the reaction temperature, and the reaction pressure is set to 0.1 MPa. The feed rate of raw material ethanol is 0.32g/min, the feed rate of trifluoroacetyl chloride gas is 1.06g/min, the residence time of the reaction is 25s, and the molar ratio of trifluoroacetyl chloride to ethanol is 1.15: 1. The reaction raw material enters a heart-shaped microchannel reaction module 4 after passing through a microchannel premixing and preheating module 3, the trifluoroacetyl chloride gas directly enters the heart-shaped microchannel reaction module 4 through a gas mass flowmeter, and trifluoroacetyl chloride and ethanol react in the heart-shaped microchannel reaction module 4-9. And collecting the reaction crude product after passing through a quenching module 10 to obtain a trifluoroacetic acid ethyl ester crude product.
GC analysis of the reaction mixture showed that the residual ethanol was 0 and the conversion of ethanol was 100%.
Example 8
The same corning microchannel reactor as in example 1 was used, and the same connection and control method were followed. This example varied the reaction conditions.
The temperature of the heat exchanger is set to 70 ℃, namely the reaction temperature, and the reaction pressure is set to 0.1 MPa. The feed rate of raw material ethanol is 0.59g/min, the feed rate of trifluoroacetyl chloride gas is 1.77g/min, the residence time of the reaction is 15s, and the molar ratio of trifluoroacetyl chloride to ethanol is 1.05: 1. The reaction raw material enters a heart-shaped microchannel reaction module 4 after passing through a microchannel premixing and preheating module 3, the trifluoroacetyl chloride gas directly enters the heart-shaped microchannel reaction module 4 through a gas mass flowmeter, and trifluoroacetyl chloride and ethanol react in the heart-shaped microchannel reaction module 4-9. And collecting the reaction crude product after passing through a quenching module 10 to obtain a trifluoroacetic acid ethyl ester crude product.
GC analysis of the reaction mixture showed that the residual ethanol was 0 and the conversion of ethanol was 100%.
Claims (6)
1. A method for continuously preparing ethyl trifluoroacetate by reacting trifluoroacetyl chloride with ethanol is characterized in that the method is carried out in a microchannel reactor and comprises the following steps:
(1) enabling the raw material 1 to enter a preheating module 3, wherein the preheating temperature is 0-100 ℃, and the raw material 1 comprises absolute ethyl alcohol;
(2) enabling the raw material 1 and the raw material 2 preheated in the step (1) to enter a microchannel reaction module 4, wherein the raw material 2 comprises trifluoroacetyl chloride, the raw material 2 and the raw material 1 are mixed and reacted in the microchannel reaction module, the molar ratio of the raw material 2 to the raw material 1 is 1.5: 1-1.0: 1, the flow of the raw material 1 is 0.1-10 g/min, the reaction temperature is 0-100 ℃, and the reaction pressure is 0-1.0 MPa; the microchannel reactor is a module 4-module 9, the material of the microchannel reactor is selected from silicon carbide, Ha C alloy or Mn-Neel alloy, the mass transfer coefficient of the microchannel reactor is 1-30 Ka, and the heat exchange capacity is 1700KW/m2 & K or more; the raw material 2 and the raw material 1 are mixed and reacted in two or more microchannel reaction modules;
(3) after a compound obtained at the outlet of the microchannel reaction module 9 passes through a quenching module 10, a product ethyl trifluoroacetate is obtained; the preheating module 3, the six micro-channel reaction modules 4-9 and the quenching module 10 are installed in series.
2. The method for continuously preparing the ethyl trifluoroacetate by reacting the trifluoroacetyl chloride and the ethanol according to claim 1, wherein the molar ratio of the raw material 2 to the raw material 1 is 1.2: 1-1.05: 1, and the preheating temperature in the step (1) is 20-80 ℃.
3. The method for continuously preparing the ethyl trifluoroacetate by reacting the trifluoroacetyl chloride with the ethanol according to claim 2, wherein the reaction temperature in the step (2) is 20-80 ℃.
4. The method for continuously preparing the ethyl trifluoroacetate by reacting the trifluoroacetyl chloride and the ethanol according to claim 1, wherein the reaction pressure in the step (2) is 0-0.5 MPa.
5. The continuous process for the preparation of ethyl trifluoroacetate by reaction of trifluoroacetyl chloride with ethanol as claimed in claim 1, wherein: the reaction module of the microchannel reactor is characterized in that a microchannel structure inside the reaction module comprises a direct-flow type channel structure and an enhanced mixed type channel structure, the direct-flow type channel structure is a tubular structure, the enhanced mixed type channel structure is a T-shaped structure, a spherical baffle plate structure, a water-drop-shaped structure or a heart-shaped structure, and the diameter of a channel is 0.5-10 mm.
6. The continuous process for the preparation of ethyl trifluoroacetate by reaction of trifluoroacetyl chloride with ethanol as claimed in claim 1, wherein: the microchannel reactor is a corning G2 microreactor, a micropore array microchannel reactor, a fin type microchannel reactor, a capillary microchannel reactor or a multi-strand parallel-flow microreactor.
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| US6278015B1 (en) * | 1999-07-21 | 2001-08-21 | Rohm And Haas Company | Process for trifluoroacetate esters and thioesters |
| CN101128257A (en) * | 2004-11-12 | 2008-02-20 | 万罗赛斯公司 | Process using microchannel technology for conducting alkylation or acylation reaction |
| 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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| US6278015B1 (en) * | 1999-07-21 | 2001-08-21 | Rohm And Haas Company | Process for trifluoroacetate esters and thioesters |
| CN101128257A (en) * | 2004-11-12 | 2008-02-20 | 万罗赛斯公司 | Process using microchannel technology for conducting alkylation or acylation reaction |
| 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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Denomination of invention: A method for continuous production of ethyl trifluoroacetate Effective date of registration: 20220628 Granted publication date: 20220419 Pledgee: Industrial and Commercial Bank of China Limited Hangzhou Zhaohui sub branch Pledgor: SINOCHEM LANTIAN Co.,Ltd. Registration number: Y2022330001143 |
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