Purification device of tris (trimethylsilane) phosphate

Abstract

The utility model discloses a purification device of tris (trimethylsilane) phosphate, which comprises a rectifying tower, and a feeding end is arranged on one side of a tower kettle of the rectifying tower and is used for feeding crude tris (trimethylsilane) phosphate; a gas phase output end is arranged at the tower top of the rectifying tower and is connected with the condenser; one path of the output end of the condenser is connected with a separation ratio controller, one path of the output end of the separation ratio controller is connected to one side of the tower top of the rectifying tower, and the other path is used as a top extraction output end; a nitrogen purging end is arranged on a connecting pipeline between the output end of the separation ratio controller and the top mining output end; the device disclosed by the utility model realizes a reliable purification effect on a TMSP crude product, obtains a TMSP product with higher purity, and is particularly suitable for being used as a TMSP purification experimental device.

Description

Technical Field

[0001] The utility model belongs to the field of battery electrolyte preparation, and particularly relates to a purification device for tris(trimethylsilyl)phosphate. Background Art

[0002] Tris(trimethylsilyl)phosphate (abbreviated as "TMSP", molecular formula C9H 27 O4PSi3) is an important organosilicon compound. In recent years, it has been widely used in the field of battery electrolytes. Adding it to the electrolyte can not only passivate the positive electrode and form a stable electrolyte interface layer, but also participate in the formation of SEI at the negative electrode, inhibiting the self-discharge of the battery to a certain extent, effectively improving the low-temperature performance and room-temperature cycle performance of the battery, and also enhancing the high-temperature performance, inhibiting the increase of battery resistance and the decrease of capacity, greatly improving the performance of lithium-ion batteries.

[0003] As market demand continues to increase, the requirements for TMSP production and quality are also increasing. However, due to the active chemical properties of silane compounds, they are unstable in humid air and easily decompose when exposed to water. Therefore, it is very necessary to develop an effective and stable purification device. Summary of the Invention

[0004] In view of this, the purpose of the present invention is to provide a purification device for tris(trimethylsilyl)phosphate, which can achieve a reliable purification effect on crude TMSP and obtain a TMSP product with higher purity, and is particularly suitable as a purification experimental device for TMSP.

[0005] The technical solutions adopted in this utility model are as follows:

[0006] A purification device for tris(trimethylsilyl)phosphate comprises a distillation tower, wherein:

[0007] A feed end is provided on one side of the bottom of the distillation tower for feeding the crude tris(trimethylsilyl)phosphate;

[0008] The top of the distillation tower is provided with a gas phase output end, which is connected to a condenser; the output end of the condenser is connected to a separation ratio controller on one side, and the output end of the separation ratio controller is connected to one side of the top of the distillation tower on one side, and the other end is used as a top extraction output end;

[0009] A nitrogen purge end is provided on the connecting pipeline between the output end of the separation ratio controller and the top extraction output end.

[0010] Preferably, a heater electrically connected to an external power source is provided at the bottom of the reactor of the distillation tower.

[0011] Preferably, a first switch valve connected to a control module is provided on the connecting pipeline between the feed end and the bottom feed port of the distillation tower.

[0012] Preferably, another output end of the condenser is connected to a vacuum pumping end for adjusting the pressure in the tower.

[0013] Preferably, a second switch valve connected to the control module is provided on the connecting pipeline between the output end and the vacuum end of the condenser.

[0014] Preferably, a third switch valve connected to the control module is provided on the connecting pipeline between the separation ratio controller and the top extraction output end.

[0015] Preferably, a fourth switch valve connected to the control module is provided on the connecting pipeline between the third switch valve and the nitrogen purge end.

[0016] Preferably, the crude tris(trimethylsilyl)phosphate is obtained by reacting hexamethyldisilazane and ammonium dihydrogen phosphate, and mainly contains hexamethyldisilazane and hexamethyldisiloxane as impurities.

[0017] Preferably, the distillation tower comprises a cylindrical tower body, and fillers are arranged in the tower body; wherein the outer diameter of the tower body is in the range of 90-110 mm, and the height of the tower body is in the range of 1.2-1.8 m.

[0018] Preferably, the filler is theta ring filler (θ filler).

[0019] The present application proposes a purification device for tris(trimethylsilyl)phosphate (TMSP), which is mainly composed of a distillation tower, a condenser, a separation ratio controller, and a nitrogen purge end. In a specific implementation, after the crude TMSP product is fed from the tower bottom under a nitrogen atmosphere, the nitrogen purge end is closed, the pressure in the tower is adjusted to a target pressure range, and the temperature in the tower is adjusted to a target temperature range, and the product is extracted from the top extraction output end. As the distillation and reaction in the distillation tower proceed, equilibrium is continuously established in the tower, so that the tower is in a relatively stable state, achieving a reliable purification effect of the crude TMSP product and obtaining a higher-purity TMSP product. The device is particularly suitable as a purification experimental device for TMSP and can provide new ideas for the preparation of TMSP. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a schematic structural diagram of a purification device for tris(trimethylsilyl)phosphate according to a specific embodiment of the present application. DETAILED DESCRIPTION

[0021] This embodiment provides a purification device for tris(trimethylsilyl)phosphate, comprising a distillation tower, wherein a feed end is provided on one side of the bottom of the distillation tower for feeding crude tris(trimethylsilyl)phosphate; a gas phase output end is provided at the top of the distillation tower, and the gas phase output end is connected to a condenser; one output end of the condenser is connected to a separation ratio controller, one output end of the separation ratio controller is connected to one side of the top of the distillation tower, and the other output end serves as a top sampling output end; a nitrogen purge end is provided on the connecting pipeline between the output end of the separation ratio controller and the top sampling output end.

[0022] In order to enable those skilled in the art to better understand the technical solutions of the present invention, the following will be combined with the drawings of the embodiments of the present invention to clearly and completely describe the technical solutions of the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts should fall within the scope of protection of the present invention.

[0023] See Figure 1 As shown, a tris(trimethylsilane)phosphate purification device includes a distillation tower T, wherein a feed end I is provided on one side of the bottom of the distillation tower T for feeding a crude tris(trimethylsilane)phosphate product. Specifically, in this embodiment, the crude tris(trimethylsilane)phosphate product is obtained by reacting hexamethyldisilazane and ammonium dihydrogen phosphate, and mainly contains hexamethyldisilazane and hexamethyldisiloxane as impurities. Preferably, in this embodiment, the distillation tower T includes a cylindrical tower body T1, in which a packing is provided. The outer diameter of the tower body T1 ranges from 90 to 110 mm, and the height of the tower body T1 ranges from 1.2 to 1.8 m. The packing is theta ring packing (θ packing).

[0024] In this embodiment, a gas phase output terminal is provided at the top of the distillation tower T, and the gas phase output terminal is connected to the condenser A; the output terminal of the condenser A is connected to the separation ratio controller B on one side, and the output terminal of the separation ratio controller B is connected to the top side T3 of the distillation tower T on one side, and the other side is used as the top sampling output terminal C1; a nitrogen purge terminal C2 is provided on the connecting pipeline between the output terminal of the separation ratio controller B and the top sampling output terminal C1;

[0025] Preferably, in order to adjust the feed flow rate, in this embodiment, a first switch valve D1 connected to the control module is provided on the connecting pipeline between the feed end I and the feed port of the bottom of the distillation tower T;

[0026] Preferably, in order to achieve the adjustment of the kettle temperature to the target temperature range, in this embodiment, a heater E electrically connected to an external power supply is provided at the bottom T2 of the kettle of the distillation tower T; preferably, in order to achieve the adjustment of the pressure in the tower to the target pressure range, in this embodiment, another output end of the condenser A is connected to the vacuum end C3 for adjusting the pressure in the tower;

[0027] Preferably, in order to achieve on-off control of the vacuum end C3, in this embodiment, a second on-off valve D2 connected to the control module is provided on the connecting pipeline between the output end of the condenser A and the vacuum end C3; preferably, in order to achieve on-off control of the top extraction output end C1, in this embodiment, a third on-off valve D3 connected to the control module is provided on the connecting pipeline between the separation ratio controller B and the top extraction output end C1; preferably, in order to achieve on-off control of the nitrogen purge end C2, in this embodiment, a fourth on-off valve D4 connected to the control module is provided on the connecting pipeline between the third on-off valve D3 and the nitrogen purge end C2.

[0028] In order to further illustrate the implementation process of this embodiment, based on the above implementation plan, this application further proposes the following specific implementation process:

[0029] The outer diameter of the distillation tower T is 100 mm and the height of the tower is 1.5 m;

[0030] After the crude TMSP product is fed from the bottom of the tower under a nitrogen atmosphere, the nitrogen purge end C2 is closed, and the vacuum end C3 is opened to adjust the pressure in the tower to the target pressure range of -90 kPa to -98 kPa. Then, the heater E (whose temperature is usually 130-140°C) is turned on to bring the bottom temperature to the target temperature range of 110-120°C (tower top temperature is: 95-105°C), and the product is withdrawn from the top sampling output end C1. As the distillation and reaction proceed in the distillation tower T, equilibrium is continuously established in the tower, making the tower in a relatively stable state, achieving a reliable purification effect of the crude TMSP product, obtaining a higher purity TMSP product and collecting it in a sample bottle. To achieve a more reliable and stable purification effect, sampling and analysis are carried out at regular intervals during the specific implementation, and nitrogen displacement is used during sampling to prevent water vapor from entering the sample bottle.

[0031] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the present invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the present invention is defined by the appended claims, not the foregoing description, and all variations within the meaning and range of equivalents of the claims are intended to be encompassed within the present invention. Any reference sign in a claim should not be construed as limiting the claim to which it relates.

[0032] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A purification device for tris(trimethylsilyl)phosphate, characterized in that, comprising a distillation column, wherein A feed end is provided on one side of the bottom of the distillation tower for feeding the crude tris(trimethylsilyl)phosphate; The top of the distillation tower is provided with a gas phase output end, which is connected to a condenser; the output end of the condenser is connected to a separation ratio controller on one side, and the output end of the separation ratio controller is connected to one side of the top of the distillation tower on one side, and the other end is used as a top extraction output end; A nitrogen purge end is provided on the connecting pipeline between the output end of the separation ratio controller and the top extraction output end.

2. The purification device for tris(trimethylsilyl)phosphate according to claim 1, characterized in that A heater electrically connected to an external power source is provided at the bottom of the reactor of the distillation tower.

3. The purification device for tris(trimethylsilyl)phosphate according to claim 1, characterized in that A first switch valve connected to a control module is provided on a connecting pipeline between the feed end and the feed port of the tower bottom of the distillation tower.

4. The purification device for tris(trimethylsilyl)phosphate according to claim 1, characterized in that Another output end of the condenser is connected to a vacuum pumping end.

5. The purification device for tris(trimethylsilyl)phosphate according to claim 4, characterized in that A second switch valve connected to the control module is provided on the connecting pipeline between the output end and the vacuum end of the condenser.

6. The purification device for tris(trimethylsilyl)phosphate according to claim 1, characterized in that A third switch valve connected to the control module is provided on the connecting pipeline between the separation ratio controller and the top extraction output end.

7. The purification device for tris(trimethylsilyl)phosphate according to claim 6, characterized in that A fourth switch valve connected to the control module is provided on the connecting pipeline between the third switch valve and the nitrogen purge end.

8. The purification device for tris(trimethylsilyl)phosphate according to claim 1, characterized in that: The crude tris(trimethylsilyl)phosphate is obtained by reacting hexamethyldisilazane and ammonium dihydrogen phosphate.

9. The purification device for tris(trimethylsilyl)phosphate according to claim 1, characterized in that The distillation tower includes a cylindrical tower body with fillers arranged inside the tower body; wherein the outer diameter of the tower body ranges from 90 to 110 mm, and the height of the tower body ranges from 1.2 to 1.8 m.

10. The purification device for tris(trimethylsilyl)phosphate according to claim 9, characterized in that: The packing is a theta ring packing.

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