Distillation equipment for preparing electronic-grade trifluoroacetic acid

Abstract

The invention relates to the technical field of chemical equipment, in particular to distillation equipment for preparing electronic-grade trifluoroacetic acid, which is characterized in that industrial-grade trifluoroacetic acid is used as a raw material, and the electronic-grade trifluoroacetic acid meeting the requirements of the semiconductor industry is produced in special distillation equipment in a normal-pressure sub-boiling distillation mode.

Description

Technical Field

[0001] This invention relates to the field of chemical equipment technology, and in particular to a distillation apparatus for preparing electronic-grade trifluoroacetic acid. Background Technology

[0002] Trifluoroacetic acid (2,2,2-trifluoroacetic acid) is an important fluorine-containing fine chemical, primarily used as a key raw material and intermediate in the synthesis of pesticides and pharmaceuticals. After purification and strict control of impurity ion content, it also has wide and crucial applications in the semiconductor and photovoltaic industries. Distillation / rectification is one of the core processes for preparing high-purity trifluoroacetic acid. Its core lies in using specialized equipment to heat and vaporize the raw material, separate the gas from the liquid, and purify and collect it, thereby removing harmful substances such as metal ions and particulate impurities from the raw material and ensuring that the product purity meets application requirements. Currently, the mainstream purification method in the industry is multi-stage series distillation, but this method has significant technical defects that restrict the preparation and application of ultra-high-purity trifluoroacetic acid.

[0003] Specifically, existing multi-stage series distillation methods involve high equipment investment costs, complex processes, and difficult operation. Furthermore, the entire distillation process consumes a great deal of energy, hindering cost control for large-scale production. More importantly, this method struggles to effectively remove metal ions and particulate impurities from the raw materials, resulting in limited product purity and failing to meet the stringent requirements of the semiconductor, photovoltaic, and other high-end electronics industries for ultra-high-purity wet electronic chemicals. In addition, existing distillation processes and equipment are prone to thermal decomposition of trifluoroacetic acid during heating, which not only reduces product yield but also affects product quality stability, further exacerbating the supply shortage of high-end electronic-grade trifluoroacetic acid. In addition to the aforementioned process-level defects, existing equipment for trifluoroacetic acid distillation / rectification also suffers from problems such as unreasonable structural design, poor purification effect, and insufficient anti-contamination capability. For example, the poor compatibility of heating and condensation structures in some equipment further exacerbates incomplete vaporization of raw materials, low condensation efficiency, and the risk of thermal decomposition. Some equipment lacks effective dust and contamination prevention structures, allowing external impurities to easily enter the equipment during distillation, which, combined with endogenous impurities that are difficult to remove by the process itself, results in the purity of electronic-grade trifluoroacetic acid products remaining at a bottleneck. At the same time, the existing equipment lacks convenient control over material conveying, gas emission, and collection, which is detrimental to process operation and stable operation.

[0004] In view of the many technical defects of the existing purification process and supporting equipment, there is an urgent need for a distillation device with a scientifically designed structure, convenient operation and low energy consumption for the preparation of electronic grade trifluoroacetic acid. This device would solve the core problems of existing technologies, such as difficulty in removing impurities, insufficient product purity, poor yield and quality stability, and meet the needs of the high-end electronics industry for the preparation of ultra-high purity trifluoroacetic acid. Summary of the Invention

[0005] The technical problem to be solved by this invention is to address the shortcomings of the prior art by providing a distillation apparatus for preparing electronic-grade trifluoroacetic acid. Addressing the current difficulties and complex processes in producing electronic-grade trifluoroacetic acid, this invention uses industrial-grade trifluoroacetic acid as raw material and employs a specially designed distillation and purification device to achieve the preparation of semiconductor-grade electronic-grade trifluoroacetic acid. It has advantages such as zero waste generation, low production cost, low equipment investment, simple operation, and easy industrial-scale production.

[0006] This invention provides a distillation apparatus for preparing electronic-grade trifluoroacetic acid, comprising:

[0007] Funnel-shaped material bottle;

[0008] The discharge pipe is connected at one end to the outlet end of the funnel-shaped material bottle;

[0009] The exhaust pipe has its peripheral sidewall connected to the other end of the discharge pipe;

[0010] A collection bottle is connected to one end of the exhaust pipe, and a valve is fixedly installed on the exhaust pipe at the position between the discharge pipe and the collection bottle.

[0011] According to the distillation apparatus for preparing electronic-grade trifluoroacetic acid provided by the present invention, an electric heating jacket is fitted on the outer peripheral wall of the lower half of the funnel-shaped material bottle, the upper half of the funnel-shaped material bottle has a double-wall structure, the inner layer is connected to the lower half of the funnel-shaped material bottle, a cooling water inlet is opened at the bottom of the outer layer, and a cooling water outlet is opened at the top of the outer layer, and the electric heating jacket is connected to an external power source.

[0012] According to the distillation apparatus for preparing electronic-grade trifluoroacetic acid provided by the present invention, one end of the discharge pipe is connected to the inner bottom sidewall of the upper half of the funnel-shaped material bottle.

[0013] According to the distillation apparatus for preparing electronic-grade trifluoroacetic acid provided by the present invention, the funnel-shaped material bottle has an open top and is detachably equipped with a dust cover.

[0014] According to the distillation apparatus for preparing electronic-grade trifluoroacetic acid provided by the present invention, a dust filter screen is provided at the end of the exhaust pipe away from the collection bottle.

[0015] Compared with the prior art, the present invention has the following advantages:

[0016] This invention provides a distillation apparatus for preparing electronic-grade trifluoroacetic acid. Using industrial-grade trifluoroacetic acid as raw material, electronic-grade trifluoroacetic acid that meets the requirements of the semiconductor industry is produced by atmospheric pressure sub-boiling distillation in a specially designed distillation apparatus.

[0017] This invention has the advantages of inexpensive and readily available raw materials, simple process, low equipment investment cost, no waste generation, easy operation, and easy industrial-scale production. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in this invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0019] Figure 1 A three-dimensional structural diagram of a distillation apparatus used to prepare electronic-grade trifluoroacetic acid;

[0020] Figure 2 This is a front view of the distillation apparatus used to prepare electronic-grade trifluoroacetic acid.

[0021] Figure label:

[0022] 1. Funnel-shaped material bottle; 101. Electric heating jacket; 102. Outer layer; 103. Inner layer; 104. Water inlet; 105. Water outlet; 106. Dust cover; 2. Discharge pipe; 3. Exhaust pipe; 301. Dust filter screen; 4. Collection bottle; 401. Valve. Detailed Implementation

[0023] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0024] In the description of the embodiments of the present invention, it should be noted that the terms "upper," "lower," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the embodiments of the present invention and simplifying the description, and do not indicate or imply that the mechanism or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the embodiments of the present invention. In addition, the terms "first," "second," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0025] In the description of the embodiments of the present invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "connected" and "linked" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in the embodiments of the present invention based on the specific circumstances.

[0026] In embodiments of the present invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature is in indirect contact with the second feature through an intermediate medium. Furthermore, "above," "on top of," and "over" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.

[0027] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0028] The following is combined Figures 1-2 The embodiment shown in this invention provides a distillation apparatus for preparing electronic-grade trifluoroacetic acid, comprising: a funnel-shaped material bottle 1; a discharge pipe 2, one end of which is connected to the outlet end of the funnel-shaped material bottle 1; an exhaust pipe 3, the sidewall of which is connected to the other end of the discharge pipe 2; and a collection bottle 4, which is connected to one end of the exhaust pipe 3. A valve 401 is fixedly installed on the exhaust pipe 3 at a position between the discharge pipe 2 and the collection bottle 4.

[0029] According to the distillation apparatus for preparing electronic-grade trifluoroacetic acid provided by the present invention, an electric heating sleeve 101 is fitted on the outer peripheral wall of the lower half of the funnel-shaped material bottle 1, the upper half of the funnel-shaped material bottle 1 has a double-wall structure, the inner layer 103 is connected to the lower half of the funnel-shaped material bottle 1, a cooling water inlet 104 is opened at the bottom of the outer layer 102, a cooling water outlet 105 is opened at the top of the outer layer 102, and the electric heating sleeve 101 is connected to an external power source.

[0030] According to the distillation apparatus for preparing electronic-grade trifluoroacetic acid provided by the present invention, one end of the discharge pipe 2 is connected to the bottom side wall of the inner layer 103 of the upper half of the funnel-shaped material bottle 1.

[0031] According to the distillation apparatus for preparing electronic-grade trifluoroacetic acid provided by the present invention, the funnel-shaped material bottle 1 has an open top and is detachably equipped with a dust cover 106.

[0032] According to the distillation apparatus for preparing electronic-grade trifluoroacetic acid provided by the present invention, a dust filter 301 is provided at the end of the exhaust pipe 3 away from the collection bottle 4.

[0033] This embodiment discloses a distillation apparatus for preparing electronic-grade trifluoroacetic acid, including a funnel-shaped material bottle 1, a discharge pipe 2, an exhaust pipe 3, and a collection bottle 4. All components are made of corrosion-resistant and high-purity materials to avoid introducing impurities into the materials themselves and to ensure the purity requirements for the preparation of electronic-grade trifluoroacetic acid.

[0034] The funnel-shaped material bottle 1 is used to hold industrial-grade trifluoroacetic acid raw material (purity of 99%) to be distilled. Its funnel-shaped structure design facilitates the accumulation of raw material in the bottle, and at the same time, it is conducive to the upward flow of gas after the raw material is heated and vaporized, thereby improving the gas-liquid separation efficiency.

[0035] An electric heating jacket 101 is fitted on the outer periphery of the lower half of the funnel-shaped material bottle 1. The electric heating jacket 101 is connected to an external power source. The heating power and heating temperature of the electric heating jacket 101 are controlled by the power source to achieve uniform heating of the raw material in the funnel-shaped material bottle 1, ensuring that the raw material can be stably vaporized. Moreover, the heating temperature can be precisely adjusted according to the requirements of the distillation process of trifluoroacetic acid to avoid local overheating that could lead to decomposition of the raw material or a decrease in purity.

[0036] The upper half of the funnel-shaped material bottle 1 has a double-walled structure, with its inner layer 103 connected to the lower half of the funnel-shaped material bottle 1. The diameter of the connection is slightly smaller than the inner diameter of the inner layer 103 of either the lower or upper half of the funnel-shaped material bottle 1, allowing the vaporized gas in the lower half to smoothly enter the space of the inner layer 103 in the upper half. The bottom of the outer layer 102 of the double-walled structure is provided with a cooling water inlet 104, and the top of the outer layer 102 is provided with a cooling water outlet 105. In use, cooling water enters the space of the outer layer 102 of the double-walled structure through the inlet 104 and flows out from the outlet 105, forming a cooling water circulation. This efficiently condenses the vaporized gas entering the space of the inner layer 103 in the upper half, rapidly cooling the vaporized gas, achieving gas-liquid separation, and improving the purification effect.

[0037] The funnel-shaped material bottle 1 has an open top and a detachable dust cover 106. When adding materials, the dust cover 106 can be opened to add the industrial-grade trifluoroacetic acid raw material to be distilled into the bottle. After adding materials, the dust cover 106 is closed, which effectively prevents external dust, impurities, etc. from entering the bottle and contaminating the raw material and distillation product. At the same time, the detachable design of the dust cover 106 facilitates the cleaning and maintenance of the inside of the funnel-shaped material bottle 1, ensuring the cleanliness of the equipment.

[0038] One end of the discharge pipe 2 is connected to the bottom side wall of the inner layer 103 of the upper half of the funnel-shaped material bottle 1, and is used to transport the condensed liquid material in the upper half of the funnel-shaped material bottle 1 to the exhaust pipe 3. The peripheral side wall of the exhaust pipe 3 is connected to the other end of the discharge pipe 2, so that the material transported by the discharge pipe 2 can enter the exhaust pipe 3, and the non-condensable gases generated during the distillation process can be discharged through the exhaust pipe 3. A dust filter 301 is provided at the end of the exhaust pipe 3 away from the collection bottle 4. The dust filter 301 is made of high-mesh filter material, which can not only ensure the smooth discharge of non-condensable gases, but also prevent external dust and other impurities from entering the equipment through the exhaust pipe 3, thus avoiding contamination of the distillation product.

[0039] The collecting bottle 4 is connected to one end of the exhaust pipe 3 and is used to collect the electronic-grade trifluoroacetic acid product after distillation and purification. A valve 401 is fixedly installed at the position of the exhaust pipe 3 between the discharge pipe 2 and the collecting bottle 4. The connection between the exhaust pipe 3 and the collecting bottle 4 can be controlled by the valve 401. At the beginning of distillation, the valve 401 can be closed. After the temperature and pressure inside the equipment are stable and the purity of the condensed material reaches the requirements, the valve 401 is opened to allow the purified material to enter the collecting bottle 4 for accurate collection. At the same time, it is easy to close the valve 401 after distillation to prevent the product in the collecting bottle 4 from being contaminated by the outside.

[0040] The operation process of the distillation equipment for preparing electronic-grade trifluoroacetic acid in this embodiment is as follows: First, open the dust cover 106 on the top of the funnel-shaped material bottle 1, add the industrial-grade trifluoroacetic acid raw material to be distilled into the funnel-shaped material bottle 1, and close the dust cover 106 after adding. Then, turn on the power of the electric heating jacket 101, adjust the heating power to heat the raw material in the lower half of the funnel-shaped material bottle 1, and at the same time, introduce cooling water into the space of the outer layer 102 of the double-layer tube wall in the upper half of the funnel-shaped material bottle 1 through the cooling water inlet 104. The cooling water flows out from the cooling water outlet 105 to form a circulation. During the heating process, the raw material is gradually heated... The gas gradually vaporizes and rises into the inner space 103 of the upper part of the funnel-shaped material bottle 1. Under the condensation of the cooling water, it is transformed into a liquid material. After the equipment is running stably and the purity of the condensed material meets the electronic grade requirements, the valve 401 on the exhaust pipe 3 is opened. The condensed material enters the exhaust pipe 3 through the discharge pipe 2 and then flows into the collection bottle 4, completing the distillation purification and collection of electronic grade trifluoroacetic acid. The non-condensable gas generated during the distillation process is discharged from the equipment through the dust filter 301 at the end of the exhaust pipe 3 away from the collection bottle 4. At the same time, the dust filter 301 effectively blocks external impurities from entering the equipment.

[0041] The distillation equipment used in this embodiment for preparing electronic-grade trifluoroacetic acid has a scientific and reasonable structural design. Through the integrated structural design of heating, condensation, separation and collection, it achieves efficient purification of industrial-grade trifluoroacetic acid. At the same time, through multiple anti-pollution structural designs, it effectively avoids the introduction of impurities, ensuring the purity of electronic-grade trifluoroacetic acid. Moreover, the equipment is easy to operate and runs stably, which can meet the needs of large-scale preparation of electronic-grade trifluoroacetic acid.

[0042] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention in any way. Any simple modifications, alterations, and equivalent changes made to the above embodiments based on the inventive essence shall still fall within the protection scope of the present invention.

Claims

1. A distillation apparatus for preparing electronic-grade trifluoroacetic acid, characterized in that, include: Funnel-shaped material bottle (1); The discharge pipe (2) is connected at one end to the outlet end of the funnel-shaped material bottle (1); The exhaust pipe (3) has its sidewall connected to the other end of the discharge pipe (2); The collection bottle (4) is connected to one end of the exhaust pipe (3), and a valve (401) is fixedly installed on the exhaust pipe (3) at the position between the discharge pipe (2) and the collection bottle (4).

2. The distillation apparatus for preparing electronic-grade trifluoroacetic acid according to claim 1, characterized in that, The lower half of the funnel-shaped material bottle (1) is fitted with an electric heating sleeve (101) on its outer peripheral side wall. The upper half of the funnel-shaped material bottle (1) has a double-wall structure. Its inner layer (103) is connected to the lower half of the funnel-shaped material bottle (1). The bottom of the outer layer (102) is provided with a cooling water inlet (104), and the top of the outer layer (102) is provided with a cooling water outlet (105). The electric heating sleeve (101) is connected to an external power source.

3. The distillation apparatus for preparing electronic-grade trifluoroacetic acid according to claim 2, characterized in that, One end of the discharge pipe (2) is connected to the bottom side wall of the inner layer (103) of the upper half of the funnel-shaped material bottle (1).

4. The distillation apparatus for preparing electronic-grade trifluoroacetic acid according to claim 2, characterized in that, The funnel-shaped material bottle (1) has an opening at the top and is detachably equipped with a dust cover (106).

5. The distillation apparatus for preparing electronic-grade trifluoroacetic acid according to claim 1, characterized in that, The exhaust pipe (3) is provided with a dust filter (301) at the end away from the collection bottle (4).

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