Preparing a special reaction kettle: when no vacuum condition exists, the air is discharged by using a method of introducing ammonia gas in advance, the residual oxygen gas consumes the residual oxygen gas in the reaction kettle by using a reaction consumption method, and because titanium tetrachloride reacts with the oxygen gas firstly, the residual nitrogen gas and the introduced ammonia gas are mixed to react in an ammonia nitrogen mixed environment, the titanium nitride has high density and small volume, but the reaction heat is overlarge, and is directly vaporized and condensed with ammonium chloride steam on the upper part of the reaction kettle; after the reaction, the ammonia gas amount is rapidly reduced, the pressure is reduced, and a pressure gauge with sensitive display needs to be installed. The sealing performance of the reaction kettle is good for producing high-quality titanium nitride. This reation kettle adopts the type of falling the pear, big-end-up, and the bottom is the drain hole, and bottom one side has the exhaust hole, and both sides are equipped with the manometer that shows pressure, and for guaranteeing going on of reaction continuously, reation kettle designs has special structure, and the titanium nitride that generates and ammonium chloride all adsorb in reation kettle, must cool off, and follow-up production of ability after the washing is emptied, and the anaerobic environment destroys, so can only intermittent type preparation.

The following technical scheme is adopted:

a method for preparing a titanium nitride section by utilizing solid titanium tetrachloride and low-temperature liquid ammonia is characterized by comprising the following steps:

the method for preparing the titanium nitride section by utilizing the solid titanium tetrachloride and the low-temperature liquid ammonia adopts the reaction of titanium tetrachloride and ammonia to prepare titanium nitride under the anaerobic condition, and meets the chemical equation: tiCl (titanium dioxide)₄ +NH₃ →TiNx+NH₄ Cl ↓solution, in order to avoid overhigh temperature and energy waste, the reaction temperature is controlled within the range of normal temperature to-77.5 ℃; in order to ensure continuous production, the melting point difference between the melting point of liquid ammonia at minus 77.75 ℃ and the melting point of titanium tetrachloride at minus 24.1 ℃ is utilized, the synthesized titanium tetrachloride is properly cooled to be more than minus 20 ℃ under the conditions of no oxygen and low temperature, the titanium tetrachloride is added into film-making equipment at minus 34 ℃ to minus 77.5 ℃ for rapid solidification, the titanium tetrachloride is prepared into a required shape, at least comprises a thin plate, a thin wire and a special shape, the solid-state formed titanium tetrachloride is combined with liquid ammonia, a single piece of the solid-state formed titanium tetrachloride is slowly inserted into a liquid ammonia tank, and on one hand, the titanium tetrachloride can be quantitatively added to control the reaction temperature; the other partySurface-stabilized solid-formed titanium tetrachloride in a defined pattern, since TiCl₄ +NH₃ →TiNx+NH₄ Emitting a large amount of heat in the Cl ≠ reaction process to cause vaporization of liquid ammonia and titanium tetrachloride, being incapable of keeping a titanium atom stable structure of the titanium tetrachloride, producing a shaped TiNx product, controlling the temperature to be-34 to-77.5 ℃, solidifying the titanium tetrachloride into a sheet under the condition that the temperature is lower than the boiling point of the liquid ammonia to be-33.5 ℃, wherein the titanium atom is in a three-dimensional structure, when the titanium tetrachloride single sheet is slowly added, the titanium tetrachloride single sheet can also move in a liquid ammonia pool to avoid overhigh local temperature, the generated TiNx still keeps the original shape, and the TiNx is thinned, thinned and in a low-temperature state, and the liquid ammonia in a liquid state and the sheet titanium tetrachloride react to not cause overhigh local temperature and change the existing shape of the TiNx;

the method for preparing the titanium nitride TiNx further comprises the following steps:

step one, creating an oxygen-free dry reaction area:

under the aerobic condition, titanium tetrachloride reacts with oxygen and water vapor to form white smoke, the curing structure of the titanium tetrachloride is damaged, the designed reaction cannot be carried out, the whole reaction area is sealed, the reaction area is firstly vacuumized to a certain degree, and then nitrogen is filled into the reaction area as protective gas, so that negative pressure operation is avoided, and high cost is generated due to the maintenance of negative pressure and vacuum environment;

step two, establishing a low-temperature reaction area:

the whole reaction is completed in a low-temperature environment, the solid state and ammonia of the titanium tetrachloride are kept in liquid state in the operation process, the low temperature is controlled between minus 34 ℃ and minus 77.5 ℃, the reaction temperature and the low temperature are kept, a corresponding low-temperature reaction area is created in advance to ensure that the expected process requirement is met, and the ammonia can exist in a normal-pressure liquid state in the low-temperature environment to form a stable reaction tank;

step three, manufacturing titanium tetrachloride curing molding equipment:

the solidification of titanium tetrachloride is finished in a film forming device or a special-shaped device, the film forming device is in the shape of a side vertical triangle of a solar water heater, the upper end of the film forming device is provided with a constant volume transverse groove, one side of the constant volume transverse groove is provided with a low-temperature forming inclined plane, one side of the constant volume transverse groove close to the low-temperature forming inclined plane is provided with a uniform slit or a point hole, the slit can condense the titanium tetrachloride leaking downwards on a forming surface into a thin plate, the point hole condenses the titanium tetrachloride leaking downwards into the design shapes of filaments, thin strips and the like, the working temperature is an upper limit area of-34 to-77.5 ℃, the constant volume transverse groove at the upper end is designed according to the width and the depth of a reaction tank and can be properly adjusted, the smaller the temperature difference is, the longer the flow is, and the titanium tetrachloride is equally formed into a longer and thinner shape;

step four, curing and molding titanium tetrachloride:

titanium tetrachloride which is close to the melting point of-24.1 ℃ is put into the constant volume transverse groove, liquid titanium tetrachloride which is close to the melting point flows to a low-temperature forming inclined plane between-34 ℃ and-77.5 ℃ from a slit of the constant volume transverse groove every time the titanium tetrachloride is added according to a standard amount, the liquid titanium tetrachloride flows out from the slit because the temperature of the low-temperature forming inclined plane is far lower than the melting point, the titanium tetrachloride flows out from the slit, the titanium tetrachloride is quickly condensed into designed titanium tetrachloride thin plates and/or thin wires on the low-temperature forming inclined plane in the gravity down-flow process, the titanium tetrachloride which is added into the constant volume transverse groove at the upper end cannot be too much because the length of the inclined plane is limited, otherwise, the titanium tetrachloride is too thick and too long, the process can be prefabricated into two types of thin plates and/or thin wires, the upper end is the lower end low temperature zone which is close to the melting point of the titanium tetrachloride, the lower end low temperature zone is between-34 ℃ and-77.5 ℃, the titanium tetrachloride is put into the upper end transverse groove, the titanium tetrachloride is laterally turned over and poured onto the titanium tetrachloride is poured onto the titanium tetrachloride forming inclined plane, the titanium tetrachloride film forming equipment to finish solidification and stripping, the stripping is paved by adopting a film-foldable inclined plane, the printing paper or the wax stripping paper, the wax stripping paper is convenient for stripping process, the titanium tetrachloride is not used for stripping, the pre-coating of the titanium tetrachloride is not used for reaction, and the pre-coated film forming inclined plane, and the titanium tetrachloride is not used for the pre-coated on the titanium tetrachloride forming inclined plane, and the titanium tetrachloride is not used for the titanium tetrachloride forming tank, and the titanium tetrachloride is not used for the reaction;

step five, reaction control:

in order to ensure that the reaction is expected, the temperature is between minus 34 ℃ and minus 77.5 ℃, the environmental temperature is as close to the lower limit or the lower area of the temperature zone as possible, the titanium tetrachloride single slice is immersed and inserted into the liquid ammonia tank in a progressive mode due to the large heat release amount of the reaction, the speed cannot be too high, and the submerging speed is adjusted according to the high and low environmental temperature and the thickness of the solid titanium tetrachloride plate;

step six, extraction and cleaning of reaction smoke dust:

reaction product NH₄ The Cl ↓reactionprocess and the Cl ℃ reaction process exist in a gas state, so that the reaction is prevented from being solidified and sinking to enter a reaction tank, and the reaction is prevented from going down and going on; an exhaust fan is arranged on one side of the upper end of the reaction tank, a collector is arranged on the rear side of the exhaust fan, and NH is timely discharged₄ Cl ↓ ] smoke dust is pumped away, condensed in the collector, and liquid ammonia is supplemented at regular time, so that the depth of the reaction tank is stabilized in a certain area, and NH which cannot be pumped away at the bottom of the reaction tank is cleaned regularly₄ Cl ≈ precipitate;

step seven, cleaning a TiNx molding finished product:

the surface of the TiNx section taken out from the liquid ammonia reaction tank is adhered with certain liquid ammonia, the TiNx section is transferred to a region with the temperature of more than 33.5 ℃ below zero for volatilization and cleaning, the volatilized ammonia gas is periodically pumped back to the lower end low temperature region with the temperature of 34 ℃ below zero to 77 ℃ below zero, and the volatilized ammonia gas is condensed into liquid ammonia for returning; or the cleaning zone is directly cooled once to

Ammonia gas is condensed into liquid ammonia at the temperature of between 34 and 77 ℃ below zero and flows back to the reaction tank, so that the utilization rate of the liquid ammonia is improved;

step eight, taking out a TiNx product:

the whole working environment is an oxygen-free and low-temperature area and nitrogen charging, and an intermediate buffer area needs to be established to ensure that the oxygen-free and low-temperature reaction environment cannot be damaged when the product is moved out of the reaction area; the method for preparing the titanium nitride section by utilizing the solid titanium tetrachloride and the low-temperature liquid ammonia is formed.

Further, titanium tetrachloride is used as the main raw material, and the titanium tetrachloride is pre-cooled to a temperature close to the melting point of-24.1 ℃.

Furthermore, the reaction area is a pure nitrogen, oxygen-free and low-temperature area, and the temperature parameter of the molding environment is-34 ℃ to-77.5 ℃.

Further, the liquid ammonia is arranged in a reaction tank according to the designed product size, and the temperature of the reaction tank is stabilized to about-70 ℃ as far as possible.

Furthermore, a layer of wax-coated or film-precoated paper or other sheet materials capable of being repeatedly folded is paved on the low-temperature forming inclined plane in advance, so that the prefabricated titanium tetrachloride section bar can be conveniently demoulded by the sucker.

The beneficial technical effects of the invention are as follows:

The invention mainly adopts the reaction of titanium tetrachloride and ammonia to prepare titanium nitride (i.e. TiCl)₄ +NH₃ →TiNx+NH₄ Cl ↓, the temperature condition can be unlimited) to discontinuously prepare titanium nitride and titanium nitride sectional materials, thus realizing the environmental protection and low-cost production of titanium nitride and titanium nitride sectional materials. Under the conditions of no oxygen, nitrogen filling and low temperature of-34 to-77.5 ℃, titanium tetrachloride is condensed, prefabricated and molded on a molding machine and slowly inserted into a reaction tank filled with liquid ammonia, and the following reactions are completed by using the titanium tetrachloride and the liquid ammonia: tiCl (titanium dioxide)₄ +NH₃ →TiNx+NH₄ Cl, the value of X is changed differently under the conditions of different thicknesses, different submergence speeds and different reaction temperatures, the method for preparing the titanium nitride has low cost, no external heat source is needed in the reaction, no three wastes are left, multiple effects of environmental protection, high resource utilization rate and less energy consumption are brought, and particularly continuous production can be realized, the productivity is greatly increased, and the cost is further reduced. The defects of the prior art are overcome.

Drawings

FIG. 1 is a flow chart of the process for preparing titanium nitride by reacting titanium tetrachloride with ammonia according to the present invention.

FIG. 2 is a process flow diagram of the preparation of titanium nitride section bar by using solid titanium tetrachloride and liquid ammonia according to the present invention.

Detailed Description

The invention will be better understood by the following description of embodiments thereof, but the applicant is not aware of the specific embodiments thereof, which should be considered as limiting the technical solution of the invention, and any changes in the definition of parts or technical features and/or in the form of a whole structure without substantial alterations should be considered as a protection scope defined by the technical solution of the invention.

The embodiment is as follows:

example one

As shown in fig. 1-2, a method for preparing a titanium nitride profile by using solid titanium tetrachloride and low-temperature liquid ammonia is characterized in that:

the method for preparing the titanium nitride section by utilizing the solid titanium tetrachloride and the low-temperature liquid ammonia adopts the reaction of titanium tetrachloride and ammonia to prepare titanium nitride under the anaerobic condition, and meets the chemical equation: tiCl (titanium dioxide)₄ +NH₃ →TiNx+NH₄ Cl ↓solution, in order to avoid overhigh temperature and energy waste, the reaction temperature is controlled within the range of normal temperature to-77.5 ℃; in order to ensure continuous production, the melting point difference between the melting point of liquid ammonia at minus 77.75 ℃ and the melting point of titanium tetrachloride at minus 24.1 ℃ is utilized, the synthesized titanium tetrachloride is properly cooled to be more than minus 20 ℃ under the conditions of no oxygen and low temperature, the titanium tetrachloride is added into film-making equipment at minus 34 ℃ to minus 77.5 ℃ for rapid solidification, the titanium tetrachloride is prepared into a required shape, at least comprises a thin plate, a thin wire and a special shape, the solid-state formed titanium tetrachloride is combined with liquid ammonia, a single piece of the solid-state formed titanium tetrachloride is slowly inserted into a liquid ammonia tank, and on one hand, the titanium tetrachloride can be quantitatively added to control the reaction temperature; on the other hand, to stabilize the set pattern of the solid-state titanium tetrachloride, since TiCl₄ +NH₃ →TiNx+NH₄ Emitting a large amount of heat in the reaction process of Cl ↓, causing liquid ammonia and titanium tetrachloride to vaporize, unable to keep the titanium atom stable structure of titanium tetrachloride, producing the TiNx product of the design, controlling the low temperature-34 ℃ -77.5 ℃, under the condition of being lower than the boiling point of liquid ammonia-33.5 ℃, titanium tetrachloride is solidified into thin slices, the titanium atom is in the three-dimensional structure, when the titanium tetrachloride single piece is slowly added, the titanium tetrachloride single piece can move in a liquid ammonia tank so as to avoid overhigh local temperature, the generated TiNx still keeps the original form, is thinned and in a low-temperature state, and the liquid ammonia in a liquid state reacts with the sheet titanium tetrachloride so as not to cause overhigh local temperature and change the existing form of the TiNx;

the method for preparing the TiNx also comprises the following steps:

step one, creating an oxygen-free dry reaction area:

step two, establishing a low-temperature reaction area:

step three, manufacturing titanium tetrachloride curing molding equipment:

step four, curing and molding titanium tetrachloride:

step five, reaction control:

step six, extraction and cleaning of reaction smoke dust:

reaction product NH₄ The Cl ↓ reaction process exists in a gas state, so that the Cl ↓ is prevented from being solidified and sinking to enter a reaction tank, and the descending of the reaction is prevented; an exhaust fan is arranged on one side of the upper end of the reaction tank, a collector is arranged on the rear side of the exhaust fan, and NH is timely discharged₄ Cl ↓ [ grain ] smoke and dust are pumped away, condensed in the collector, and liquid ammonia is supplemented at regular time, so that the depth of the reaction tank is stabilized in a certain area, and NH which cannot be pumped away at the bottom of the reaction tank is cleaned regularly₄ Cl ↓precipitate;

step seven, cleaning TiNx forming finished products:

the surface of the TiNx section taken out from the liquid ammonia reaction tank is adhered with certain liquid ammonia, the TiNx section is transferred to a region with the temperature of more than minus 33.5 ℃ for volatilization and cleaning, volatilized ammonia gas is periodically pumped back to the lower-end low-temperature region at minus 34 ℃ to minus 77 ℃, and the volatilized ammonia gas is condensed into liquid ammonia to be returned for use; or the cleaning area is directly cooled to minus 34 ℃ to minus 77 ℃ once, ammonia gas is condensed into liquid ammonia and flows back to the reaction tank, and the utilization rate of the liquid ammonia is improved;

step eight, taking out a TiNx product:

the whole operation environment is an oxygen-free and low-temperature area and nitrogen is filled, and an intermediate buffer area needs to be established to ensure that the oxygen-free and low-temperature reaction environment cannot be damaged when the product is moved out of the reaction area; the method for preparing the titanium nitride section by utilizing the solid titanium tetrachloride and the low-temperature liquid ammonia is formed.

Furthermore, a layer of wax-coated or film-precoated paper or other sheet materials capable of being repeatedly folded should be paved on the low-temperature forming inclined plane in advance, so that the prefabricated titanium tetrachloride section bar can be conveniently demoulded by the suction cup.

Example two

As shown in fig. 1-2, the fabricated reaction kettle is fixed, the discharge port of the reaction kettle and a titanium tetrachloride nozzle valve are closed, the exhaust hole of the reaction kettle is opened to introduce ammonia gas vaporized from liquid ammonia into the reaction kettle, when the PH test paper of the exhaust hole shows blue, the result shows that the air in the reaction kettle is completely exhausted, the reaction kettle is filled with ammonia gas, the exhaust hole is closed, the ammonia gas is continuously introduced, when the pressure gauge at the side shows 1.5 standard atmospheric pressures, the result shows that the reaction kettle is filled with ammonia gas, and the ammonia gas inlet valve is closed; extracting titanium tetrachloride liquid from a titanium tetrachloride storage bottle by using an extractor with a long suction tube, wherein the titanium tetrachloride liquid consists of TiCl as a chemical component₄ 98.8％、VCl_x 0.21％,CaCl₂ 0.33％,MgCl₂ 0.146％,NaCl0.15％.SiClx0.12％,FeCl₂ 0.203%) from titanium tetrachloride into the tubeTitanium tetrachloride is sprayed into the upper part of the reaction kettle in proportion, because partial oxygen is remained, red and yellow deposits are rapidly formed on the inner wall of the kettle, the temperature in the kettle is rapidly raised, and the temperature is controlled within a specific range (less than 600 ℃). When the external temperature of the reaction kettle is reduced to about 60 ℃, supplementing ammonia gas, spraying titanium tetrachloride, repeating for three times, stopping adding when more reactants are deposited on the inner wall of the reaction kettle, and opening a discharge hole of the reaction kettle when the outer wall of the reaction kettle is reduced to below 30 ℃.

Water dissolving and separating: adding water into the reaction kettle according to the solubility of ammonium chloride at normal temperature, and pouring out a reaction product in a flushing mode, wherein otherwise, the product has large adhesive force on the inner wall, and the mechanical separation is difficult and incomplete; filtering the slurry after water dissolution, and delivering the filtrate to a concentration link to obtain ammonium chloride crystals which are used as ammonia recovery raw materials for alkalization treatment for later use; the filter cake was washed three additional times with water, and the washing solution was used as the lower solution.

Drying titanium nitride: in this case, the titanium nitride is unstable in properties, and the drying temperature is controlled to 300 ℃ or lower, so that high-temperature nitriding treatment is required to obtain stable titanium nitride.

EXAMPLE III

As shown in FIGS. 1-2, the whole reaction is carried out in a horizontal refrigerator capable of cooling to-80 deg.C, the temperature can be adjusted according to the test requirements

The titanium tetrachloride is prepared in 30 g and the composition is (the chemical component is TiCl)₄ 98.8％、VCl_x 0.21％,CaCl₂ 0.33％,MgCl₂ 0.146％,NaCl0.15％.SiClx0.12％,FeCl₂ 0.203 percent), a small reaction chamber made of polyvinyl chloride film, a transparent plastic box as a reaction tank, a mould for preparing titanium tetrachloride sheets and the transparent plastic box are firstly placed in the polyvinyl chloride film, then the fire float is melted, the opening is sealed, the air valve is bonded, the reaction chamber is a perspective space, because of the soft body, the polyvinyl chloride film can be externally operated, the two sides which are vacuumized are tightly attached together, then nitrogen is filled in the reaction chamber to expand and bulge to form a reaction space, the titanium tetrachloride is filled into an intermediate storage device made of an infusion liquid bag in advance, the reaction chamber model and the storage device are placed in a refrigerator together, the temperature of the refrigerator is-40 ℃, and the mould (the width of which is 20 m) made of thin steel plates is used at the early stage (the temperature of the refrigerator is-40℃)m, 30mm in length and 3mm in thickness), putting a cotton string in advance, and taking the sheet out of the die through a thin cotton thread solidified in the sheet when the titanium tetrachloride extruded into the die is condensed into the sheet; and (3) continuously cooling the small reaction chamber, when the temperature of the refrigerated cabinet reaches-70 ℃, injecting 500 g of liquid ammonia at the same temperature of (-40 ℃) into a plastic reaction tank (with the length of 50mm, the width of 50mm and the depth of 50 mm) in the reaction chamber, putting the prepared titanium tetrachloride slice into the liquid ammonia reaction tank through a fine cotton thread, slowly sinking the titanium tetrachloride slice into the liquid ammonia reaction tank, generating a small amount of smoke, and obviously reducing the reaction speed. After fifteen minutes of reaction, stopping heat preservation, and when the temperature of the refrigerating chamber is restored to-40 ℃, pouring redundant liquid ammonia into a liquid ammonia bottle of a refrigerating cabinet, wherein the temperature is-40 ℃, and the ammonia is still liquid; opening the refrigerated cabinet, and moving the small reaction chamber out of the refrigerated cabinet; the reaction tank is placed for 1 hour at normal temperature, the plastic reaction tank is taken out, the sheet shape of the titanium tetrachloride is still maintained, the sheet is cleaned and naturally dried to obtain about 4.5 g of titanium nitride sheets, the reaction conditions are relatively harsh, the titanium nitride sheets can be cooled to-80 ℃ and can only be provided by a vendor, and the experiment can be implemented with the appearance of small-sized refrigeration equipment.

The implementation of the method for preparing the titanium nitride section by utilizing the solid titanium tetrachloride and the low-temperature liquid ammonia is completed.

The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it is therefore intended that all such changes and modifications as fall within the true spirit and scope of the invention be considered as within the following claims.

Claims

1. A method for preparing a titanium nitride section by utilizing solid titanium tetrachloride and low-temperature liquid ammonia is characterized by comprising the following steps:

the method for preparing the titanium nitride section by utilizing the solid titanium tetrachloride and the low-temperature liquid ammonia adopts the reaction of titanium tetrachloride and ammonia to prepare titanium nitride under the anaerobic condition, and meets the chemical equation:

TiCl₄ +NH₃ →TiNx+NH₄ cl ↓, in order to avoid the over-high temperature and the energy waste, the reaction temperature is controlled from normal temperature to-77.5 ℃ or less; in order to ensure continuous production, the melting point difference between the melting point of liquid ammonia at minus 77.75 ℃ and the melting point of titanium tetrachloride at minus 24.1 ℃ is utilized, the synthesized titanium tetrachloride is properly cooled to be more than minus 20 ℃ under the conditions of no oxygen and low temperature, the titanium tetrachloride is added into film-making equipment at minus 34 ℃ to minus 77.5 ℃ for rapid solidification, the titanium tetrachloride is prepared into a required shape, at least comprises a thin plate, a thin wire and a special shape, the solid-state formed titanium tetrachloride is combined with liquid ammonia, a single piece of the solid-state formed titanium tetrachloride is slowly inserted into a liquid ammonia tank, and on one hand, the titanium tetrachloride can be quantitatively added to control the reaction temperature; on the other hand, to stabilize the set pattern of the solid-state titanium tetrachloride, since TiCl₄ +NH₃ →TiNx+NH₄ Emitting a large amount of heat in the Cl ≠ reaction process to cause vaporization of liquid ammonia and titanium tetrachloride, being incapable of keeping a titanium atom stable structure of the titanium tetrachloride, producing a shaped TiNx product, controlling the temperature to be-34 to-77.5 ℃, solidifying the titanium tetrachloride into a sheet under the condition that the temperature is lower than the boiling point of the liquid ammonia to be-33.5 ℃, wherein the titanium atom is in a three-dimensional structure, when the titanium tetrachloride single sheet is slowly added, the titanium tetrachloride single sheet can also move in a liquid ammonia pool to avoid overhigh local temperature, the generated TiNx still keeps the original shape, and the TiNx is thinned, thinned and in a low-temperature state, and the liquid ammonia in a liquid state and the sheet titanium tetrachloride react to not cause overhigh local temperature and change the existing shape of the TiNx;

step one, creating an oxygen-free dry reaction area:

step two, establishing a low-temperature reaction area:

step three, manufacturing titanium tetrachloride curing molding equipment:

the solidification of titanium tetrachloride is finished in a film forming device or a special-shaped device, the film forming device is in a shape of a side vertical triangle of a solar water heater, the upper end of the film forming device is provided with a constant volume transverse groove, one side of the constant volume transverse groove is provided with a low-temperature forming inclined plane, one side of the constant volume transverse groove close to the low-temperature forming inclined plane is provided with a uniform slit or a point hole, the slit can condense the titanium tetrachloride leaked downwards on a forming surface into a thin plate, the point hole condenses the titanium tetrachloride leaked downwards into the design shapes of filaments, strips and the like, the working temperature is an upper limit area of minus 34 ℃ to minus 77.5 ℃, the constant volume transverse groove at the upper end is designed according to the width and the depth of a reaction tank and can be properly adjusted, the smaller the temperature difference is, the longer the flow is, and the shape of the titanium tetrachloride with the same quantity is longer and thinner;

step four, curing and molding titanium tetrachloride:

step five, reaction control:

in order to ensure that the reaction reaches the expected temperature, the temperature is between minus 34 ℃ and minus 77.5 ℃, the ambient temperature is as close to the lower limit or the lower area of the temperature area as possible, the titanium tetrachloride single plate is gradually and downwards inserted into the liquid ammonia tank in a descending way due to the large heat release of the reaction, the descending speed cannot be too fast, and the descending speed is adjusted due to the high and low ambient temperature and the thickness of the solid titanium tetrachloride plate;

step six, extraction and cleaning of reaction smoke dust:

reaction product NH₄ The Cl ↓ reaction process exists in a gas state, so that the Cl ↓ is prevented from being solidified and sinking to enter a reaction tank, and the descending of the reaction is prevented; an exhaust fan is arranged on one side of the upper end of the reaction tank, a collector is arranged on the rear side of the exhaust fan, and NH is timely discharged₄ Cl ↓ ] smoke dust is pumped away, condensed in the collector, and liquid ammonia is supplemented at regular time, so that the depth of the reaction tank is stabilized in a certain area, and NH which cannot be pumped away at the bottom of the reaction tank is cleaned regularly₄ Cl ↓precipitate;

step seven, cleaning a TiNx molding finished product:

step eight, taking out a TiNx product:

2. The method of claim 1, wherein titanium tetrachloride is used as the main raw material, and the titanium tetrachloride is pre-cooled to a temperature near the melting point of-24.1 ℃.

3. The method for preparing the titanium nitride section bar by utilizing the solid titanium tetrachloride and the low-temperature liquid ammonia according to the claim 1, wherein the reaction area is a pure nitrogen and oxygen-free low-temperature area, and the temperature parameter of the molding environment is-34 ℃ to-77.5 ℃.

4. The method for preparing titanium nitride sectional material by using solid titanium tetrachloride and low-temperature liquid ammonia according to claim 1, wherein the liquid ammonia is contained in a reaction tank according to the designed product size, and the temperature of the reaction tank is stabilized as much as possible at about-70 ℃.

5. The method for preparing the titanium nitride section bar by utilizing the solid titanium tetrachloride and the low-temperature liquid ammonia as claimed in claim 1, wherein a layer of wax-coated or pre-coated paper or other repeatedly foldable sheet materials is paved on the low-temperature forming inclined plane in advance, so that the prefabricated titanium tetrachloride section bar can be conveniently demoulded by a sucking disc.