Tetramethylsilane high-efficiency adsorption and purification small-scale experiment device

Abstract

The utility model provides a tetramethylsilane high-efficiency adsorption and purification small-scale experiment device which is characterized in that one opening of a three-neck flask is communicated with a vertically arranged adsorption column, the adsorption column is filled with an adsorbent, the top of the adsorption column is communicated with a vertically arranged cooling pipe through a concave pipe, an adding sleeve on the outer wall of the adsorption column is communicated with a heating circulation box, and the heating circulation box is communicated with a heating circulation box; the cooling sleeve on the outer wall of the adsorption column is communicated with the cooling circulation box. The whole experiment system is transparent glass, so that the dynamic process in the system can be clearly observed, and the unreliable experiment result caused by flow back-mixing and material flow flowing abnormity can be obviously prevented. After the experiment parameters are adjusted, the system response time is short, the adjustment experiment can be quickly carried out, and the overall experiment failure caused by faults is avoided. The small-scale test experimental device can efficiently screen adsorbents and determine experimental conditions required by various pilot tests, and after industrial-grade tetramethylsilane (94%) is adsorbed through the device, the purity of the industrial-grade tetramethylsilane can reach 99.999%.

Description

Technical Field

[0001] The utility model relates to the field of chemical experiments, in particular to a small-scale experimental device for efficient adsorption and purification of tetramethylsilane. Background Technique

[0002] Electronic-grade tetramethylsilane belongs to an important emerging chemical vapor deposition precursor material in the electronics industry. In the field of ultra-large-scale integrated circuits, it is one of the important precursors for atomic layer deposition (ALD) and chemical vapor deposition (CVD) to prepare low-dielectric-constant thin films, mainly used as an etching barrier layer and a copper barrier layer. At present, the electronics industry is developing rapidly. As a raw material, the market demand for electronic-grade tetramethylsilane continues to grow. However, the output of tetramethylsilane above the electronic grade in China is insufficient, and electronic-grade tetramethylsilane seriously relies on the overseas market.

[0003] To meet the demand for the localization of the source of electronic-grade high-purity silicon precursors, a rigorous purification scheme needs to be formulated. Through theoretical analysis and experimental verification, it is found that the adsorption process has very excellent effects on the purification of tetramethylsilane, which can solve the difficulties of the existence of azeotropes in the raw materials and their extremely low boiling points and easy volatility. Further, we propose a high-efficiency small-scale experimental device specifically for the adsorption and purification of tetramethylsilane. Content of the Utility Model

[0004] The main purpose of the utility model is to provide a small-scale experimental device for efficient adsorption and purification of tetramethylsilane, so as to solve the difficulties of the existence of azeotropes in the purified raw materials and the low overall boiling point and easy volatility in the above background technique. It has the advantages of rapid discharging, easy debugging, process temperature, not easy to interfere, etc., effectively reducing the cost of expenses and time and saving human resources.

[0005] To solve the above technical problems, the technical solution adopted by the utility model is: a small-scale experimental device for efficient adsorption and purification of tetramethylsilane, one opening of a three-necked flask is communicated with a vertically arranged adsorption column, the inside of the adsorption column is filled with an adsorbent, the top of the adsorption column is communicated with a vertically arranged cooling pipe through a concave pipe, the adding sleeve on the outer wall of the adsorption column is communicated with a heating circulation tank, and the cooling sleeve on the outer wall of the adsorption column is communicated with a cooling circulation tank.

[0006] In a preferred scheme, the three-necked flask is arranged inside a water bath, and the water bath is arranged on a heating table.

[0007] In a preferred scheme, the adsorption column is a straight condenser, the lower end of the adding sleeve on the outer wall of the adsorption column is communicated with the water outlet of the heating circulation tank, and the water inlet of the heating circulation tank is communicated with the upper end of the adding sleeve on the outer wall of the adsorption column.

[0008] In a preferred scheme, the adsorption column is a 30-40 cm straight condenser.

[0009] In the preferred embodiment, the water temperature heated by the heating circulation tank is 25 - 35 °C.

[0010] In the preferred embodiment, the weight of the adsorbent inside the adsorption column is 80 - 90 grams.

[0011] In the preferred embodiment, the cooling pipe is a 30 - 40 cm straight condenser pipe. The lower end of the cooling jacket on the outer wall of the cooling pipe is connected to the water outlet of the cooling circulation tank, and the upper end of the cooling jacket on the outer wall of the cooling pipe is connected to the water inlet of the cooling circulation tank.

[0012] In the preferred embodiment, the lower end of the cooling pipe is connected to the liquid receiving pipe, and the aperture of the discharging end of the liquid receiving head at the end of the liquid receiving pipe is 0.4 - 0.6 cm.

[0013] In the preferred embodiment, the coolant in the cooling circulation tank is ethylene glycol, and its temperature is controlled at -7 °C to -4 °C.

[0014] In the preferred embodiment, one of the openings of the three-necked flask is also provided with an air extraction head, and the middle opening is provided with a thermometer.

[0015] In the preferred embodiment, the interfaces of the cooling pipe, the adsorption column and the concave pipe are wrapped with sealing film.

[0016] The present utility model provides a small-scale experimental device for efficient adsorption and purification of tetramethylsilane. Compared with the prior art, the beneficial effects of the present utility model are as follows: A small-scale device for efficient adsorption and purification of preparing electronic-grade tetramethylsilane has the following advantages:

[0017] (1) The entire experimental system is made of glass and transparent, and the dynamic process inside the system can be clearly observed, which can significantly prevent backmixing of the flow stream and abnormal flow of the material flow, resulting in unreliable experimental results. After the experimental parameters are adjusted, the response time of the system is short, and the experiment can be quickly adjusted to avoid overall experimental failure caused by small mistakes.

[0018] (2) The adsorption column and the cooling pipe are connected by a concave pipe with self-designed dimensions instead of a cow horn pipe, which can ensure that both the adsorption column and the cooling pipe are in the vertical direction, effectively avoiding a large amount of material accumulation at the cow horn pipe, avoiding material backmixing and untimely discharging, and effectively improving the accuracy of the experimental results.

[0019] (3) The entire system is provided with a purging device, that is, a gas source is installed in the three-necked flask. At the end of the experiment, all the gas-phase materials can be blown into the cooling pipe for condensation and collection, so as to prevent diffusion to the outside and affect the experimental personnel and the environment; and the device joints use sealing film instead of vaseline oil, which can effectively avoid blockage of the pore diameter of the adsorbent and contamination of organic substances. Description of the Drawings

[0020] The following further describes the present utility model in conjunction with the drawings and embodiments:

[0021] Figure 1 It is a front view structural schematic diagram of the present utility model.

[0022] In the figure: three-necked flask 1; air extraction head 2; adsorption column 3; concave tube 4; cooling tube 5; liquid receiving tube 6; water bath 7; heating table 8; heating circulation box 9; cooling circulation box 10; thermometer 11. Specific embodiments

[0023] Example 1

[0024] As Figure 1 shown, a small-scale experimental device for high-efficient adsorption and purification of tetramethylsilane, one of the openings of the three-necked flask 1 is communicated with the vertically arranged adsorption column 3, the inside of the adsorption column 3 is filled with an adsorbent, the top of the adsorption column 3 is communicated with the vertically arranged cooling tube 5 through the concave tube 4, the addition sleeve on the outer wall of the adsorption column 3 is communicated with the heating circulation box 9, and the cooling sleeve on the outer wall of the adsorption column 3 is communicated with the cooling circulation box 10.

[0025] The three-necked flask 1 is a round-bottomed flask with a capacity of 50 ml. The right opening of the three-necked flask 2 is connected to the adsorption column 3. The adsorption column 3 is a straight condensation tube with a length of 30 cm. The interlayer of the adsorption column needs to be connected to the heating circulation box 9 to keep the adsorption column at 30 °C and the inner tube can be filled with 90 g of the specified adsorbent. The top of the adsorption column 3 is connected to the concave tube 4. The size of the concave tube 4 is 5 cm in horizontal length and 6 cm in vertical length at both ends. This size can just ensure that the adsorbed gas-phase material can smoothly enter the cooling tube without condensation.

[0026] The size of the concave tube needs to be determined according to the properties of the material. If it is too long, material backmixing is likely to occur. If it is too short, the connection will fail. Through testing and calculation, the concave tube is 5 cm in horizontal length and 6 cm in vertical length at both ends. This size can just ensure that the adsorbed gas-phase material can smoothly enter the cooling tube without condensation. If a cow horn tube is used instead of the concave tube, serious liquid accumulation and backmixing will occur, resulting in failure of material separation.

[0027] The other end of the concave tube is connected to the condensation tube 5. The condensation tube 5 is a straight condensation tube with a length of 30 cm.

[0028] In a preferred scheme, the three-necked flask 1 is arranged inside the water bath 7, and the water bath 7 is arranged on the heating table 8. The volume of the three-necked flask is 50 ml, and it needs to be heated in a 35 °C water bath to ensure that the temperature inside the flask is maintained at 32 °C.

[0029] In a preferred scheme, the adsorption column 3 is a straight condensation tube. The lower end of the addition sleeve on the outer wall of the adsorption column 3 is communicated with the water outlet of the heating circulation box 9, and the water inlet of the heating circulation box 9 is communicated with the upper end of the addition sleeve on the outer wall of the adsorption column 3.

[0030] In the preferred embodiment, the adsorption column 3 is a 30-40 cm straight condenser tube.

[0031] In the preferred embodiment, the water temperature heated by the heating circulation tank 9 is 25-35 °C. The heating medium of the heating circulation tank is pure water, and its temperature is controlled at 35 °C, or 30 °C.

[0032] In the preferred embodiment, the weight of the adsorbent inside the adsorption column 3 is 80-90 grams. The lower end of the adsorption column should be blocked with absorbent cotton to prevent the adsorbent from falling off.

[0033] In the preferred embodiment, the cooling tube 5 is a 30-40 cm straight condenser tube. The lower end of the cooling jacket on the outer wall of the cooling tube 5 is connected to the water outlet of the cooling circulation tank 10, and the upper end of the cooling jacket on the outer wall of the cooling tube 5 is connected to the water inlet of the cooling circulation tank 10.

[0034] In the preferred embodiment, the lower end of the cooling tube 5 is connected to the liquid receiving tube 6. The aperture of the discharging end of the liquid receiving head of the liquid receiving tube 6 is 0.4-0.6 cm. An aperture of 0.4 cm at the discharging end of the liquid receiving head can effectively reduce the volatilization of the material.

[0035] In the preferred embodiment, the coolant of the cooling circulation tank 10 is ethylene glycol, and its temperature is controlled at -7 °C to -4 °C. The coolant of the cooling circulation tank is ethylene glycol, and its temperature is controlled at -7 °C.

[0036] In the preferred embodiment, one of the openings of the three-necked flask 1 is also provided with an air extraction head 2, and the middle opening is provided with a thermometer 11. A thermometer is connected to the left side opening of the three-necked flask to observe the material in the flask in time to control the volatilization rate. The middle opening of the three-necked flask 1 is connected to the air extraction head 2, and the air extraction head 2 is connected to a nitrogen source to blow the gaseous material to the condenser tube for collection in time at the end of the experiment.

[0037] In the preferred embodiment, the interfaces of the cooling tube 5, the adsorption column 3 and the concave tube 4 are wrapped with sealing film. Since the overall material is extremely volatile, the airtightness of the overall system should be ensured. Therefore, the interfaces of equipment such as the three-necked flask, the adsorption column, the concave tube, and the condenser tube should be wrapped with sealing film, and vaseline oil cannot be used because vaseline oil will affect the adsorption effect of the adsorbent.

[0038] Example 2

[0039] Further described in combination with Example 1, as Figure 1For the shown structure, when in use, the heating circulation tank 9 should be started for heating and the cooling circulation tank 9 should be started for circulating the cooling medium. After connecting the device and wrapping appropriate sealing film around each interface, the material to be adsorbed and purified is added into the three-necked flask 1. Then, start heating the adsorption column and the three-necked flask 1. Note that the cooling liquid should be introduced into the interlayer of the cooling pipe 5 in advance, so as to ensure that the material in the adsorption column is in the gas phase and can be quickly liquefied when the material reaches the condenser, avoiding loss and improving the experimental accuracy. After the experiment, stop the water bath heating and heating circulation, start a nitrogen source with a certain flow rate to ensure that nitrogen can smoothly enter the three-necked flask 1, and completely discharge the internal gas-phase material into the cooling pipe 5 for cooling and collection and recycling treatment.

[0040] This utility model has a simple structure, a small volume, is convenient for experimental personnel to operate, can be used without being in a closed environment state, is less interfered by environmental factors for its system, has a short experimental period, and saves experimental costs.

[0041] Specifically, the entire experimental system is made of glass and transparent, and the dynamic process inside the system can be clearly observed, which can significantly prevent backmixing of the flow stream and abnormal flow of the material flow, resulting in unreliable experimental results. After the experimental parameters are adjusted, the system response time is short, and the experiment can be quickly adjusted to avoid overall experimental failure caused by small mistakes.

[0042] Specifically, the adsorption column 3 and the cooling pipe 5 are connected by a concave pipe 4 with self-designed dimensions instead of a cow horn pipe, so as to ensure that both the adsorption column and the cooling pipe are in the vertical direction, effectively avoiding a large amount of material accumulation at the cow horn pipe, avoiding material backmixing and untimely discharging, and effectively improving the accuracy of the experimental results.

[0043] Specifically, a purging device is set in the entire system, that is, a gas source is installed in the three-necked flask 1, and at the end of the experiment, all the gas-phase materials can be blown into the cooling pipe for condensation and collection, so as to avoid diffusion to the outside and affecting the experimental personnel and the environment; and the joints of the device use sealing film instead of vaseline oil, which can effectively avoid blockage of the pore diameter of the adsorbent and pollution of organic substances.

[0044] Working principle:

[0045] This system is designed according to the properties of the materials to be experimented, which also includes the application of the basic adsorption theory.

[0046] First, the material vaporizes at a certain rate under the heating state, and the gas-phase material sequentially enters the adsorption column heated to a certain temperature to achieve gas-phase adsorption. After the adsorption is completed, the impurities enter the condenser for condensation and collection. After the experiment, the residual material can be collected and processed through nitrogen purging.

[0047] The design of the adsorption device can ensure the tightness and stability of the system. The adsorbed materials can be quickly condensed and collected separately, and the materials at different times will not be back-mixed, ensuring the accuracy of sampling. In addition, the parameter setting and pipeline layout of the heating, cooling, and water bath devices play a crucial role in the heat preservation of the adsorption column and the condenser tube. The design of the specific dimensions of the concave tube plays an important role in the normal connection of the adsorption column and the cooling tube. It can not only quickly condense the gaseous materials but also prevent the back-mixing of the materials, avoiding the influence on the experimental results and further improving the experimental accuracy.

[0048] The above embodiments are only the preferred technical solutions of the present invention and should not be regarded as limitations to the present invention. The protection scope of the present invention should be the technical solutions recorded in the claims, including the equivalent replacement solutions of the technical features in the technical solutions recorded in the claims. That is, the equivalent replacement improvements within this scope are also within the protection scope of the present invention.

Claims

1. A small-scale experimental device for efficient adsorption and purification of tetramethylsilane, characterized in that: One opening of the three-necked flask (1) is connected to a vertically arranged adsorption column (3), the interior of the adsorption column (3) is filled with an adsorbent, the top of the adsorption column (3) is connected to a vertically arranged cooling pipe (5) through a concave tube (4), the addition jacket on the outer wall of the adsorption column (3) is connected to a heating circulation box (9), and the cooling jacket on the outer wall of the adsorption column (3) is connected to a cooling circulation box (10).

2. According to claim 1, a small-scale experimental device for efficient adsorption and purification of tetramethylsilane is characterized in that: The three-necked flask (1) is arranged inside a water bath (7), and the water bath (7) is arranged on a heating platform (8).

3. According to claim 1, a small-scale experimental device for efficient adsorption and purification of tetramethylsilane is characterized in that: The adsorption column (3) is a straight condenser tube. The lower end of the outer wall of the adsorption column (3) is connected to the water outlet of the heating circulation box (9). The water inlet of the heating circulation box (9) is connected to the upper end of the outer wall of the adsorption column (3) and the water inlet of the heating circulation box (9).

4. According to claim 3, a small-scale experimental device for efficient adsorption and purification of tetramethylsilane is characterized in that: The adsorption column (3) is a 30-40 cm straight condenser tube; The water temperature heated by the heating circulation box (9) is 25-35°C.

5. According to claim 1, a small-scale experimental device for efficient adsorption and purification of tetramethylsilane is characterized in that: The weight of the adsorbent inside the adsorption column (3) is 80-90 grams.

6. A small-scale experimental device for efficient adsorption and purification of tetramethylsilane according to claim 1, characterized in that: The cooling pipe (5) is a 30-40 cm straight condenser pipe. The lower end of the cooling jacket on the outer wall of the cooling pipe (5) is connected to the water outlet of the cooling circulation box (10), and the upper end of the cooling jacket on the outer wall of the cooling pipe (5) is connected to the water inlet of the cooling circulation box (10).

7. A small-scale experimental device for efficient adsorption and purification of tetramethylsilane according to claim 6, characterized in that: The lower end of the cooling pipe (5) is connected to the liquid receiving pipe (6), and the aperture of the liquid receiving head at the end of the liquid receiving pipe (6) is 0.4-0.6 cm.

8. A small-scale experimental device for efficient adsorption and purification of tetramethylsilane according to claim 6, characterized in that: The cooling liquid of the cooling circulation box (10) is ethylene glycol, and its temperature is controlled at -7°C to -4°C.

9. A small-scale experimental device for efficient adsorption and purification of tetramethylsilane according to claim 1, characterized in that: One of the openings of the three-necked flask (1) is also provided with a vacuum head (2), and the middle opening is provided with a thermometer (11).

10. A small-scale experimental device for efficient adsorption and purification of tetramethylsilane according to claim 1, characterized in that: The interfaces of the cooling tube (5), the adsorption column (3) and the concave tube (4) are wrapped with sealing films.

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