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CN-122006581-A - Preparation device and preparation method of nano silicon-nitrogen-hydrogen powder

CN122006581ACN 122006581 ACN122006581 ACN 122006581ACN-122006581-A

Abstract

The application provides a preparation device and a preparation method of nano silicon nitrogen hydrogen powder. The preparation device comprises a feeder, a liquid evaporator, a first electric heating insulation sleeve, a gas buffer, a second electric heating insulation sleeve, a reaction container and a controller, wherein a feed inlet is formed in the feeder, the liquid evaporator is communicated with the feeder, the first electric heating insulation sleeve is sleeved outside the liquid evaporator and used for heating the liquid evaporator, the gas buffer is communicated with the liquid evaporator, the second electric heating insulation sleeve is sleeved outside the gas buffer and used for heating the gas buffer, the reaction container is communicated with the gas buffer through a second air inlet pipe and is provided with a vacuumizing port, a second pressure transmitter and a second air inlet, and the first pressure transmitter and an electromagnetic valve are sequentially arranged on the second air inlet pipe along the air conveying direction of the second air inlet pipe. The device completely avoids the blockage of the nano silicon-nitrogen-hydrogen powder products in the second air inlet and the second air inlet pipe, and is beneficial to continuous production.

Inventors

  • WANG YUAN

Assignees

  • 北京市嵘麒科技有限公司

Dates

Publication Date
20260512
Application Date
20260226

Claims (10)

  1. 1. The preparation device of the nano silicon nitrogen hydrogen powder is characterized by comprising the following components: the feeding device comprises a feeder (4), wherein a feeding port (1) is formed in the feeder (4); A liquid evaporator (8) in communication with the feeder; The first electric heating insulation sleeve (7) is sleeved outside the liquid evaporator and is used for heating the liquid evaporator; a gas buffer (11) in communication with the liquid evaporator; The second electric heating insulation sleeve (10) is sleeved outside the gas buffer and is used for heating the gas buffer; the reaction container (18) is communicated with the gas buffer through a second gas inlet pipe (13), and the reaction container (18) is provided with a vacuumizing port (15), a second pressure transmitter (16) for monitoring the internal pressure of the reaction container and a second gas inlet (17); A first pressure transmitter (12) and an electromagnetic valve (14) for monitoring the internal pressure of the gas buffer are sequentially arranged on the second gas inlet pipe along the gas conveying direction of the second gas inlet pipe; and the controller is electrically connected with the first pressure transmitter, the electromagnetic valve and the second pressure transmitter.
  2. 2. The device according to claim 1, characterized in that the liquid evaporator (8) is communicated with the feeder (4) through a liquid inlet pipe (6), the feeder (4) is also provided with a first air inlet (2), and the liquid inlet pipe (6) is also provided with a ball valve (5); And the height H2 of the liquid evaporator (8) is taken as a meter, and the distance between the communication position of the liquid inlet pipe (6) and the liquid evaporator (8) and the bottom height of the liquid evaporator (8) is 0.05-0.15H2.
  3. 3. The device according to claim 2, wherein the gas buffer (11) is communicated with the liquid evaporator (8) through a first air inlet pipe (9), and the communication position between the liquid evaporator (8) and the first air inlet pipe (9) is 0.05-0.15h2 from the top of the liquid evaporator (8).
  4. 4. A device according to claim 3, characterized in that the first inlet pipe (9) is on the same centre line as the second inlet pipe (13).
  5. 5. The device according to claim 1, wherein the communication position between the second air inlet pipe (13) and the reaction vessel (18) is 0.3-0.8h4 from the bottom of the reaction vessel (18) by taking the height H4 of the reaction vessel (18) as a reference.
  6. 6. A method for preparing nano silazane powder by using the device of any one of claims 1-5, characterized in that the preparation method comprises the following steps: step 1), closing the ball valve (5) and the electromagnetic valve (14); Step 2), vacuumizing the reaction container (18) through a vacuumizing port (15) and a second air inlet (17) in sequence, and introducing N 2 , and repeating for a plurality of times to ensure that the initial negative pressure in the reaction container is-100 to-50 kPa; Adding SiCl 4 liquid into the feeder (4) from the feed inlet (1), and sealing the feed inlet (1); Heating the liquid evaporator (8) and the gas buffer (11) to 50-200 ℃ respectively, and preserving heat, wherein the temperature of the gas buffer is more than or equal to the temperature of the liquid evaporator; Step 3), opening a ball valve (5), introducing N 2 into the feeder through a first air inlet (2), pushing SiCl 4 liquid into a liquid evaporator, and closing the ball valve (5) to obtain SiCl 4 gas in a gas buffer (11); Step 4), the first pressure transmitter (12) monitors the SiCl 4 gas pressure information in the gas buffer in real time and transmits the information to the controller, the second pressure transmitter (16) monitors the pressure information in the reaction vessel in real time and transmits the information to the controller, and the controller controls the opening and closing of the electromagnetic valve after processing the two kinds of pressure information, so that the SiCl 4 gas is led into the reaction vessel in stages and reacts with NH 3 gas which is continuously led in through the second air inlet (17) to generate the nano silicon-nitrogen-hydrogen powder.
  7. 7. The method according to claim 6, wherein the step 4) comprises: Step 4-1), a first pressure transmitter monitors first pressure information of SiCl 4 gas in the gas buffer in real time and transmits the first pressure information to a controller, the controller processes the first pressure information to obtain a first pressure value and compares the first pressure value with a solenoid valve on set value and a solenoid valve off set value, and when the first pressure value reaches the solenoid valve on set value, the solenoid valve is controlled to be opened so as to enable SiCl 4 gas to be introduced into a reaction container; Step 4-2), in the process of introducing SiCl 4 gas into the reaction vessel, a second pressure transmitter monitors second pressure information in the reaction vessel in real time and transmits the second pressure information to a controller, the controller processes the second pressure information to obtain a second pressure value and compares the second pressure value with a first set pressure value, when the second pressure value reaches the first set pressure value, an electromagnetic valve is closed, NH 3 gas is continuously introduced into the reaction vessel through a second air inlet and reacts with SiCl 4 gas to generate nano silicon-nitrogen-hydrogen powder, a second pressure transmitter (16) monitors third pressure information in the reaction vessel in real time and transmits the third pressure information to the controller, the controller processes the third pressure information to obtain a third pressure value and compares the third pressure value with the second set pressure value, and when the third pressure value reaches the second set pressure value, the electromagnetic valve is controlled to be opened again; Step 4-3), the SiCl 4 gas is introduced into the reaction vessel again, the second pressure transmitter monitors the fourth pressure information in the reaction vessel in real time and transmits the fourth pressure information to the controller, the controller processes the fourth pressure information to obtain a fourth pressure value and compares the fourth pressure value with the first set pressure value, and when the fourth pressure value reaches the first set pressure value, the electromagnetic valve is closed; Step 4-4), the step 4-3) is circulated until the sixth pressure value obtained after the sixth pressure information transmitted by the first pressure transmitter is processed by the controller is smaller than or equal to the electromagnetic valve disconnection set value, the electromagnetic valve is closed, and NH 3 gas is introduced.
  8. 8. The method according to claim 7, wherein the solenoid valve on setting value is 0.007 to 0.015mpa and the solenoid valve off setting value is 0.001 to 0.006mpa.
  9. 9. The method of claim 7, wherein the first set pressure value is-80 to-10 kPa, the second set pressure value is-100 to-60 kPa, and the second set pressure value is less than the first set pressure value.
  10. 10. The method according to claim 7, wherein the flow rate of the NH 3 gas is 0.1 to 10 liters/min and the pressure is 0.002 to 0.05MPa.

Description

Preparation device and preparation method of nano silicon-nitrogen-hydrogen powder Technical Field The disclosure relates to the technical field of nano-silicon-nitrogen-hydrogen inorganic powder production, in particular to a preparation device and a preparation method of nano-silicon-nitrogen-hydrogen powder. Background The silicon-nitrogen-hydrogen inorganic powder is a core precursor for preparing nitride ceramics. Silicon nitride ceramics, which are high-value added nitride ceramics, are widely used in the field of high-quality, high-value added ceramic materials. The existing preparation method of the silicon-nitrogen-hydrogen inorganic substance powder adopts a liquid-liquid phase reaction method, namely, liquid ammonia and liquid silicon tetrachloride are adopted to react, and an organic solvent, namely toluene, is selected as an interface reaction phase, and the liquid ammonia and the liquid silicon tetrachloride are contacted and react in a toluene phase interface, so that the silicon-nitrogen-hydrogen inorganic substance powder is prepared. However, the liquid-liquid phase reaction method has the defects that firstly, in the device for preparing the nano silicon nitrogen hydrogen powder by adopting the liquid-liquid phase reaction method at present, the nano silicon nitrogen hydrogen powder which is a product generated by the reaction of silicon tetrachloride liquid and liquid ammonia is easy to expand to a pipeline and aggregate, so that the product is blocked in the pipeline, and the process continuity and the production safety are affected. Secondly, the liquid-liquid reaction releases heat to cause vaporization of liquid ammonia and toluene, but the ammonia and toluene in a gas phase obtained by the vaporization of the liquid ammonia and the toluene are required to be separated, pressurized and liquefied or absorbed by other substances, so that higher production cost is caused, leakage and environmental pollution can be even caused, and thirdly, the pollution sources in the silicon-nitrogen-hydrogen inorganic powder prepared by the method can introduce toluene besides silicon tetrachloride and ammonia, so that the purity of the product is seriously reduced, and the performance of the subsequent preparation of silicon nitride powder is deteriorated. Therefore, the existing preparation of the silicon-nitrogen-hydrogen inorganic powder has the technical problems of pipeline blockage, low product purity and high energy consumption. Disclosure of Invention The application provides a preparation device and a preparation method of nano silicon nitrogen hydrogen powder, which are used for at least solving one of the technical problems in the prior art. In a first aspect, the present application provides a device for preparing nano silazane powder, including: The feeder is provided with a feed inlet; A liquid evaporator in communication with the feeder; The first electric heating insulation sleeve is sleeved outside the liquid evaporator and is used for heating the liquid evaporator; A gas buffer in communication with the liquid evaporator; the second electric heating insulation sleeve is sleeved outside the gas buffer and is used for heating the gas buffer; the reaction container is communicated with the gas buffer through a second air inlet pipe, and is provided with a vacuumizing port, a second pressure transmitter for monitoring the internal pressure of the reaction container and a second air inlet; a first pressure transmitter and an electromagnetic valve for monitoring the internal pressure of the gas buffer are sequentially arranged on the second air inlet pipe along the air conveying direction of the second air inlet pipe; and the controller is electrically connected with the first pressure transmitter, the electromagnetic valve and the second pressure transmitter. In an implementation manner, the liquid evaporator is communicated with the feeder through a liquid inlet pipe, a first air inlet is further formed in the feeder, a ball valve is further arranged on the liquid inlet pipe, the height H2 of the liquid evaporator is taken as a meter, and the distance between the communication position of the liquid inlet pipe and the liquid evaporator and the height of the bottom of the liquid evaporator is 0.05-0.15H2. In an implementation manner, the gas buffer is communicated with the liquid evaporator through a first air inlet pipe, and the distance between the communication position of the liquid evaporator and the first air inlet pipe and the height of the top of the liquid evaporator is 0.05-0.15H2. In an embodiment, the first air inlet pipe and the second air inlet pipe are on the same central line. In an embodiment, the height H4 of the reaction vessel is 0.3-0.8H 4, where the distance between the second air inlet pipe and the bottom of the reaction vessel is the height of the second air inlet pipe. In a second aspect, the present application provides a method for preparing nano silazane powde