Chlorosilane pretreatment device

Abstract

The utility model relates to the technical field of polycrystalline silicon production, in particular to a chlorosilane pretreatment device which comprises a reaction kettle, a lining container and a tail gas absorption device, the reaction kettle comprises a reaction container and an end cover; the upper end of the reaction container is provided with an opening; the end cover can be detachably locked at the opening of the reaction container and is hermetically connected with the reaction container; an opening is formed in the upper end of the lining container; the lining container can resist the corrosion of hydrofluoric acid; the lining container can be selectively arranged in the reaction container; a sample inlet is formed in the reaction kettle; the sample inlet is provided with a control valve I; an exhaust port is formed in the reaction kettle; the exhaust port is provided with a control valve II; a pressure gauge is arranged on the reaction kettle; the tail gas absorption device is communicated with the exhaust port and used for absorbing gas exhausted from the exhaust port. By adopting the sample pretreatment device, sample pollution and impurity loss in the sample pretreatment process can be avoided, and the detection time is shortened on the premise of ensuring the accuracy and stability of detection data.

Description

Technical Field

[0001] The utility model relates to the technical field of polysilicon production, in particular to a chlorosilane pre-treatment device. Background Art

[0002] In the production of polysilicon, chlorosilane is an important raw material for preparing polysilicon, and the impurity content in chlorosilane is the main factor affecting the quality of polysilicon products. The main method for detecting impurities in the prior art is: add the chlorosilane sample to a clean PTFE crucible, add mannitol, and then add ultrapure water to generate silicon dioxide; then add hydrofluoric acid to dissolve the silicon dioxide, put it into a graphite furnace, and evaporate it with an electric heating plate; then dissolve the residue with nitric acid and make it constant with ultrapure water; finally, use inductively coupled plasma optical emission spectroscopy (ICP-OES) to quantitatively analyze the impurity elements.

[0003] Chlorosilane samples are prone to introducing impurities during the pretreatment process, and are also prone to losing impurities during the volatilization process, resulting in poor accuracy and repeatability of test data; moreover, the pretreatment of samples is time-consuming, affecting the detection efficiency. Utility Model Content

[0004] In view of this, the utility model provides a chlorosilane pretreatment device, the main purpose of which is to avoid sample contamination and impurity loss during sample pretreatment, and to shorten the detection time under the premise of ensuring accurate and stable detection data.

[0005] In order to achieve the above purpose, the utility model mainly provides the following technical solutions:

[0006] The embodiment of the utility model provides a chlorosilane pretreatment device, comprising: a reaction kettle, a lined container, and a tail gas absorption device;

[0007] The reactor comprises: a reaction container and an end cover;

[0008] The upper end of the reaction container has an opening;

[0009] The end cover is detachably locked at the opening of the reaction container and is sealed with the reaction container;

[0010] The upper end of the lined container has an opening; the lined container can withstand corrosion by hydrofluoric acid;

[0011] The liner container can be selectively placed in the reaction container;

[0012] The reactor is provided with an injection port for adding materials to the liner container in the reactor; the injection port is provided with a control valve 1;

[0013] The reactor is provided with an exhaust port for exhausting the gas in the reactor; the exhaust port is provided with a second control valve;

[0014] The reactor is provided with a pressure gauge;

[0015] The tail gas absorption device is communicated with the exhaust port and is used for absorbing the gas exhausted from the exhaust port.

[0016] Furthermore, the lined container is a polytetrafluoroethylene container.

[0017] Furthermore, the exhaust gas absorption device is detachably connected to the exhaust port via a quick connector.

[0018] Furthermore, the reaction container is a stainless steel cylindrical structure.

[0019] Furthermore, the reaction container is connected to the end cover via a threaded structure or a flange structure.

[0020] Furthermore, an anti-slip structure is provided on the outer wall of the reaction container.

[0021] Further, the injection port is arranged on the end cover;

[0022] The exhaust port is arranged on the end cover;

[0023] The pressure gauge is arranged on the end cover.

[0024] By means of the above technical solution, the chlorosilane pretreatment device of the present invention has at least the following advantages:

[0025] It can avoid sample contamination and impurity loss during sample pretreatment, shorten the detection time while ensuring the accuracy and stability of the detection data.

[0026] The above description is only an overview of the technical solution of the utility model. In order to more clearly understand the technical means of the utility model and implement it according to the contents of the specification, the following is a detailed description of the preferred embodiments of the utility model in conjunction with the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 A schematic diagram of a chlorosilane pretreatment device provided in an embodiment of the utility model.

[0028] As shown in the figure:

[0029] 1 is a reaction container, 2 is a liner container, 3 is an end cover, 4 is a tail gas absorption device, 5 is an injection port, 6 is an exhaust port, 7 is a control valve 2, 8 is a control valve 1, and 9 is a pressure gauge. DETAILED DESCRIPTION

[0030] In order to further explain the technical means and effects adopted by the utility model to achieve the predetermined utility model purpose, the specific implementation methods, structures, features and effects of the utility model application are described in detail below in conjunction with the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "embodiment" does not necessarily refer to the same embodiment. In addition, specific features, structures, or characteristics in one or more embodiments may be combined in any suitable form.

[0031] like Figure 1 As shown, a chlorosilane pretreatment device proposed in one embodiment of the utility model includes: a reactor, a liner container 2, and a tail gas absorption device 4; the reactor includes: a reaction vessel 1 and an end cap 3; the upper end of the reaction vessel 1 has an opening; preferably, the reaction vessel 1 is a stainless steel cylindrical structure with a reliable structure. The end cap 3 can be removably locked at the opening of the reaction vessel 1 and sealed with the reaction vessel 1; preferably, the reaction vessel 1 is connected to the end cap 3 by a threaded structure or a flange structure, which can achieve the sealing of the end cap 3 and the reaction vessel 1, and is convenient for disassembly and assembly. Further preferably, an anti-slip structure is provided on the outer wall of the reaction vessel 1 to facilitate the operator to operate the reaction vessel 1.

[0032] The upper end of the liner container 2 has an opening for convenient addition of materials; the liner container 2 can withstand the corrosion of hydrofluoric acid; in this embodiment, the liner container 2 is preferably a polytetrafluoroethylene container, which will not be corroded by hydrofluoric acid, has the characteristics of being resistant to acid and alkali, and resistant to various organic solvents, and is almost insoluble in all solvents. The liner container 2 can be selectively placed in the reaction container 1, and the liner container 2 is convenient to take out from the reaction container 1, which is convenient for operation.

[0033] The reactor is provided with an injection port 5 for adding materials to the liner container 2 in the reactor; the injection port 5 is provided with a control valve 1 8 for controlling the on-off of the injection port 5. The reactor is provided with an exhaust port 6 for discharging the gas in the reactor; the exhaust port 6 is provided with a control valve 2 7 for controlling the on-off of the exhaust port 6. The reactor is provided with a pressure gauge 9 for detecting the pressure in the reactor; the tail gas absorption device 4 is connected to the exhaust port 6 for absorbing the gas discharged from the exhaust port 6. In this embodiment, the tail gas absorption device 4 is preferably detachably connected to the exhaust port 6 through a quick connector to facilitate the quick connection of the tail gas absorption device 4 with the reactor.

[0034] As a preferred embodiment of the above, the injection port 5 is arranged on the end cover 3, which is conducive to the material entering the liner container 2 from above the liner container 2; the exhaust port 6 is arranged on the end cover 3, which is conducive to the discharge of gas. The pressure gauge 9 is arranged on the end cover 3.

[0035] The specific operation process is as follows:

[0036] Place a predetermined amount of ice cubes in the lined container 2, then freeze the lined container 2 and put it into the reactor; then put a certain amount of sample into the lined container 2 and lock the reactor; slowly open the exhaust port 6 after a period of reaction, and recover the exhaust gas through the exhaust gas absorption device 4; observe that the pressure gauge 9 shows that the predetermined pressure has been reached or wait until there are no bubbles in the exhaust gas absorption device 4, then open the injection port 5, and inject hydrofluoric acid into the lined container 2 through the injection port 5, and close the injection port 5 after the injection is completed; wait until the reaction is completed, close the exhaust port 6 and remove the exhaust gas absorption device 4; finally, transfer the reacted solution to a volumetric flask, fix the volume, and test.

[0037] A chlorosilane pretreatment device proposed in an embodiment of the utility model can avoid sample contamination and loss of impurities during sample pretreatment, shorten the detection time while ensuring the accuracy and stability of detection data, and achieve a detection limit of ppt or ppb level.

[0038] Further explanation, although the terms first, second, etc. can be used to describe various elements in this article, these terms should not limit these elements. These terms are only used to distinguish one element from another element. For example, the first element can be called the second element, and, similarly, the second element can be called the first element, and these terms are only used to distinguish one element from another element. This does not depart from the scope of exemplary embodiments. Similarly, element one and element two do not represent the order of elements, and these terms are only used to distinguish one element from another element. As used herein, the term "and / or" includes any combination and all combinations of one or more associated listed items.

[0039] In the description of the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", and "fixed" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0040] The standard parts used in the utility model can all be purchased from the market, and special-shaped parts can be customized according to the instructions and the drawings. The specific connection methods of each part adopt the conventional means such as mature bolts, rivets, welding, etc. in the existing technology. The machinery, parts and equipment all adopt the conventional models in the existing technology, and the circuit connection adopts the conventional connection method in the existing technology, which will not be described in detail here.

[0041] The above is only a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Any simple modification, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A chlorosilane pretreatment device, characterized in that: Including: reactor, lining container, tail gas absorption device; The reactor comprises: a reaction container and an end cover; The upper end of the reaction container has an opening; The end cover is detachably locked at the opening of the reaction container and is sealed with the reaction container; The upper end of the lined container has an opening; the lined container can withstand corrosion by hydrofluoric acid; The liner container can be selectively placed in the reaction container; The reactor is provided with an injection port for adding materials to the liner container in the reactor; the injection port is provided with a control valve 1; The reactor is provided with an exhaust port for exhausting the gas in the reactor; the exhaust port is provided with a second control valve; The reactor is provided with a pressure gauge; The tail gas absorption device is communicated with the exhaust port and is used for absorbing the gas exhausted from the exhaust port.

2. The chlorosilane pretreatment device according to claim 1, characterized in that: The lined container is a polytetrafluoroethylene container.

3. The chlorosilane pretreatment device according to claim 1, characterized in that: The tail gas absorption device is detachably connected to the exhaust port via a quick connector.

4. The chlorosilane pretreatment device according to claim 1, characterized in that: The reaction container is a stainless steel cylindrical structure.

5. The chlorosilane pretreatment device according to claim 1, characterized in that: The reaction container is connected to the end cover via a threaded structure or a flange structure.

6. The chlorosilane pretreatment device according to claim 5, characterized in that: An anti-slip structure is arranged on the outer wall of the reaction container.

7. The chlorosilane pretreatment device according to claim 1, characterized in that: The injection port is arranged on the end cover; The exhaust port is arranged on the end cover; The pressure gauge is arranged on the end cover.

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