Device and method for preparing electronic grade triethyl borate

Abstract

The invention belongs to the field of chemical product purification, and particularly relates to a preparation device and method of electronic grade triethyl borate. The method specifically comprises the following steps: S1, adding ethanol and boric acid into a reactor for reaction to obtain a product, enabling the product to enter a product collecting tank, then enabling the product to enter a product separating tower from the product collecting tank to separate ethanol in the product to obtain a crude product triethyl borate, and enabling the ethanol to enter an ethanol recycling tank for recycling; and S2, dehydrating the crude product triethyl borate in the step S1, feeding the dehydrated crude product triethyl borate into a crude product collecting tank, feeding the dehydrated crude product triethyl borate into a light component removal tower to remove light components, feeding the dehydrated crude product triethyl borate into a heavy component removal tower to remove heavy components, and feeding electronic-grade triethyl borate into a product tank. Raw materials react to prepare a crude product, the crude product is collected and then introduced into a separation tower, ethanol is dehydrated and recycled at the top, and a triethyl borate crude product at the bottom is also dehydrated. After the crude product is subjected to primary filtration, impurities are removed through a light component removal tower and a heavy component removal tower to obtain a high-purity product, and after the product is subjected to secondary fine filtration, the electronic-grade high-purity standard is achieved, and the high-end application requirement is met.

Description

Technical Field

[0001] The present application belongs to the field of chemical product purification, and specifically relates to a device and method for preparing electronic-grade triethyl borate. Background Art

[0002] Triethyl borate, also known as ethyl borate, triethoxyborane, or TEB for short, has low toxicity and volatility. It is a colorless, transparent liquid that is miscible with ethanol and ether and easily decomposes into alcohol and boric acid when in contact with water. Currently, the main production method of triethyl borate is to synthesize it using ethanol and boric acid as raw materials.

[0003] According to different uses, it can be divided into industrial-grade triethyl borate and electronic-grade triethyl borate. Industrial-grade triethyl borate can be used as a solvent, catalyst, preservative, lubricant, plasticizer, plasticizer, cosolvent, etc. It is a widely used organic compound. Electronic-grade triethyl borate is mainly used in the deposition process of wafer manufacturing to form borophosphosilicate glass (BPSG). Borophosphosilicate glass is silicon dioxide doped with boron and phosphorus. It is an insulating medium, mainly used for insulating layers between layers before multi-layer metal wiring, reflow dielectric layers, surface passivation protective layers, etc. It is an important material required for the thin film deposition process of semiconductor chip front-end manufacturing.

[0004] A Chinese patent with announcement number CN116036633B discloses an environmentally friendly and energy-saving preparation method and supporting equipment for electronic-grade triethyl borate. The patent uses a specially prepared molecular sieve membrane to physically filter the substance to be separated, and then achieves the purpose of purification. However, the separation membrane preparation process in this method is complicated and involves multiple substances, which not only prolongs the entire reaction cycle, but also may introduce some impurities that are difficult to separate.

[0005] With the continuous development of the domestic semiconductor industry, the demand for electronic-grade TEB continues to increase, but most domestic companies currently remain at the industrial level, and the current purification process of triethyl borate is imperfect, and the purity of the product is difficult to meet market demand. Therefore, there is an urgent need for a device and method for preparing electronic-grade triethyl borate with high efficiency, stable quality, and high product purity to meet market demand. Summary of the invention

[0006] In view of the fact that most companies in the prior art remain at the industrial level, and the current purification process of triethyl borate is imperfect, and the purity of the product is difficult to meet market demand, the present application provides a device and method for preparing electronic grade triethyl borate.

[0007] The technical solution of this application:

[0008] On the one hand, the present application provides a preparation device for electronic grade triethyl borate, comprising a reactor, a product collecting tank, a product separation tower, a crude product dehydration tower, a crude product collecting tank, a light removal tower, a heavy removal tower and a product tank connected in sequence;

[0009] The side wall of the reactor is provided with a reaction raw material inlet, and the bottom of the reactor is provided with a product outlet, the product outlet of the reactor is connected to the side wall of the product collecting tank, the bottom of the product collecting tank is connected to the middle part of the product separation tower, the bottom of the reaction tower is connected to the bottom of the crude product dehydration tower, the top of the crude product dehydration tower is connected to the top of the crude product collecting tank, the bottom of the crude product collecting tank is connected to the middle part of the light-removing tower, the bottom of the light-removing tower is connected to the middle part of the heavy-removing tower, and the top of the heavy-removing tower is connected to the top of the product tank.

[0010] Preferably, the top of the product separation tower is also connected to the bottom of the ethanol dehydration tower, the top of the ethanol dehydration tower is also connected to the top of the ethanol recovery tank, and the bottom of the ethanol recovery tank is connected to the reaction raw material inlet of the reactor; the interior of the ethanol dehydration tower is filled with adsorption material, and the adsorption material includes zeolite molecular sieve, phosphorus pentoxide and calcium chloride.

[0011] Preferably, a primary filter is provided on the pipelines of the crude product collection tank and the light removal tower, and a secondary filter is provided on the pipeline connected to the bottom of the product tank; both the primary filter and the secondary filter are high-density polyethylene filters with a pore size of 0.1 to 2 μm.

[0012] Preferably, a stirring mechanism is provided inside the reactor, the stirring mechanism comprises a stirring shaft and stirring blades, and the stirring shaft is driven by a motor provided outside the reactor.

[0013] Preferably, a light component outlet is provided at the top of the light-removing tower, and a heavy component outlet is provided at the bottom of the heavy-removing tower.

[0014] Preferably, the interior of the crude product dehydration tower is filled with adsorption materials, and the adsorption materials include zeolite molecular sieve, phosphorus pentoxide and calcium chloride; the light removal tower, heavy removal tower and product tank are all electrolytically polished or lined with PFA material.

[0015] On the other hand, the present application provides a method for preparing electronic grade triethyl borate, comprising the following steps:

[0016] Step S1. adding ethanol and boric acid into a reactor to obtain a product which enters a product collection tank, and then enters a product separation tower from the product collection tank to separate ethanol from the product to obtain crude triethyl borate, and the ethanol enters an ethanol recovery tank for recycling;

[0017] Step S2. After the crude triethyl borate in step S1 is dehydrated, it enters a crude product collection tank, then enters a light-removing tower to remove light components, and then enters a heavy-removing tower to remove heavy components. The electronic-grade triethyl borate enters a product tank.

[0018] Preferably, in step S1, boric acid and ethanol are both industrial pure, boric acid is ground into powder before use, the molar ratio of boric acid to ethanol is 1:(1-3), the operating temperature of the reactor is 80-90°C, and the reaction time is 4-5h; the operating temperature of the product collection tank is 10-30°C; the top operating temperature of the product separation tower is 60-90°C, the operating pressure is 0.1-0.2MPa, and the reflux ratio is 5-10; the operating temperature of the ethanol recovery tank is 10-30°C.

[0019] Preferably, in step S2, the operating temperatures of the crude product collection tank and the product tank are both 10-30°C; the top operating temperature of the light removal tower is 70-90°C, the operating pressure is 0.1-0.2 MPa, and the reflux ratio is 5-10; the operating temperature of the heavy removal tower is 110-130°C, the operating pressure is 0.1-0.2 MPa, and the reflux ratio is 5-10.

[0020] Beneficial effects of this application:

[0021] (1) The present application first adds the purchased raw materials into the reactor for chemical reaction to obtain a preliminary crude product. Subsequently, these crude products are collected in a product collection tank. Next, the collected crude products are passed into a product separation tower for preliminary separation treatment. At the top of the product separation tower, ethanol is dehydrated to remove the water therein, and the treated ethanol is finally collected in an ethanol recovery tank. At the same time, the crude triethyl borate at the bottom of the product separation tower is also dehydrated, and the crude triethyl borate after dehydration is collected in a crude product collection tank. Next, the crude triethyl borate passes through a primary filter to remove most of the particulate impurities therein. After the primary filtration, it is passed into a light and heavy tower, during which impurity components such as ethanol and water are removed, thereby obtaining a high-purity product. Finally, these high-purity products enter the product tank and are further finely filtered through a secondary filter to ensure that the final triethyl borate product reaches the high purity standard of the electronic grade and meets the needs of high-end application fields.

[0022] (2) During the reaction stage, the boric acid needs to be fully ground. In this way, the particles of boric acid will become finer, thereby increasing its surface area in contact with the solvent. Ethanol is used as a solvent for the dissolution operation. The conversion rate of the product is significantly improved. By fully grinding the boric acid and dissolving it in ethanol, the reaction can be more effectively promoted, ultimately obtaining a higher product yield and better product quality.

[0023] (3) In the initial product separation stage, ethanol raw material is extracted from the top of the product separation tower, and the ethanol is dehydrated and can be used as raw material and returned to the reactor for recycling, thereby saving costs and improving economic efficiency.

[0024] (4) Before light and heavy removal, a crude dehydration tower is used to remove water from the crude triethyl borate, which not only controls the water content of the crude triethyl borate, but also prevents the triethyl borate from being hydrolyzed by water to produce other impurities.

[0025] (5) The optimized distillation operating temperature and pressure range, as well as the reasonable reflux ratio setting, not only improve the purification efficiency, but also effectively reduce energy consumption, making the production process more economical and efficient.

[0026] (6) Using two-stage filtration in the lightness removal tower and before filling can more effectively control the particulate impurities in the product and ensure that the particulate matter index is stable and meets the standard. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Attached Figure 1 A schematic diagram of a device for preparing electronic grade triethyl borate for this application;

[0028] Figure symbols: 1. Reactor; 2. Product collecting tank; 3. Product separation tower; 4. Ethanol dehydration tower; 5. Ethanol recovery tank; 6. Crude product dehydration tower; 7. Crude product collecting tank; 8. Primary filter; 9. Light removal tower; 10. Heavy removal tower; 11. Product tank; 12. Secondary filter. DETAILED DESCRIPTION

[0029] In order to further explain the technical means and effects adopted by the present application to achieve the predetermined invention purpose, the specific implementation method, structure, characteristics and effects of the present application are described in detail below in combination with the preferred embodiments.

[0030] Device Embodiment

[0031] See also Figure 1 This embodiment provides a device for preparing electronic grade triethyl borate, comprising a reactor 1, a product collecting tank 2, a product separation tower 3, a crude product dehydration tower 6, a crude product collecting tank 7, a light removal tower 9, a heavy removal tower 10 and a product tank 11 which are connected in sequence;

[0032] The side wall of the reactor 1 is provided with a reaction raw material inlet, and the bottom of the reactor 1 is provided with a product outlet. The product outlet of the reactor 1 is connected to the side wall of the product collecting tank 2, the bottom of the reactor 1 is connected to the middle part of the product separation tower 3, the bottom of the reaction tower is connected to the bottom of the crude product dehydration tower 6, the top of the crude product dehydration tower 6 is connected to the top of the crude product collecting tank 7, the bottom of the crude product collecting tank 7 is connected to the middle part of the light removal tower 9, the bottom of the light removal tower 9 is connected to the middle part of the heavy removal tower 10, and the top of the heavy removal tower 10 is connected to the top of the product tank 11.

[0033] In the embodiment of the present equipment, a reaction raw material inlet is provided on the side wall of the reactor 1, and the boric acid and ethanol treated in advance are introduced into the reactor 1 through the reaction raw material inlet. A heating jacket is also provided on the outer wall of the reactor 1 for heating the reactor 1. The heating medium in the heating jacket can be water or other materials that can be used as a heating medium.

[0034] In the embodiment of the present device, a product outlet is provided at the bottom of the reactor 1, and the product outlet of the reactor 1 is connected to the side wall of the product collecting tank 2. The substances generated by the reaction enter the product collecting tank 2 through the product outlet at the bottom of the reactor 1 through a pipeline. A stirring mechanism is provided inside the reactor 1 for stirring the reaction raw materials so that the reactants are fully contacted for reaction. The stirring mechanism includes a stirring shaft and stirring blades, and the stirring shaft is driven by a motor provided outside the reactor 1.

[0035] In the embodiment of the present equipment, the bottom of the product collecting tank 2 is connected to the middle of the product separation tower 3, the reaction product enters the product separation tower 3 from the product collecting tank 2, ethanol is extracted from the top of the product separation tower 3, and other components are extracted from the bottom of the product separation tower 3. The condenser of the product separation tower 3 uses 7°C water as a cooling medium, and the reboiler uses 160°C heat transfer oil as a heat medium. The condenser uses cooling water at a lower temperature to effectively reduce the condensation temperature and improve the refrigeration efficiency; while the reboiler uses heat transfer oil as a heat medium, which has the advantages of relatively low pressure, easier temperature control, and coal consumption saving, and can ensure the stable operation and efficient separation of the product separation tower 3.

[0036] Ethanol returns to the reactor 1 through the ethanol recovery path to continue to participate in the reaction as a reaction raw material. Specifically, ethanol enters from the bottom of the ethanol dehydration tower 4 through a pipeline, and the water in the ethanol is removed by the adsorbent in the ethanol dehydration tower 4. The adsorbent can be made of zeolite molecular sieve, phosphorus pentoxide, calcium chloride and other materials. The ethanol after the water is removed enters the ethanol recovery tank 5 for storage through the top of the ethanol dehydration tower 4. As needed, the ethanol in the ethanol recovery tank 5 enters the reactor 1 through the pipeline at the bottom of the ethanol recovery tank 5. The ethanol entering the reactor 1 can be achieved by pressure difference or by a liquid delivery pump.

[0037] The other components extracted from the bottom of the product separation tower 3 enter the bottom of the crude dehydration tower 6 through the pipeline, and the water in the crude triethyl borate is removed by the adsorbent in the crude dehydration tower 6. The adsorbent can be made of zeolite molecular sieve, phosphorus pentoxide, calcium chloride and other materials. The crude triethyl borate after dehydration enters the crude collection tank 7 through the top of the crude dehydration tower 6. The crude product flows out from the bottom of the crude collection tank 7, enters the light removal tower 9 through the primary filter 8, and light components such as water and ethanol are extracted from the light component outlet at the top of the light removal tower 9. Other components flow into the de-weighting tower 10 along the bottom pipeline of the de-weighting tower 9, and the heavy components are extracted from the heavy component outlet at the bottom of the de-weighting tower 10. The fine triethyl borate enters the product tank 11 from the top of the de-weighting tower 10 along the pipeline for storage. The bottom pipeline of the product tank 11 is provided with a secondary filter 12, and the solid particles are further removed through the secondary filter 12 to ensure the purity and stability of the product. Among them, the primary filter 8 and the secondary filter 12 are both made of high-density polyethylene material, and their pore sizes are precisely controlled within the range of 0.1 to 2 μm, which can effectively block tiny particles and ensure that the triethyl borate has a high degree of purity and safety after filtration. At the same time, the high-density polyethylene material also gives the filter good chemical corrosion resistance and mechanical strength, extending its service life and improving the reliability and economy of the overall filtration system.

[0038] In the embodiment of the present equipment, the light removal tower 9, the heavy removal tower 10 and the product tank 11 are electropolished or lined with PFA material, which can ensure that the metal ion index is qualified. It can significantly improve the surface finish and corrosion resistance of the equipment, enhance stability and durability, and meet the high requirements of modern industry for environmental protection, safety and efficient operation.

[0039] In the present equipment embodiment, the condensers of the light removal tower 9 and the heavy removal tower 10 use 7° C. water as the cooling medium, and the reboilers use 160° C. heat transfer oil as the heat medium.

[0040] Example 1

[0041] Based on the device provided in the equipment embodiment, this embodiment provides a method for preparing electronic grade triethyl borate, which is as follows:

[0042] Step S1. Using purchased industrial-grade boric acid and ethanol as raw materials, grind the boric acid into powder, dissolve it in an ethanol solution, and introduce it into a reactor 1 at a molar ratio of 1:3. The temperature of the reactor 1 is 85°C. The reaction is carried out for 4.5 hours. The obtained product enters a product collecting tank 2. The operating temperature of the product collecting tank 2 is 15°C. Subsequently, the product enters a product separation tower 3 from the product collecting tank 2 to separate the ethanol in the product to obtain crude triethyl borate. The operating temperature of the top of the product separation tower 3 is 68°C, the operating pressure is 0.15MPa, and the reflux ratio is 7. The ethanol is extracted from the top of the product separation tower 3 and enters an ethanol recovery tank 5 for recycling. The operating temperature of the ethanol recovery tank 5 is 15°C.

[0043] Step S2. The crude triethyl borate is taken out from the bottom of the product separation tower 3, passed into the crude dehydration tower 6 for dehydration, and collected into the crude recovery tank at an operating temperature of 15° C., and passed into the primary filter 8 to remove particulate impurities in the material itself and residual particles of the adsorbent. Subsequently, the product enters the light-removing tower 9, the top temperature of the light-removing tower 9 is 85°C, the top pressure is 0.13MPa, and the reflux ratio is 8. Light components such as ethanol and water are extracted from the top of the light-removing tower 9, and other components enter the heavy-removing tower 10 through a pipeline from the bottom of the light-removing tower 9. The top temperature of the heavy-removing tower 10 is 130°C, the top pressure is 0.12MPa, and the reflux ratio is 7. Heavy components and most of the metal ions are removed, and high-purity triethyl borate is extracted from the top of the heavy-removing tower 10 and enters the product tank 11. The operating temperature of the product tank 11 is 20°C. The bottom of the product tank 11 is connected to the secondary filter 12, and electronic grade triethyl borate is filtered again and filled through the filling pipeline.

[0044] Example 2

[0045] Based on the device provided in the equipment embodiment, this embodiment provides a method for preparing electronic grade triethyl borate, which is as follows:

[0046] Step S1. Using purchased industrial-grade boric acid and ethanol as raw materials, grind the boric acid into powder, dissolve it in an ethanol solution, and introduce it into a reactor 1 at a molar ratio of 1:2. The temperature of the reactor 1 is 80°C. The reaction is carried out for 5 hours. The obtained product enters a product collecting tank 2. The operating temperature of the product collecting tank 2 is 30°C. Subsequently, the product enters a product separation tower 3 from the product collecting tank 2 to separate the ethanol in the product to obtain crude triethyl borate. The operating temperature of the top of the product separation tower 3 is 60°C, the operating pressure is 0.1MPa, and the reflux ratio is 5. The ethanol is extracted from the top of the product separation tower 3 and enters an ethanol recovery tank 5 for recycling. The operating temperature of the ethanol recovery tank 5 is 10°C.

[0047] Step S2. The crude triethyl borate is extracted from the bottom of the product separation tower 3, passed into the crude dehydration tower 6, dehydrated, and collected into the crude product recovery tank, the operating temperature is 30°C, passed into the primary filter 8, and the particulate impurities of the material itself and the residual particles of the adsorbent are removed. The product then enters the light removal tower 9, the tower top temperature of the light removal tower 9 is 70°C, the tower top pressure is 0.2MPa, the reflux ratio is 10, and the light components such as ethanol and water are extracted from the tower top of the light removal tower 9, and the other components enter the deweighting tower 10, the tower top temperature of the deweighting tower 10 is 110°C, the tower top pressure is 0.19MPa, the reflux ratio is 10, and the heavy components and most of the metal ions are removed. High-purity triethyl borate is extracted from the tower top of the deweighting tower 10, and enters the product tank 11, the operating temperature of the product tank 11 is 10°C, and the bottom of the product tank 11 is connected to the secondary filter 12, and the electronic grade triethyl borate is filtered again, and filled through the filling pipeline.

[0048] Example 3

[0049] Based on the device provided in the equipment embodiment, this embodiment provides a method for preparing electronic grade triethyl borate, which is as follows:

[0050] Step S1. Using purchased industrial-grade boric acid and ethanol as raw materials, grind the boric acid into powder, dissolve it in an ethanol solution, and introduce it into a reactor 1 at a molar ratio of 1:1. The temperature of the reactor 1 is 90°C. The reaction is carried out for 4 hours. The obtained product enters a product collecting tank 2. The operating temperature of the product collecting tank 2 is 10°C. Subsequently, the product enters a product separation tower 3 from the product collecting tank 2 to separate the ethanol in the product to obtain crude triethyl borate. The operating temperature of the top of the product separation tower 3 is 90°C, the operating pressure is 0.2MPa, and the reflux ratio is 5. The ethanol is extracted from the top of the product separation tower 3 and enters an ethanol recovery tank 5 for recycling. The operating temperature of the ethanol recovery tank 5 is 30°C.

[0051] Step S2. The crude triethyl borate is extracted from the bottom of the product separation tower 3, passed into the crude dehydration tower 6, dehydrated, and collected into the crude product recovery tank, the operating temperature is 10°C, passed into the primary filter 8, and the particulate impurities of the material itself and the residual particles of the adsorbent are removed. The product then enters the light removal tower 9, the top temperature of the light removal tower 9 is 90°C, the top pressure is 0.15MPa, the reflux ratio is 5, and the light components such as ethanol and water are extracted from the top of the light removal tower 9, and the other components enter the deweighting tower 10, the top temperature of the deweighting tower 10 is 130°C, the top pressure is 0.1MPa, the reflux ratio is 5, and the heavy components and most of the metal ions are removed. High-purity triethyl borate is extracted from the top of the deweighting tower 10 and enters the product tank 11. The operating temperature of the product tank 11 is 30°C, and the bottom of the product tank 11 enters the secondary filter 12, and is filtered again to obtain electronic grade triethyl borate, which is filled through the filling pipeline.

[0052] After testing and analysis, under the process conditions of the present application, in Examples 1 to 3, the purity of electronic grade triethyl borate is not less than 99.99%, the moisture content is not higher than 20 ppm, the metal ion impurities meet the 8.5N purity, and the particle index (≥0.2 μm) is not higher than 10 p / ml.

[0053] The above is only a preferred embodiment of the present application and does not constitute any form of limitation to the present application. Although the present application has been disclosed as a preferred embodiment as above, it is not intended to limit the present application. Any technical personnel in this field can make some changes or modify the technical contents disclosed above into equivalent embodiments without departing from the scope of the technical solution of the present application. However, any modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present application without departing from the content of the technical solution of the present application are still within the scope of the technical solution of the present application.

Claims

1. A preparation device for electronic grade triethyl borate, characterized in that, It comprises a reactor (1), a product collecting tank (2), a product separation tower (3), a crude product dehydration tower (6), a crude product collecting tank (7), a light-removal tower (9), a heavy-removal tower (10) and a product tank (11) which are connected in sequence; The side wall of the reactor (1) is provided with a reaction raw material inlet, and the bottom of the reactor (1) is provided with a product outlet. The product outlet of the reactor (1) is in communication with the side wall of the product collecting tank (2), the bottom of the product collecting tank (2) is in communication with the middle of the product separation tower (3), the bottom of the reaction tower is in communication with the bottom of the crude product dehydration tower (6), the top of the crude product dehydration tower (6) is in communication with the top of the crude product collecting tank (7), the bottom of the crude product collecting tank (7) is in communication with the middle of the light-removal tower (9), the bottom of the light-removal tower (9) is in communication with the middle of the heavy-removal tower (10), and the top of the heavy-removal tower (10) is in communication with the top of the product tank (11).

2. A preparation device for electronic grade triethyl borate according to claim 1, characterized in that, The top of the product separation tower (3) is also connected to the bottom of the ethanol dehydration tower (4), and the top of the ethanol dehydration tower (4) is also connected to the top of the ethanol recovery tank (5), and the bottom of the ethanol recovery tank (5) is connected to the reaction raw material inlet of the reactor (1); the interior of the ethanol dehydration tower (4) is filled with adsorption material, and the adsorption material includes zeolite molecular sieve, phosphorus pentoxide and calcium chloride.

3. A preparation device for electronic grade triethyl borate according to claim 1, characterized in that, A primary filter (8) is provided on the pipelines of the crude product collection tank (7) and the light removal tower (9), and a secondary filter (12) is provided on the pipeline connected to the bottom of the product tank (11); both the primary filter (8) and the secondary filter (12) are high-density polyethylene filters with a pore size of 0.1 to 2 μm.

4. A preparation device for electronic grade triethyl borate according to claim 1, characterized in that, A stirring mechanism is provided inside the reactor (1), wherein the stirring mechanism comprises a stirring shaft and stirring blades, and the stirring shaft is driven by a motor provided outside the reactor (1).

5. A preparation device for electronic grade triethyl borate according to claim 1, characterized in that, The top of the light component removal tower (9) is provided with a light component outlet, and the bottom of the heavy component removal tower (10) is provided with a heavy component outlet.

6. A preparation device for electronic grade triethyl borate according to claim 1, characterized in that, The interior of the crude product dehydration tower (6) is filled with adsorption materials, and the adsorption materials include zeolite molecular sieve, phosphorus pentoxide and calcium chloride; the light removal tower (9), heavy removal tower (10) and product tank (11) are all electrolytically polished or lined with PFA material.

7. A method for preparing electronic grade triethyl borate, based on the device for preparing electronic grade triethyl borate according to any one of claims 1 to 6, characterized in that: The steps include: Step S1. adding ethanol and boric acid into a reactor (1) to obtain a product for reaction, and the product enters a product collecting tank (2). The product then enters a product separation tower (3) from the product collecting tank (2) to separate ethanol from the product to obtain crude triethyl borate. The ethanol enters an ethanol recovery tank (5) for recycling; Step S2. After the crude triethyl borate in step S1 is dehydrated, it enters the crude product collection tank (7), then enters the light component removal tower (9) to remove the light components, and then enters the heavy component removal tower (10) to remove the heavy components. The electronic grade triethyl borate enters the product tank (11).

8. A method for preparing electronic grade triethyl borate according to claim 7, characterized in that, In the step S1, both boric acid and ethanol are industrial pure, the boric acid is ground into powder before use, the molar ratio of boric acid to ethanol is 1:(1-3), the operating temperature of the reactor (1) is 80-90°C, and the reaction time is 4-5h; the operating temperature of the product collecting tank (2) is 10-30°C; the operating temperature of the top of the product separation tower (3) is 60-90°C, the operating pressure is 0.1-0.2MPa, and the reflux ratio is 5-10; the operating temperature of the ethanol recovery tank (5) is 10-30°C.

9. A method for preparing electronic grade triethyl borate according to claim 7, characterized in that, In the step S2, the operating temperatures of the crude product collecting tank (7) and the product tank (11) are both 10-30°C; the top operating temperature of the light removal tower (9) is 70-90°C, the operating pressure is 0.1-0.2 MPa, and the reflux ratio is 5-10; the operating temperature of the heavy removal tower (10) is 110-130°C, the operating pressure is 0.1-0.2 MPa, and the reflux ratio is 5-10.

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