Synthetic solid-liquid two-phase continuous feeding device

Abstract

The utility model relates to the technical field of chemical production, in particular to a synthetic solid-liquid two-phase continuous feeding device. According to the technical scheme, the synthetic solid-liquid two-phase continuous feeding device comprises a solvent feeding pipeline, a reaction solid feeding device, a reaction liquid feeding pipeline and a synthesis reactor, the solvent feeding pipeline is connected with an inlet of the reaction solid feeding device, and an outlet of the reaction solid feeding device is connected with a feeding hole of the synthesis reactor; the reaction liquid feeding pipeline is connected with a feeding hole of the synthesis reactor, and an inlet and an outlet of the reaction solid feeding device are connected with self-locking type quick sealing joints. According to the utility model, a solvent is connected with a plurality of groups of reaction solid feeding devices through the L-shaped ball valves, and the plurality of groups of reaction solid feeding devices are alternately used to realize scouring feeding of solids, so that the problem that the reaction cannot be continuously fed is solved, and the working efficiency is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to a chemical production technical field especially relates to a synthetic solid-liquid two-phase continuous feeding device. BACKGROUND

[0002] In recent years, trimethylsilane ((CH3)3SiH) as a semiconductor layer film forming raw material, mainly used for manufacturing semiconductor device thin film dielectric chemical vapor deposition silicon source gas, can deposit silicon carbide, silicon oxide or silicon nitride on the thin film dielectric, is the important raw material of plasma enhanced chemical vapor deposition (PECVD) industry, commonly used PECVD protective coating and damascene metallization application in low K dielectric layer and barrier layer PECVD process. The chemical used in the semiconductor field has very high requirements for its purity, the organic purity needs to reach 99.99%, and the inorganic purity is as high as 7N (99.99999%), so it is called electronic grade trimethylsilane. At present, there is no production in China, and the demand relies on import.

[0003] The synthesis method faces the safety problems of water decomposition or flammability of lithium aluminum hydride solid feeding, and the reaction feeding cannot be continuously carried out.

[0004] The patent with publication number CN221046028U discloses a continuous solid-liquid feeding device, which comprises a tank body and a guide pipe, the guide pipe vertically extends into the inside of the tank body, a powder feeding assembly communicating with the guide pipe is arranged above the tank body, a liquid uniform distribution piece is fixed to the outer side of the middle part of the guide pipe, a liquid feeding assembly extending into the tank body and guiding the liquid to flow into the liquid uniform distribution piece is arranged on the outer side of the top end of the tank body, and a liquid curtain forming assembly is fixed to the outer side of the bottom end of the guide pipe to receive and overflow the liquid on the outer side of the liquid uniform distribution piece. A liquid curtain is formed, which completely prevents the escape of dust and avoids environmental pollution caused by the escape of dust in the previous powder feeding equipment, but it does not realize continuous mixing during the solid-liquid feeding process and cannot be applied to various mixing forms. UTILITY MODEL CONTENTS

[0005] The utility model provides a kind of synthetic solid-liquid two-phase continuous feeding device, solve the problem that trimethylsilane synthesis in prior art faces lithium aluminum hydride solid feeding meets water decomposition or flammable, and reaction feeding cannot be continuously carried out.

[0006] To solve the above technical problems, the technical scheme adopted by the utility model is:

[0007] A kind of synthetic solid-liquid two-phase continuous feeding device, including solvent feeding pipe line, reaction solid feeding device, reaction liquid feeding pipe line and synthesis reactor;

[0008] The solvent feeding pipeline is connected with the inlet of the reaction solid feeding device, and the outlet of the reaction solid feeding device is connected with the feeding inlet of the synthesis reactor; the reaction liquid feeding pipeline is connected with the feeding inlet of the synthesis reactor, and the inlet and outlet of the reaction solid feeding device are both connected with self-locking quick sealing joints.

[0009] Further, the solvent feeding pipeline is connected with multiple reaction solid feeding devices through an L-shaped ball valve.

[0010] Further, the reaction solid feeding device comprises a tank body, a middle pipe is arranged in the middle of the top cover of the tank body and extends to the inside lower part of the tank body, a bottom plate is fixedly connected to the lower part of the outer ring surface of the middle pipe, an outer ring is fixedly connected to the inner ring surface of the tank body, a gap is left between the outer ring and the bottom plate, a lifting driving element is installed on the top cover of the tank body and extends into the tank body, a blocking ring is fixedly connected to the lifting end of the lifting driving element and blocks the gap between the outer ring and the bottom plate, and a dispersing cover is fixedly connected to the bottom end of the middle pipe, and the middle pipe and the dispersing cover are both fixed to the inner side wall of the tank body through branch rods.

[0011] Further, an elastic vibration mixing element is further arranged in the inside of the bottom cover of the tank body.

[0012] Further, a feeding inlet is arranged on the top cover of the tank body.

[0013] Further, the upper surface of the dispersing cover is semispherical, and the elastic vibration mixing element is located below the dispersing cover.

[0014] Further, a metering device is arranged on the reaction liquid feeding pipeline.

[0015] The positive effects of the synthetic solid-liquid two-phase continuous feeding device are as follows: 1. One of diethylene glycol dimethyl ether, 2-methyl tetrahydrofuran, ethylene glycol dimethyl ether and methyl tert-butyl ether is selected as a reaction solvent, the solvent is connected with multiple reaction solid feeding devices through an L-shaped ball valve, multiple groups are alternately used to realize the "flushing" feeding of the solid, the problem of non-continuous feeding in the reaction is solved, and the working efficiency is improved;

[0016] 2. Trimethylchlorosilane is selected as a liquid reactant, and one of lithium aluminum hydride, sodium aluminum hydride and sodium hydride is selected as a solid reactant, the solid reactant is filled into the reaction solid feeding device in anhydrous and oxygen-free environment, and the two ends are connected through self-locking quick sealing joints, so that the safety problems such as water flammability of the solid reactant are solved.

[0017] 3. The utility model discloses a solvent post-treatment and recovery system can realize the recycling of solvent, reach the purpose of continuous reaction, thereby reduce raw material cost, improve the output efficiency of trimethylsilane, have important industrial application value. BRIEF DESCRIPTION OF DRAWINGS

[0018] Figure 1 It is the flow chart of solid-liquid two-phase continuous feeding device of the utility model synthesis;

[0019] Figure 2 It is the structure diagram of reaction solid feeding device in the utility model;

[0020] Figure 3 It is the internal structure diagram of reaction solid feeding device in the utility model;

[0021] Figure 4 It is the longitudinal section view of reaction solid feeding device in the utility model;

[0022] Figure 5 It is the structure diagram of dispersion cover and middle pipe in the utility model;

[0023] Figure 6 It is the local structure diagram of reaction solid feeding device in the utility model;

[0024] In the drawing: 1, solvent feed line;2, L type ball valve;3, self-locking quick sealing joint;4, reaction solid feeding device;5, reaction solid discharge line;6, synthesis reactor;7, synthesis reactor bottom discharge line;8, reaction liquid feed line;9, metering device;401, tank;402, middle pipe;403, feed inlet;404, bottom plate;405, outer ring;406, lifting driving part;407, material blocking ring;408, dispersion cover;409, elastic vibration mixing part. DETAILED DESCRIPTION

[0025] The technical scheme in the embodiments of the utility model will be described clearly and completely below in conjunction with the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by those skilled in the art without creative labor are involved in the protection scope of the utility model.

[0026] Embodiment 1

[0027] In conjunction with Figure 1 As shown in the figure, a synthesized solid-liquid two-phase continuous feeding device includes solvent feed line 1, reaction solid feeding device 4, reaction liquid feed line 8 and synthesis reactor 6;

[0028] The solvent feeding pipe 1 is connected with the inlet of the reaction solid feeding device 4, and the outlet of the reaction solid feeding device 4 is connected with the feeding inlet of the synthesis reactor 6; the reaction liquid feeding pipe 8 is connected with the feeding inlet of the synthesis reactor 6, and the inlet and outlet of the reaction solid feeding device 4 are both connected with the self-locking quick sealing joint 3.

[0029] After the synthesis reactor 6 outlet is connected with the solvent post-treatment and recovery system, the solvent is returned to the solvent feeding pipe 1 for recycling, so that the excess raw materials are recycled and utilization rate of the raw materials is improved.

[0030] The solvent feeding pipe 1 is connected with multiple reaction solid feeding devices 4 through the L-shaped ball valve 2, and in actual use, multiple reaction solid feeding devices 4 can be used alternately to avoid production line shutdown and improve production efficiency.

[0031] The reaction liquid feeding pipe 8 is provided with a metering device 9, such as a flow controller or a liquid metering control device such as a feeding pump.

[0032] The reaction solid feeding device 4 should be filled with reaction solid particles in a water-free and oxygen-free environment.

[0033] The solid particles in the reaction solid feeding device 4 fall by gravity and are “flushed” by solvent to enter the synthesis reactor 6 through the reaction solid outlet pipe 5.

[0034] The bottom of the synthesis reactor 6 is provided with a synthesis reactor bottom outlet pipe 7, and after the reaction is completed, the solvent is recycled through the solvent post-treatment and recovery system, and the treated solvent is returned to the solvent feeding pipe 1 for recycling.

[0035] The solid reactants in the reaction solid feeding device 4 are flammable solids or water-reactive flammable solids such as lithium aluminum hydride, sodium aluminum hydride and sodium hydride.

[0036] In this embodiment, diethylene glycol dimethyl ether is connected with the L-shaped ball valve 2 through the solvent feeding pipe 1, and is connected with multiple reaction solid feeding devices 4 through the self-locking quick sealing joint 3 for alternating use.

[0037] Lithium aluminum hydride is filled into the reaction solid feeding device 4 in a water-free and oxygen-free environment.

[0038] The lithium aluminum hydride particles in the reaction solid feeding device 4 fall through the reaction solid outlet pipe 5 and most of them enter the synthesis reactor 6, and the remaining lithium aluminum hydride particles enter the synthesis reactor 6 through the “flushing” of solvent.

[0039] Trimethylchlorosilane is fed into the synthesis reactor 6 through the reaction liquid feeding pipe 8 after the flow rate is controlled by the metering device 9.

[0040] After the reaction is completed, the synthesis reactor 6 enters the solvent post-treatment and recovery system through the synthesis reactor bottom discharge pipeline 7 and then returns to the solvent feed pipeline 1 for recycling.

[0041] The continuous feeding of the solid reactant is realized, and the violent reaction caused by the contact of the solid reactant with air and water during the feeding process is avoided, so that the safety of the synthesis is ensured.

[0042] As can be understood by those skilled in the art, the continuous feeding device provided by the utility model can also be applied to the reaction production of other flammable solids or water-reactive flammable solids and liquid reactants, which are not listed here.

[0043] Example 2

[0044] When the internal space of the reaction solid feeding device 4 is filled with the solid reactant, the solvent is input from the top opening at this time, and due to the blockage of the lower solid reactant, the solvent cannot be in full contact with the solid reactant at this time, which will cause the solvent to be retained on the upper side of the solid reactant, and the solvent can flow down smoothly only after the lower solid reactant is completely dropped out, so that the full mixing of the solid reactant and the solvent cannot be realized, which affects the reaction efficiency and the synthesis effect. The following scheme is proposed in the embodiment:

[0045] In combination with Figures 2-6 The embodiment differs from example 1 in that the reaction solid feeding device 4 comprises a tank body 401, a middle through pipe 402 is arranged in the middle of the top cover of the tank body 401, the top end of the middle through pipe 402 is connected with the self-locking quick sealing joint 3, and the bottom cover outlet of the tank body 401 is also connected with the self-locking quick sealing joint 3.

[0046] The bottom end of the middle through pipe 402 extends to the inner lower part of the tank body 401, the outer ring surface of the middle through pipe 402 is fixedly connected with a bottom plate 404, the inner ring surface of the tank body 401 is fixedly connected with an outer ring 405, a gap is left between the outer ring 405 and the bottom plate 404, a lifting driving member 406 is installed on the top cover of the tank body 401, the lifting end of the lifting driving member 406 extends into the tank body 401, the lifting end of the lifting driving member 406 is fixedly connected with a blocking ring 407, the blocking ring 407 blocks the gap between the outer ring 405 and the bottom plate 404, the bottom end of the middle through pipe 402 is fixedly connected with a dispersing cover 408, and the middle through pipe 402 and the dispersing cover 408 are both fixed to the inner side wall of the tank body 401 through branch rods.

[0047] The top cover of the tank body 401 is provided with a feeding port 403.

[0048] In the embodiment, firstly, the lithium aluminum hydride is filled into the reaction solid feeding device 4 through the feeding port 403 in anhydrous and oxygen-free environment, and the solid material is placed in the space above the bottom plate 404 in the tank body 401, and the filling is completed, and then when the reaction is carried out, the solvent enters from the middle pipe 402;

[0049] The bottom end of the middle pipe 402 is fixed to the position of the dispersion cover 408, and the outlet is left, and the solvent flows out to the upper surface of the dispersion cover 408, and the lifting driving part 406 drives the blocking ring 407 to descend, the gap between the outer ring 405 and the bottom plate 404 is opened, and then the solid material on the upper side of the bottom plate 404 begins to fall down from the gap position, and then the solid material falls down to the surface of the dispersion cover 408 and is in contact with the reaction solvent, and then the solid reactant and the reaction solvent are fully mixed, and after mixing, the solid reactant and the solvent flow out from the outlet at the bottom of the tank body 401, and the problem of insufficient mixing caused by the overall filling of the solid material in the tank is avoided.

[0050] The elastic vibration mixing part 409 is installed on the inner side of the bottom cover of the tank body 401.

[0051] The upper surface of the dispersion cover 408 is hemispherical, and the elastic vibration mixing part 409 is located below the dispersion cover 408.

[0052] When the solid reactant and the solvent move to the bottom of the tank body 401, they will impact the elastic vibration mixing part 409, and the elastic vibration mixing part 409 will vibrate due to the elastic force, and further mix the solid reactant and the solvent during the vibration process, and further achieve the effect of full mixing.

[0053] The above-described embodiment describes the content in more detail and concretely, expresses the preferred embodiment of the utility model, and is only used for explaining the technical thought and characteristics of the utility model, and the purpose is to enable the person skilled in the art to understand the content of the utility model and to implement it, but is not limited to the utility model, and the patent range of the utility model cannot be limited by the embodiment, that is, any equivalent change or modification of the spirit disclosed by the utility model is still within the patent range of the utility model, and the local improvement of the system and the change between the subsystems, the transformation and the like are still within the patent range of the utility model.

Claims

1. A synthetic solid-liquid two-phase continuous feeding device, characterized by, The device comprises a solvent feeding pipeline (1), a reaction solid feeding device (4), a reaction liquid feeding pipeline (8) and a synthesis reactor (6). The solvent feeding pipeline (1) is connected with the inlet of the reaction solid feeding device (4), the outlet of the reaction solid feeding device (4) is connected with the feeding inlet of the synthesis reactor (6), and the reaction liquid feeding pipeline (8) is connected with the feeding inlet of the synthesis reactor (6).

2. A synthetic solid-liquid two-phase continuous feeding device according to claim 1, characterized in that, The solvent feeding pipeline (1) is connected with multiple reaction solid feeding devices (4) through L-shaped ball valves (2).

3. A synthetic solid-liquid two-phase continuous feeding device according to claim 1, characterized in that, The reaction solid feeding device (4) comprises a tank body (401), a middle pipe (402) is arranged in the middle part of the top cover of the tank body (401), the bottom end of the middle pipe (402) extends to the inner lower part of the tank body (401), a bottom plate (404) is fixedly connected to the lower part of the outer ring surface of the middle pipe (402), an outer ring (405) is fixedly connected to the inner ring surface of the tank body (401), a gap is left between the outer ring (405) and the bottom plate (404), a lifting driving element (406) is installed on the top cover of the tank body (401), the lifting end of the lifting driving element (406) extends into the tank body (401), a material blocking ring (407) is fixedly connected to the lifting end of the lifting driving element (406), the material blocking ring (407) blocks the gap between the outer ring (405) and the bottom plate (404), and a dispersing cover (408) is fixedly connected to the bottom end of the middle pipe (402).

4. A synthetic solid-liquid two-phase continuous feeding device according to claim 3, characterized in that, An elastic vibration mixing element (409) is further arranged in the inner side of the bottom cover of the tank body (401).

5. A synthetic solid-liquid two-phase continuous feeding device according to claim 4, characterized in that, A feeding inlet (403) is arranged on the top cover of the tank body (401).

6. A synthetic solid-liquid two-phase continuous feeding device according to claim 4, characterized in that, The upper surface of the dispersing cover (408) is semispherical, and the elastic vibration mixing element (409) is located below the dispersing cover (408).

7. A synthetic solid-liquid two-phase continuous feeding device according to claim 1, characterized in that, A metering device (9) is arranged on the reaction liquid feeding pipeline (8).

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