WO2024045103A1 - Système de réaction et méthode de production de nitrure de silicium - Google Patents

Système de réaction et méthode de production de nitrure de silicium Download PDF

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WO2024045103A1
WO2024045103A1 PCT/CN2022/116407 CN2022116407W WO2024045103A1 WO 2024045103 A1 WO2024045103 A1 WO 2024045103A1 CN 2022116407 W CN2022116407 W CN 2022116407W WO 2024045103 A1 WO2024045103 A1 WO 2024045103A1
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inlet
micro
reaction
silicon nitride
reaction tower
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PCT/CN2022/116407
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Chinese (zh)
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张志炳
孙海宁
李磊
吕权
张豪
李夏冰
周政
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南京延长反应技术研究院有限公司
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00873—Heat exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00905—Separation
    • B01J2219/00909—Separation using filters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/0095—Control aspects
    • B01J2219/00952—Sensing operations
    • B01J2219/00954—Measured properties
    • B01J2219/00961—Temperature

Definitions

  • the present invention relates to the technical field of silicon nitride preparation, and specifically to a reaction system and method for producing silicon nitride.
  • Silicon nitride is an inorganic substance with the chemical formula Si 3 N 4. It is an important structural ceramic material with high hardness, lubricity, atomic crystal, wear resistance, and oxidation resistance at high temperatures. It can also resist hot and cold shocks. It can be heated to more than 1000°C in the air and will not break even if it is rapidly cooled and then heated rapidly. Precisely because silicon nitride ceramics have such excellent properties, people often use it to manufacture mechanical components such as bearings, turbine blades, mechanical seal rings, and permanent molds.
  • the existing technology prepares silicon nitride powder through a low-temperature liquid phase method, that is, under low temperature conditions of -40°C, liquid ammonia is reacted with an organic solution of silicon tetrachloride to obtain the intermediate product silicon imine and the by-product chloride Ammonium is filtered, washed and heat treated to obtain silicon nitride powder.
  • the reaction process requires controlling the heat release so that the system temperature is always maintained at -40°C and the pressure in the reactor is approximately slightly positive.
  • the reaction is quite exothermic, and the instantaneous temperature rise can reach 10 to 20°C, which makes it difficult to stably control the reaction temperature in the tower;
  • the first object of the present invention is to provide a reaction system for producing silicon nitride, which achieves solvent-free production of silicon nitride and at the same time overcomes the problems of severe reaction exotherm and difficulty in controlling particle size in the prior art.
  • the second object of the present invention is to provide a method using the above reaction system, which is simple to operate and capable of producing silicon nitride with uniform and fine particle sizes.
  • the invention provides a reaction system for producing silicon nitride, which includes: a reaction tower and a heat transfer component; the heat transfer component is installed on the reaction tower; a micro-interface unit is provided in the reaction tower, and the micro-interface unit is installed in the reaction tower.
  • the interface unit includes a micro-interface generator and an expansion tube located above the micro-interface generator. The bottom of the expansion tube is connected to the micro-interface generator; the top of the expansion tube is connected to a silicon tetrachloride delivery pipeline.
  • the micro-interface generator is connected to a liquid ammonia delivery pipeline.
  • the present invention provides a reaction system for producing silicon nitride.
  • the reaction system can disperse and break the raw materials into micron-level droplets, thereby increasing the mass transfer area between the oil and water phases. , thus achieving the effect of strengthening the reaction;
  • the heat transfer component by setting up the heat transfer component, the heat released by the reaction can be removed in time, thereby controlling the reaction temperature in the tower, and at the same time providing conditions for solvent-free production of silicon nitride.
  • a circulation pipeline is provided outside the reaction tower, the inlet of the circulation pipeline is connected to the side wall of the reaction tower, and the outlet is connected to the top of the expansion tube; a heat exchanger is provided on the circulation pipeline. .
  • the heat transfer component includes a coiled tube and an outer jacket, the coiled tube is arranged on the inner wall of the reaction tower, and the outer jacket is arranged on the outer wall of the reaction tower.
  • a discharger is provided at the bottom of the reaction tower; the discharger is funnel-shaped, and the reaction product in the reaction tower flows out through the discharger.
  • the reaction product is solid silicon imine crystal, and the funnel-shaped discharger can prevent the outlet from being blocked.
  • the diameter of the expansion tube gradually increases from top to bottom, and the bottom of the expansion tube is in contact with the top wall of the micro-interface generator. This enables the various fluids to be fully mixed here, because the Reynolds number of the fluid in this tube is higher, the turbulence is more intense, and the mixing effect is better.
  • the reaction system of the present invention does not require the use of solvents during the production of silicon nitride, thereby avoiding separation difficulties in subsequent processing, which not only helps ensure the purity of the product, but also saves costs.
  • a heat transfer component composed of a coil and an outer jacket in the reaction tower
  • the reaction heat can be removed in time, thus ensuring the stability of the reaction temperature in the tower and effectively preventing system collapse caused by reaction heat.
  • the reaction speed is no longer a constraint in the production of silicon nitride, creating conditions for solvent-free production, the product purity is also greatly improved, and the ammonium chloride by-product can be more easily purified in the follow-up process. , to realize the collection and reuse of by-products.
  • the present invention realizes a solvent-free preparation scheme through a specific setting method of heat transfer components, greatly reduces production costs, and simultaneously improves production efficiency.
  • the present invention also integrates micro-interface technology into the production process of silicon nitride. Specifically, during the reaction, the raw material liquid ammonia and silicon tetrachloride can enter from the micro-interface unit, and are directly sent to the reaction after being emulsified by the micro-interface. The interior of the tower. In this way, it not only enhances the reaction by increasing the mass transfer area between the two phases and greatly improves the production efficiency, but also enables the effective generation of micron-sized silimine intermediates in the micron-level reaction system.
  • the use of micro-interface technology can also enable the reaction to generate The powder particle size distribution is more uniform.
  • the micro-interface unit of the present invention is composed of a micro-interface generator and an expansion tube. Liquid ammonia directly enters the micro-interface generator, and silicon tetrachloride enters the micro-interface generator through the expansion tube. In this way, the two liquid flows can pass through the micro-interface Collision is formed in the generator, and at the same time, under the action of the micro-interface generator, the pressure energy of silicon tetrachloride and liquid ammonia transported into the tower is converted into droplet surface energy and transferred to silicon tetrachloride and liquid ammonia, so that The two are broken to form a micron-scale oil-water two-phase reaction system that reacts in the tower, which increases the mass transfer area between the two phases, strengthens the reaction within the preset condition range, and allows the reaction to generate micron-scale silicon imine powder.
  • the reaction tower of the present invention is also provided with a circulation pipeline outside.
  • the circulation pipeline can continuously circulate the reaction liquid through external circulation, and send the reaction liquid into the expansion tube to mix with silicon tetrachloride and enter the micro-interface to generate In the reactor, it is conducive to the depth of the reaction; on the other hand, the heat exchanger set up on the circulation pipeline can remove the reaction heat in time. It cooperates with the heat transfer component to achieve better temperature control effect, which is beneficial to the tower.
  • the internal temperature remains constant.
  • the micro-interface generator used in the present invention has been reflected in the inventor's previous patents, such as application numbers CN201610641119.6, CN201610641251.7, CN201710766435.0, CN106187660, CN105903425A, Patents of CN109437390A, CN205833127U and CN207581700U.
  • the prior patent CN201610641119.6 introduces in detail the specific product structure and working principle of the micron bubble generator (i.e., micro-interface generator).
  • the application document records that “the micron bubble generator includes a main body and a secondary crushing part. It has a cavity, and the body is provided with an inlet communicating with the cavity.
  • the opposite first and second ends of the cavity are open, and the cross-sectional area of the cavity extends from the middle of the cavity to the first end and the second end of the cavity.
  • the second end is reduced; the secondary crushing piece is located at at least one of the first end and the second end of the cavity, a part of the secondary crushing piece is located in the cavity, and the secondary crushing piece is open to both ends of the cavity
  • An annular channel is formed between the through holes.
  • the micron bubble generator also includes an air inlet pipe and a liquid inlet pipe.” From the specific structure disclosed in the application document, we can know that its specific working principle is: the liquid enters the micron tangentially through the liquid inlet pipe.
  • the gas is rotated and cut at ultra-high speed, breaking the gas bubbles into micro-bubbles at the micron level, thereby increasing the mass transfer area between the liquid phase and the gas phase.
  • the micron bubble generator in this patent is a pneumatic micro-interface generator. device.
  • the primary bubble breaker has a circulating liquid inlet, a circulating gas inlet and a gas-liquid mixture outlet, while the secondary bubble breaker connects the feed inlet with the gas-liquid mixture outlet, indicating that the bubble breaker is Gas and liquid need to be mixed in.
  • the primary bubble breaker mainly uses circulating liquid as power, so in fact the primary bubble breaker is a hydraulic micro-interface generator, and the secondary bubble breaker is a gas-liquid generator. The mixture is simultaneously introduced into the elliptical rotating ball for rotation, thereby achieving bubble crushing during the rotation. Therefore, the secondary bubble breaker is actually a gas-liquid linkage micro-interface generator.
  • micro-interface generators are all specific forms of micro-interface generators.
  • the micro-interface generator used in the present invention is not limited to the above forms.
  • the specific structure of the bubble breaker recorded in the previous patent is only one of the forms that the micro-interface generator of the present invention can adopt.
  • the previous patent 201710766435.0 records that "the principle of the bubble breaker is high-speed jet flow to achieve mutual collision of gases", and also explains that it can be used in micro-interface strengthening reactors to verify the relationship between bubble breaker and micro-interface generator.
  • the correlation between; and the specific structure of the bubble breaker is also recorded in the previous patent CN106187660.
  • the top of the bubble breaker is the liquid phase inlet, and the side is the gas phase inlet.
  • the liquid phase coming in from the top provides entrainment power, thereby achieving the effect of crushing into ultra-fine bubbles. It can also be seen in the attached picture.
  • the bubble breaker has a conical structure, and the diameter of the upper part is larger than the diameter of the lower part, so that the liquid phase can better provide entrainment power.
  • micro-interface generator Since the micro-interface generator had just been developed in the early stages of the prior patent application, it was initially named micron bubble generator (CN201610641119.6), bubble breaker (201710766435.0), etc. With continuous technological improvements, it was later renamed micro-interface generator. Now the micro-interface generator and micro-interface generator in the present invention are equivalent to the previous micron bubble generator, bubble breaker, etc., but the names are different. To sum up, the micro-interface generator of the present invention belongs to the prior art.
  • the inlet of the circulation pipeline includes a first inlet and a second inlet, and the first inlet is located above the second inlet.
  • different inlets can be used to achieve circulation of the reaction liquid according to the height of the liquid level in the tower.
  • the reaction tower is provided with a first baffle, the top of the first baffle is higher than the first inlet in the vertical direction, and the bottom is located between the first inlet and the second inlet in the vertical direction. between imports.
  • a second baffle is provided in the reaction tower, the top of the second baffle is located between the first inlet and the second inlet in the vertical direction, and the bottom is located between the first inlet and the second inlet in the vertical direction. Below the second entrance.
  • the present invention can prevent the silimine crystals generated in the tower during the external circulation process from entering the circulation pipeline and blocking or damaging the devices on the pipeline, thereby improving the overall service life.
  • it also includes a washing filter, the discharger is connected to the washing filter, the filter residue outlet of the washing filter is connected to a silicon nitride output pipeline, and the filtrate outlet of the washing filter is connected to a recovery pipeline.
  • a screw conveyor is provided in the washing filter, and the filter residue is output through the screw conveyor; a liquid ammonia washing liquid transportation pipeline is provided above the washing filter.
  • the silicon nitride output pipeline includes a temperature-programmed furnace and a silicon nitride transport pipeline. After the filter residue is processed by the temperature-programmed furnace, it is output from the silicon nitride transport pipeline.
  • the recovery pipeline includes a crude ammonium chloride storage tank, an ammonia evaporator and an ammonia condenser.
  • the ammonia gas obtained enters the ammonia condenser.
  • the obtained crude ammonium chloride enters the crude ammonium chloride storage tank.
  • the invention also provides a method for producing silicon nitride, using the above production system to produce silicon nitride.
  • This method is simple to operate and can produce silicon nitride powder with uniform particle size and fineness.
  • Solvent-free The present invention adopts the preparation idea of solvent-free production of silicon nitride, which avoids the separation problem in subsequent processing. In addition, it adopts multiple heat transfer methods, so there is no need to worry about system collapse and reaction due to obvious heat release. Speed is no longer a constraint in silicon nitride production, product purity has been greatly improved, and ammonium chloride by-products can be purified more easily in the follow-up process;
  • the reaction system of the present invention can realize continuous production, and the liquid ammonia during the reaction process can be continuously recycled;
  • the product has uniform particle size and high fineness: after the present invention changes the traditional silicon nitride preparation process to a micro-interface strengthening process, the raw materials liquid ammonia and silicon tetrachloride can enter from the micro-interface unit, and then emulsified through the micro-interface Then it is sent directly to the inside of the reaction tower. In this way, it not only enhances the reaction by increasing the mass transfer area between the two phases and greatly improves the production efficiency, but also enables the effective generation of micron-sized silimine intermediates in the micron-level reaction system.
  • the use of micro-interface technology can also enable the reaction to generate The powder particle size distribution is more uniform.
  • Figure 1 is a schematic structural diagram of a reaction system provided by an embodiment of the present invention.
  • connection should be understood in a broad sense.
  • connection or 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 an internal connection between two components.
  • connection or integral connection
  • connection or integral connection
  • connection 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 an internal connection between two components.
  • specific meanings of the above terms in the present invention can be understood on a case-by-case basis.
  • this embodiment provides a reaction system for producing silicon nitride, including: a reaction tower 24 and a heat transfer component.
  • the heat transfer component is installed on the reaction tower 24; a micro-interface unit is provided in the reaction tower 24.
  • the interface unit includes a micro-interface generator 7 and an expansion tube 4 located above the micro-interface generator 7.
  • the bottom of the expansion tube 4 is connected to the micro-interface generator 7; the top of the expansion tube 4 is connected to a silicon tetrachloride delivery pipeline 2.
  • the interface generator 7 is connected to a liquid ammonia delivery pipeline 9 .
  • the diameter of the expansion tube 4 in this embodiment gradually increases from top to bottom, and the bottom of the expansion tube 4 is in contact with the top wall of the micro-interface generator 7 .
  • the heat transfer component includes a coil 8 and an outer jacket 10.
  • the coil 8 is coiled on the inner wall of the reaction tower 24, and the outer jacket 10 is set on the outer wall of the reaction tower 24.
  • the coil 8 is passed through Low-temperature heat transfer oil, -55°C/-65°C ethylene glycol aqueous solution or low-temperature heat transfer oil is passed into the outer jacket 10 to keep it cold.
  • a circulation pipeline 25 is provided outside the reaction tower 24.
  • the inlet of the circulation pipeline 25 is connected to the side wall of the reaction tower 24, and the outlet is connected to the top of the expansion tube 4; a heat exchanger 1 is provided on the circulation pipeline 25. and circulation pump 22.
  • the inlet of the circulation pipeline 25 includes a first inlet 26 and a second inlet 27 , and the first inlet 26 is located above the second inlet 27 .
  • different inlets can be selected to realize circulation of the reaction liquid according to the height of the liquid level in the tower.
  • the top of the reaction tower 24 is also connected to a flushing pipeline 3.
  • the flushing pipeline 3 is used to prevent the internal blockage of the reaction tower 24 from occurring.
  • an organic solvent can be input through the flushing pipeline 3. dredge.
  • a first baffle 5 and a second baffle 6 are provided in the reaction tower 24, wherein the top of the first baffle 5 is high in the vertical direction.
  • the bottom is located between the first inlet 26 and the second inlet 27 in the vertical direction.
  • the top of the second baffle 6 is located between the first inlet 26 and the second inlet 27 in the vertical direction, and the bottom is located below the second inlet 27 in the vertical direction.
  • a discharger 11 is provided at the bottom of the reaction tower 24; the discharger 11 is funnel-shaped, and the reaction product in the reaction tower 24 passes through The discharger 11 flows out.
  • the reaction system of this embodiment also includes a washing filter 12.
  • the discharger 11 is connected to the washing filter 12.
  • the filter residue outlet of the washing filter 12 is connected to a silicon nitride output pipeline, and the filtrate outlet of the washing filter 12 is connected to a recovery pipeline.
  • a screw conveyor 14 is provided in the washing filter 12, and the filter residue is output through the screw conveyor 14 and enters the silicon nitride output pipeline; a liquid ammonia washing liquid transportation pipeline 13 is provided above the washing filter 12.
  • a nitrogen pressurizing device 23 can also be provided to increase the filtration pressure.
  • the silicon nitride output pipeline includes a programmed temperature furnace 15 and a silicon nitride transport pipeline 16.
  • the filter residue is processed by the programmed temperature furnace 15 to generate the final product silicon nitride, and the generated silicon nitride is output from the silicon nitride transport pipeline 16.
  • the recovery pipeline includes a crude ammonium chloride storage tank 20, an ammonia evaporator 19 and an ammonia condenser 18.
  • the filtrate filtered out by the washing filter 12 is processed by the ammonia evaporator 19, the obtained ammonia gas enters the ammonia condenser 18, and the obtained The crude ammonium chloride enters the crude ammonium chloride storage tank 20 .
  • the liquid ammonia is sent to the liquid ammonia transport pipeline 9 through the return pipeline 17 above it.
  • the crude ammonium chloride storage tank 20 is connected to a crude ammonium chloride delivery pipeline 21 for outputting crude ammonium chloride.
  • the entire system is replaced with nitrogen, and silicon tetrachloride and liquid ammonia are cooled to -35°C ⁇ -45°C and then input into the micro-interface unit; silicon tetrachloride and liquid ammonia are dispersed and crushed in the micro-interface unit After forming into micro droplets, it is sent to the reaction tower 24 for reaction.
  • the generated product is sent to the washing filter 12. It is sprayed with liquid ammonia and washed 4-5 times until the ammonium chloride is completely dissolved in the liquid ammonia filtrate, and the obtained filter residue is sent to the washing filter 12.
  • the filtrate obtained by washing is sent to the ammonia evaporator 19, and the ammonia gas obtained by evaporation is cooled to liquid ammonia in the ammonia condenser 18 and then sent to the liquid ammonia
  • the ammonia transport pipeline 9 is reused, and the crude ammonium chloride obtained after evaporation enters the crude ammonium chloride storage tank 20 and is output to the purification process through the crude ammonium chloride transport pipeline 21.
  • the silicon nitride powder produced has uniform particle size, with a particle size between 1 ⁇ m and 3 ⁇ m.
  • Embodiment 1 The only difference between this example and Embodiment 1 is that in this example, the bottom of the expansion tube 4 is deep inside the micro-interface generator 7 .
  • the silicon nitride powder produced has a uniform particle size, with a particle size between 2 ⁇ m and 6 ⁇ m.
  • Example 1 The only difference between this example and Example 1 is that no micro-interface unit is used.
  • the silicon nitride powder produced has a relatively uniform particle size, with a particle size between 5 ⁇ m and 20 ⁇ m.
  • Example 2 Comparing the silicon nitride powder produced in Example 1 and Example 2, it can be seen that although the minimum particle size of the silicon nitride powder of Example 1 and Example 2 is basically the same, the particle size distribution of the silicon nitride powder of Example 1 is Narrower, and the overall particle size is finer. This may be because the expansion tube directly penetrates into the microinterface generator, which affects the residence time of silicon tetrachloride and the circulating fluid itself in the microinterface generator, and also affects the retention time of silicon tetrachloride and the circulating fluid itself in the microinterface generator. The hedging effect between silicon nitride, circulating liquid and liquid ammonia shows that the best quality silicon nitride can be obtained only when the bottom of the expansion tube is in direct contact with the top wall of the micro-interface generator.
  • Example 1 Comparing with the silicon nitride powder produced in Example 1, it can be seen that the silicon nitride powder in Example 1 has finer particle size, narrower particle size distribution, and better uniformity, indicating that the use of micro-interface technology can improve the performance of silicon nitride. Uniformity, while making the generated silicon nitride powder finer.
  • the reaction system for producing silicon nitride of the present invention can achieve solvent-free production, has low production cost, and produces silicon nitride powder with uniform particle size and high fineness.

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Abstract

L'invention concerne un système de réaction pour produire du nitrure de silicium, comprenant : une colonne de réaction (24) et un ensemble de transfert de chaleur, l'ensemble de transfert de chaleur étant monté sur la colonne de réaction (24) ; une unité de micro-interface est disposée dans la colonne de réaction (24) ; l'unité de micro-interface comprend un générateur de micro-interface (7) et un tuyau d'expansion (4) situé au-dessus du générateur de micro-interface (7) ; le bas du tuyau d'expansion (4) est en communication avec le générateur de micro-interface (7) ; la partie supérieure du tuyau d'expansion (4) est reliée à une conduite de transport de tétrachlorure de silicium (2) ; et le générateur de micro-interface (7) est relié à une conduite de transport d'ammoniac liquide (9).
PCT/CN2022/116407 2022-08-31 2022-09-01 Système de réaction et méthode de production de nitrure de silicium WO2024045103A1 (fr)

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CN202211051665.6A CN115337882A (zh) 2022-08-31 2022-08-31 一种生产氮化硅的反应系统及方法
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CN111569789A (zh) * 2020-04-13 2020-08-25 南京延长反应技术研究院有限公司 一种微界面强化环己酮氨肟化反应系统及方法
CN113546583A (zh) * 2021-07-16 2021-10-26 南京延长反应技术研究院有限公司 一种dmc的微界面制备系统及制备方法
CN113680287A (zh) * 2021-09-01 2021-11-23 南京延长反应技术研究院有限公司 一种制备三甲基苯醌的强化氧化系统及方法

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