Sponge titanium distillation process control system and control method

Abstract

The invention relates to the technical field of sponge titanium production, in particular to a sponge titanium distillation process control system and method. A titanium sponge distillation process control system comprises a distiller, a condenser, an electric distillation furnace and a vacuum unit. The system further comprises a distiller pressure detection control unit, a distiller temperature detection control unit, a condenser pressure detection control unit, a condenser temperature detection control unit, a vacuum unit detection control unit, a man-machine interaction system and a DCS control system. According to the sponge titanium distillation process control system provided by the invention, the DCS is utilized to cooperate with the distiller pressure detection control unit, the distiller temperature detection control unit, the condenser pressure detection control unit, the condenser temperature detection control unit, the vacuum unit detection control unit and the man-machine interaction system; and key process parameters of distillation are monitored and accurately controlled, so that the method has a remarkable effect on improving the quality of the sponge titanium.

Description

Technical Field

[0001] The present invention relates to the technical field of titanium sponge production, and in particular to a titanium sponge distillation process control system and a control method. Background Art

[0002] Titanium and titanium alloys have the characteristics of high specific strength, corrosion resistance, and good high temperature resistance. They are widely used in aerospace, deep sea exploration, chemical industry, medical and other fields. Sponge titanium is the raw material for the preparation of titanium and titanium alloys. It is only prepared by magnesium thermal method in industry. Magnesium reduction of TiCl 4 The reactor after the reaction is left with excess magnesium and the reduction byproduct MgCl 2 In order to obtain pure titanium sponge, the industry generally uses vacuum distillation to separate Mg / MgCl 2 Separate from sponge titanium. During the vacuum distillation of sponge titanium, key parameters such as distiller temperature, distiller vacuum, condenser condensation strength, vacuum unit switching, and distillation cycle need to be controlled. When process parameters deviate, the quality of sponge titanium will be seriously affected. For example, when the distillation cycle is not properly controlled, a high level of chlorine impurities may remain in the sponge titanium; if the distiller temperature is too high, the shrinkage of the sponge titanium will intensify, and the content of impurities such as Fe in the sponge titanium will also increase.

[0003] In order to accurately and automatically control the key process parameters of the reduction process, domestic titanium sponge enterprises use advanced distributed control systems (Distributed control system) to solve the adverse effects of key process parameter deviations on the quality of titanium sponge. Chinese utility model patent CN215376162U discloses a control system for titanium sponge DSC system. This patent has the functions of automatic feeding of reactor, automatic adjustment of reaction pressure, and automatic control of wall temperature during the reduction process; the distillation stage has the functions of temperature control of the distiller, condenser cooling intensity regulation, and automatic loosening of the middle aisle; the cooling stage can spray water cooling and automatic argon filling of the reactor. Chinese utility model patent CN216144195U discloses a condenser temperature control system. This patent uses a DSC system to realize the temperature monitoring and flow rate automatic adjustment of the condensed water of the condenser during the vacuum distillation stage of titanium sponge. Chinese invention patent application CN115857448A discloses a method for online monitoring of process parameters of titanium sponge production process, by placing data collectors at different positions of the titanium making furnace; and calculating the process index compliance and equipment index compliance, and judging whether the titanium sponge production process is running stably.

[0004] During the titanium sponge distillation process, due to the Mg / MgCl 2There are differences in the residual amount, so the pressure conditions of different distiller often differ. In addition, under different pressure conditions of the distiller, the vacuum pump's suction capacity and the amount of volatiles in the condenser are different, so it is necessary to constantly adjust the condensation strength of the condenser and switch the vacuum unit. Therefore, accurate and automatic control of distillation process parameters is of great significance to improving distillation production efficiency and ensuring the quality of titanium sponge. Summary of the invention

[0005] In view of this, the present invention provides a titanium sponge distillation process control system and control method, which can specifically solve the technical problem that the distillation process parameters are difficult to control in the prior art.

[0006] The first aspect of the present invention provides a titanium sponge distillation process control system, comprising a distiller, a condenser, a distillation electric furnace for heating the distiller, and a vacuum unit connected to the condenser. It also comprises: a distiller pressure detection control unit and a distiller temperature detection control unit arranged on the distiller, a condenser pressure detection control unit and a condenser temperature detection control unit arranged on the condenser, and a vacuum unit detection control unit arranged on the vacuum unit; A titanium sponge distillation process control system further comprises: A human-computer interaction system configured to set a distiller working pressure, a distiller working temperature, a condenser internal working pressure, and a condenser internal working temperature; The DCS control system is configured to receive detection values ​​fed back by the distiller pressure detection control unit, the distiller temperature detection control unit, the condenser pressure detection control unit, and the condenser temperature detection control unit, and to regulate the process parameters of the distiller, condenser, and vacuum unit based on the distiller working pressure, distiller working temperature, condenser internal working pressure, and condenser internal working temperature set in the human-computer interaction system.

[0007] In some embodiments, the vacuum unit includes a low vacuum unit and a high vacuum unit arranged in parallel; the low vacuum unit and the high vacuum unit are connected through a vacuum pipeline and connected to a condenser, and the vacuum unit detection control unit includes a first vacuum gauge and a remote automatic pneumatic valve arranged on the vacuum pipeline.

[0008] In some embodiments, the distiller pressure detection control unit includes a second vacuum gauge, a first automatic argon filling valve, and a first automatic argon release valve that are connected to the DCS control system in communication; wherein the second vacuum gauge is installed in the vacuum system of the distiller to monitor the gas pressure in the distiller in real time; the first automatic argon filling valve is installed on the air inlet pipe of the distiller to control the flow rate and timing of argon entering the distiller. The first automatic argon release valve is installed on the air outlet pipe of the distiller to control the gas discharge in the distiller.

[0009] In some embodiments, the temperature detection control unit of the distiller includes a thermocouple and a power regulator that are communicatively connected to the DCS control system, and the thermocouples are arranged in 5 to 6 groups longitudinally along the outer wall of the distiller, and each group includes 2 to 4 thermocouples uniformly arranged longitudinally. The power regulator is installed on the distillation electric furnace to adjust the heating power of the distillation electric furnace.

[0010] In some embodiments, the condenser pressure detection control unit includes a third vacuum gauge, a second automatic argon filling valve, and a second automatic argon release valve that are communicatively connected to the DCS control system. The third vacuum gauge is installed on the condenser. The second automatic argon filling valve is installed on the air inlet pipe of the condenser. The second automatic argon release valve is installed on the air outlet pipe of the condenser.

[0011] In some embodiments, the condenser temperature detection control unit includes a condenser water flow remote control valve, a water inlet temperature detection thermocouple, and a water outlet temperature detection thermocouple that are connected to the DCS control system for communication. The condenser water flow remote control valve is installed on the water inlet pipe of the condenser. The water inlet temperature detection thermocouple is installed on the water inlet pipe of the condenser. The water outlet temperature detection thermocouple is installed on the water outlet pipe of the condenser; wherein the condenser is a vertical shell and tube condenser, and its cooling water inlet is arranged at the top of the condenser.

[0012] In some embodiments, the vacuum pump of the low vacuum unit is a first slide valve pump, and the vacuum pump of the high vacuum unit is a combination of a second slide valve pump and an oil booster pump.

[0013] A second aspect of the present invention provides a method for controlling a titanium sponge distillation process, comprising the following steps: S1, initial stage: the staff sets the distiller working pressure, distiller working temperature, condenser internal working pressure and condenser internal working temperature; S2, reduction stage: turning on the distillation electric furnace, heating the distillation electric furnace according to the set distiller working temperature, and performing a reduction process on the raw materials in the distiller; S3, distillation stage: real-time detection of the pressure inside the distiller, the temperature inside the distiller, the pressure inside the condenser, and the temperature inside the condenser, and control of the process parameters of the distiller, condenser and vacuum unit based on the set distiller working pressure, distiller working temperature, condenser working pressure and condenser working temperature.

[0014] In some embodiments, in step S2, the reduction stage further comprises: when the pressure in the distiller is 10 5 ~50Pa, turn on the low vacuum unit to evacuate air; when the distiller pressure is 50Pa~1Pa, turn on the high vacuum unit to evacuate air.

[0015] In some embodiments, in step S3, the distillation stage further comprises: S31, regulating the pressure in the distiller: when it is detected that the pressure in the distiller is greater than 100Pa and the pressure drop rate is less than 2Pa / h, or when the pressure in the distiller is 100~10Pa and the pressure drop rate is less than 0.5Pa / h, or when the pressure in the distiller is less than 1Pa but the pressure in the distiller gradually increases, the distiller pressure is judged to be in an abnormal state, the vacuum unit is controlled to be shut down, and the distiller is filled with argon and tested for air tightness.

[0016] In some embodiments, in step S3, the distillation stage further comprises: S32, regulating the temperature in the distiller: when the distiller pressure is 10 5 ~100Pa, control the distiller temperature at 950~955℃; when the distillation pressure is 100~1Pa, control the distiller temperature at 1000~1005℃.

[0017] In some embodiments, in step S3, the distillation stage further comprises: S33, regulating the pressure in the condenser: when it is detected that the pressure in the condenser is greater than 100Pa and the pressure drop rate is less than 2Pa / h, or when the condenser pressure is 100~10Pa and the pressure drop rate is less than 0.5Pa / h, or when the condenser pressure is less than 1Pa but the condenser pressure rises, the condenser pressure is judged to be abnormal, the vacuum unit is controlled to be shut down, and the condenser is given argon filling and air tightness detection instructions.

[0018] In some embodiments, in step S3, the distillation stage further comprises: S34, regulating the temperature inside the condenser: controlling the inlet temperature of the cooling water on the condenser to be less than or equal to 25°C, and the outlet temperature of the cooling water to be 55°C~60°C.

[0019] In some embodiments, the titanium sponge distillation process control method further includes step S35: distillation cycle control: When the pressure values ​​of the distiller and condenser are less than 1Pa, and the duration of the distiller pressure being less than 10Pa exceeds the preset time, the distillation is terminated; When the pressure value of the distiller and the condenser is greater than or equal to 1Pa, or the duration of the distiller pressure being less than 10Pa is less than the preset time, the distillation cycle is controlled according to the preset cycle.

[0020] In some embodiments, the titanium sponge distillation process control method further includes step S4, a cooling stage: monitoring the pressure of the distiller and the condenser, and when the pressure of the distiller and the condenser is lower than 5 kPa, filling the distiller and the condenser with argon; when the pressure reaches above 15 kPa, stopping the argon filling.

[0021] The beneficial effects of the present invention are as follows: a titanium sponge distillation process control system provided by the present invention utilizes the coordinated effects of a DCS control system, a distiller pressure detection control unit, a distiller temperature detection control unit, a condenser pressure detection control unit, a condenser temperature detection control unit and a human-computer interaction system to monitor and precisely control key process parameters of distillation, which has a significant effect on improving the quality of titanium sponge. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention. For ordinary technicians in this field, other embodiments can be obtained based on these drawings without paying creative work.

[0023] Figure 1 A logic diagram of a titanium sponge distillation process control system provided by one embodiment of the present invention; Figure 2 A schematic structural diagram of a distiller and a condenser and their accessory components provided for one embodiment of the present invention.

[0024] Description of reference numerals: 101. Thermocouple for detecting water inlet temperature; 102. Thermocouple for detecting water outlet temperature; 103. Remote control valve for condensate flow; 104. Condenser; 105. Second automatic argon release valve; 201. Distiller; 202. Second vacuum gauge; 203. First automatic argon filling valve; 204. Third vacuum gauge; 205. Second automatic argon filling valve; 301. First vacuum gauge; 302. First remote automatic pneumatic valve; 303. Third remote automatic pneumatic valve; 304. Oil booster pump; 305. Second slide valve pump; 306. Second remote automatic pneumatic valve; 307. First slide valve pump; 401. Distillation furnace; 402. Thermocouple; 403. Power regulator. DETAILED DESCRIPTION

[0025] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the embodiments of the present invention are further described in detail below in combination with specific embodiments and with reference to the accompanying drawings.

[0026] It should be noted that all expressions using "first" and "second" in the embodiments of the present invention are for distinguishing two non-identical entities with the same name or non-identical parameters. It can be seen that "first" and "second" are only for the convenience of expression and should not be understood as limitations on the embodiments of the present invention. The subsequent embodiments will not explain this one by one.

[0027] The first aspect of the present invention proposes a titanium sponge distillation process control system, comprising a distiller 201, a condenser 104, a distillation electric furnace 401 for heating the distiller 201, and a vacuum unit connected to the condenser 104. The distiller 201 is used to receive the product after the reduction reaction (mainly a mixture of titanium, magnesium and magnesium chloride), and separate high-purity titanium sponge through a vacuum distillation process. The condenser 104 is connected to the top of the distiller 201, and is used to cool and condense the gas evaporated from the distiller 201 to achieve the separation of metallic titanium from other impurities. The distillation electric furnace 401 is used to heat the distiller 201 and provide the necessary temperature conditions to promote the evaporation and separation process of the substance. The vacuum unit is connected to the condenser 104 to maintain the vacuum state of the system, ensure the smooth progress of the distillation process, and prevent the outside air from affecting the product quality.

[0028] A titanium sponge distillation process control system also includes: a distiller pressure detection control unit and a distiller temperature detection control unit arranged on the distiller 201, a condenser pressure detection control unit and a condenser temperature detection control unit arranged on the condenser 104, and a vacuum unit detection control unit arranged on the vacuum unit; the distiller pressure detection control unit is used to monitor the pressure inside the distiller 201, ensure that the distillation process is carried out under a suitable pressure, and provide necessary data for temperature control. The distiller temperature detection control unit is used to measure the temperature of the distiller 201 in real time to ensure that the heating process is uniform and avoid overheating. The condenser pressure detection control unit is used to monitor the pressure state inside the condenser 104, ensure the safe operation of the system, and adjust the condensation efficiency in time. The condenser temperature detection control unit is used to monitor the temperature of the condenser 104, ensure that titanium metal is effectively separated from other impurities, and improve the purity of the product. The vacuum unit detection control unit is used to control the start and stop and operation state of the vacuum unit, and adjust the working efficiency of the vacuum pump according to the real-time data of the system pressure and temperature.

[0029] A titanium sponge distillation process control system of the present application further comprises: The human-computer interaction system is configured to set the working pressure of the distiller 201, the working temperature of the distiller 201, the working pressure in the condenser 104, and the working temperature in the condenser 104; specifically, the human-computer interaction system is directly connected to each detection unit through a dedicated data transmission line to achieve fast and accurate data transmission. The human-computer interaction system can be a microcomputer, which has the functions of setting process parameters, feedback of parameters, access to historical process data, monitoring of the operating status of process parameters, and abnormal parameter alarms.

[0030] The DCS control system is configured to receive the detection values ​​fed back by the distiller pressure detection control unit, the distiller temperature detection control unit, the condenser pressure detection control unit, and the condenser temperature detection control unit, and to adjust the process parameters of the distiller 201, the condenser 104, and the vacuum unit based on the distiller 201 working pressure, the distiller 201 working temperature, the condenser 104 working pressure, and the condenser 104 working temperature set in the human-computer interaction system. The DCS control system is used to control the execution of steps S31 to S35 and step S4 to be described below. Specifically, the DCS control system (Distributed control system) is a centralized distributed control system based on a microprocessor for centralized monitoring, operation, management, and decentralized control of the production process. The system applies several microcomputers to process control in a decentralized manner. All information is monitored by the upper management computer through the communication network to achieve optimal control. The entire device inherits the advantages of conventional instrument decentralized control and computer centralized control, and overcomes the shortcomings of conventional instruments with single functions, poor human-machine communication and highly concentrated dangers of a single microcomputer control system. It achieves both centralization in management, operation and display, and decentralization in function, load and danger.

[0031] The first aspect of the present application provides a titanium sponge distillation process control system that utilizes a DCS control system in collaboration with a distiller pressure detection control unit, a distiller temperature detection control unit, a condenser pressure detection control unit, a condenser temperature detection control unit, and a human-computer interaction system to monitor and precisely control key process parameters of distillation, which has a significant effect on improving the quality of titanium sponge.

[0032] In some embodiments, the vacuum unit includes a low vacuum unit and a high vacuum unit arranged in parallel; the low vacuum unit and the high vacuum unit are connected through a vacuum pipeline and connected to the condenser 104, and the vacuum unit detection control unit includes a first vacuum gauge 301 and a remote automatic pneumatic valve arranged on the vacuum pipeline and connected to the DCS control system for communication. Specifically, the vacuum pipeline includes two branches corresponding to the low vacuum unit and the high vacuum unit respectively, and a main line connecting the two branches and connected to the condenser 104, and the two branches and the main line are both provided with remote automatic pneumatic valves, such as Figure 2As shown, the remote automatic pneumatic valve set on the main line is the first remote automatic pneumatic valve 302, the remote automatic pneumatic valve set on the low vacuum unit is the second remote automatic pneumatic valve 306, and the remote automatic pneumatic valve set on the high vacuum unit is the third remote automatic pneumatic valve 303. Different vacuum units have different working pressures. The working pressure range of the low vacuum unit is 50-101325Pa, with high working pressure and large exhaust volume, but relatively low pumping speed. It is mainly used for initial vacuum establishment and rapid exhaust under atmospheric pressure. The vacuum unit of the high vacuum unit has a lower working pressure (0.1Pa-50Pa), a small exhaust volume, and a high pumping speed, which is suitable for maintaining a low-pressure high vacuum environment. The first vacuum gauge 301 is used to monitor the vacuum degree in the vacuum pipeline in real time and provide the operator with accurate pressure data to adjust the operation of the vacuum unit. The first remote automatic pneumatic valve 302 installed on the main line is used to automatically adjust according to the data of the first vacuum gauge 301, control the gas flow and vacuum degree, and ensure the efficient and safe operation of the system. The second remote automatic pneumatic valve 306 and the third remote automatic pneumatic valve 303 installed on the branch line are used to control the opening and closing of the low vacuum unit and the high vacuum unit respectively. The low vacuum unit and the high vacuum unit are connected in parallel, and can be operated independently or simultaneously according to actual needs, thereby improving the flexibility and efficiency of the system. Through the vacuum pipeline, both the high and low vacuum units are connected to the condenser 104, effectively maintaining and controlling the vacuum state of the condenser 104, and optimizing the distillation process of sponge titanium.

[0033] In some embodiments, the distiller pressure detection control unit includes a second vacuum gauge 202, a first automatic argon filling valve 203, and a first automatic argon release valve that are connected to the DCS control system in communication; wherein the second vacuum gauge 202 is installed in the vacuum system of the distiller 201 to monitor the gas pressure in the distiller 201 in real time, and provide the operator with necessary data support to ensure that the distillation process is carried out under a suitable pressure. The first automatic argon filling valve 203 is installed on the air inlet pipe of the distiller 201 to control the flow rate and timing of argon entering the distiller 201. Argon, as a protective gas, can prevent oxidation reactions during the distillation process and plays an important role in improving product quality. The first automatic argon release valve is installed on the air outlet pipe of the distiller 201 to control the gas discharge in the distiller 201. The first automatic argon release valve can be automatically adjusted according to the real-time monitoring data of the system pressure to maintain the balance of pressure in the system. Through this configuration, the working status of these detection units can be monitored in real time and transmitted to the DCS control system, so that the DCS control system can adjust parameters or operating instructions as needed to achieve fine control of the distillation process, thereby optimizing the production process.

[0034] In some embodiments, the distiller temperature detection control unit includes a thermocouple 402 and a power regulator 403 that are communicatively connected to the DCS control system. The thermocouple 402 is longitudinally arranged in 5 to 6 groups along the outer wall of the distiller 201, and each group includes 2 to 4 thermocouples 402 evenly arranged along the longitudinal direction. The temperature distribution of the outer wall of the distiller 201 can be monitored more comprehensively and finely, thereby more accurately reflecting the actual temperature conditions inside the distiller 201. The power regulator 403 is installed on the distillation furnace 401 to adjust the heating power of the distillation furnace 401. When in use, the thermocouple 402 transmits the detected temperature data to the DCS control system. The DCS control system adjusts the heating power of the distillation furnace 401 based on the temperature data provided by the thermocouple 402 and through the power regulator 403, thereby achieving precise control of the temperature of the distillation process and ensuring that the distillation process is carried out at the optimal temperature.

[0035] In some embodiments, the condenser pressure detection control unit includes a third vacuum gauge 204, a second automatic argon filling valve 205, and a second automatic argon release valve 105 that are communicatively connected to the DCS control system. The third vacuum gauge 204 is installed on the condenser 104 to monitor the vacuum degree, i.e., the gas pressure, in the condenser 104 in real time. The second automatic argon filling valve 205 is installed on the air inlet pipe of the condenser 104 to control the inflow of argon gas. The second automatic argon release valve 105 is installed on the air outlet pipe of the condenser 104 to control the discharge of gas. Through this configuration, the working status of these detection units can be monitored in real time and transmitted to the DCS control system, so that the DCS control system can adjust parameters or operating instructions as needed to achieve fine control of the distillation process, thereby optimizing the production process.

[0036] In some embodiments, the condenser temperature detection control unit includes a condensing water flow remote control valve 103, a water inlet temperature detection thermocouple 101, and a water outlet temperature detection thermocouple 102. The condensing water flow remote control valve 103 is installed on the water inlet pipe of the condenser 104, and is used to remotely control the flow of cooling water. By adjusting the opening and closing degree of the valve, the amount of cooling water entering the condenser 104 can be controlled, thereby affecting the condensation efficiency and the temperature control inside the condenser 104. The water inlet temperature detection thermocouple 101 is installed on the water inlet pipe of the condenser 104, and is used to monitor the temperature of the cooling water entering the condenser 104 in real time. The water outlet temperature detection thermocouple 102 is installed on the water outlet pipe of the condenser 104, and is used to detect the temperature of the cooling water flowing out of the condenser 104. The condenser 104 is a vertical shell and tube condenser 104, and its cooling water inlet is arranged at the top of the condenser 104. The cooling water enters the condenser 104 tube from the top, flows down along the inner wall of the tube in a film shape and is evenly sprayed on the outer wall of the condenser 104 to cool the high-temperature gas generated in the evaporator.

[0037] In some embodiments, the vacuum pump of the low vacuum unit is a first slide valve pump 307, which is suitable for large vacuum equipment and can provide sufficient pumping speed to achieve effective vacuum extraction, thereby ensuring the smooth progress of the titanium sponge production process. The vacuum pump of the high vacuum unit is a combination of the second slide valve pump 305 and the oil booster pump 304. In the high vacuum unit, the combination of the slide valve pump and the oil booster pump 304 can achieve more efficient and stable vacuum extraction.

[0038] A second aspect of the present invention provides a method for accurately controlling process parameters in a titanium sponge distillation process, comprising the following steps: S1, initial stage: the staff sets the working pressure of the distiller 201, the working temperature of the distiller 201, the working pressure in the condenser 104, and the working temperature in the condenser 104. Specifically, the staff sets the working parameters of the distiller pressure detection control unit, the distiller temperature detection control unit, the condenser pressure detection control unit, and the condenser temperature detection control unit through the human-computer interaction system.

[0039] S2, reduction stage: turn on the distillation furnace 401, heat the distillation furnace 401 according to the temperature parameters of the set distiller temperature detection control unit, and implement a reduction process on the raw materials in the distiller 201; in an argon atmosphere at 880°C to 950°C, react titanium tetrachloride with metallic magnesium to obtain sponge-like metallic titanium and magnesium chloride, and use vacuum distillation to remove excess metallic magnesium and reduction by-product magnesium chloride in the sponge titanium, thereby obtaining pure titanium.

[0040] S3, distillation stage: real-time detection of the pressure in the distiller 201, the temperature in the distiller 201, the pressure in the condenser 104, the temperature in the condenser 104, and regulation of the process parameters of the distiller 201, the condenser 104 and the vacuum unit based on the set working pressure of the distiller 201, the working temperature of the distiller 201, the working pressure in the condenser 104 and the working temperature in the condenser 104. Specifically, the pressure in the distiller 201 can be detected by the second vacuum gauge 202, the temperature in the distiller 201 can be detected by the thermocouple 402, the pressure in the condenser 104 can be detected by the third vacuum gauge 204, and the working temperature in the condenser 104 can be detected by the water inlet temperature detection thermocouple 101 and the water outlet temperature detection thermocouple 102. The process parameters of the distiller 201, the condenser 104 and the vacuum unit are regulated by the DCS control system based on the working parameters set in the human-computer interaction system.

[0041] The method for accurately controlling the process parameters of the titanium sponge distillation process proposed in the second aspect of this application plays an important role in ensuring product quality, optimizing production efficiency and improving safety. By accurately controlling the process parameters at each stage, not only can the structure and performance of titanium sponge be improved, but also the efficient and stable operation of the production process can be ensured.

[0042] In some embodiments, in step S2, the reduction stage further comprises: when the pressure in the distiller 201 is 10 5 When the pressure of distiller 201 is 50Pa to 1Pa, a deeper vacuum is required to completely separate Ti, Mg and MgCl. 2 The DCS control system sends instructions to the vacuum unit to control the high vacuum unit to start pumping. The high vacuum unit can work at a lower pressure to ensure the maximum removal of residual gas, thereby improving the purity of sponge titanium.

[0043] In some embodiments, in step S3, the distillation stage further comprises: S31, regulating the pressure in the distiller 201: When the distiller pressure detection control unit detects that the pressure in the distiller 201 is greater than 100 Pa, such as 10 5 When the pressure in the distiller 201 is between 100 and 10Pa and the pressure drop rate is less than 2Pa / h, or when the pressure in the distiller 201 is between 100 and 10Pa and the pressure drop rate is less than 0.5Pa / h, or when the pressure in the distiller 201 is less than 1Pa but the pressure in the distiller 201 gradually rises, the DCS control system determines that the pressure in the distiller 201 is in an abnormal state, controls the vacuum unit to shut down, and sends an argon filling and airtightness detection instruction to the distiller pressure detection control unit, so that the first automatic argon filling valve 203 is opened, and the distiller 201 is filled with argon and the airtightness detection is performed.

[0044] Specifically, when the distiller pressure detection control unit detects that the pressure in the distiller 201 is greater than 100Pa, and the pressure drop rate is less than 2Pa / h, this indicates that the system is in a high-pressure state and the pressure drops slowly, which may be due to system leakage or insufficient distillation of the material. When the pressure in the distiller 201 is 100-10Pa, and the pressure drop rate is less than 0.5Pa / h, although the pressure is low at this stage, the pressure drop rate is too slow, which may also reflect insufficient distillation efficiency or a slight leakage problem in the system. In addition, when the pressure of the distiller 201 is less than 1Pa, but the pressure of the distiller 201 gradually rises, this is usually an abnormal state, indicating that external gas has infiltrated the system, or internal reactions have produced additional gas. Therefore, leak detection is required. During leak detection, first close the remote automatic pneumatic valve of the vacuum pipeline, and then fill argon into the distiller 201 through the first automatic argon filling valve 203. When the pressure reaches above 101325Pa, spray leak detection water (soapy water) on the connection between the distiller 201 and the condenser 104, and then use vacuum mud or welding to repair the leak.

[0045] In some embodiments, in step S3, the distillation stage further comprises: S32, regulating the temperature in the distiller 201: when the pressure in the distiller 201 is 10 5 When the pressure of distiller 201 is 100-1Pa, the DCS control system controls the temperature of distiller 201 to 950-955°C through the distillation furnace 401. This temperature range is conducive to promoting the evaporation of magnesium and magnesium chloride under higher pressure, while the vapor pressure of titanium is close to zero. This means that under this condition, magnesium and magnesium chloride can evaporate from the mixture first, while titanium remains in a solid state, thereby achieving separation. When the pressure of distiller 201 is 100-1Pa, the DCS control system controls the temperature of distiller 201 to 1000-1005°C through the distillation furnace 401. Under this temperature and pressure condition, the saturated vapor pressure of magnesium and magnesium chloride is further increased, which promotes a more thorough evaporation and separation process. At the same time, such a high temperature also helps to maintain the fluidity and activity of sponge titanium, preventing it from becoming dense and hardened due to low temperature during the distillation process.

[0046] In some embodiments, in step S3, the distillation stage further comprises: S33, regulating the pressure in the condenser 104: When the condenser pressure detection control unit detects that the pressure in the condenser 104 is greater than 100 Pa, such as 10 5When the pressure of the condenser 104 is between 100 and 10Pa and the pressure drop rate is less than 2Pa / h, or when the pressure of the condenser 104 is between 100 and 10Pa and the pressure drop rate is less than 0.5Pa / h, or when the pressure of the condenser 104 is less than 1Pa, but the pressure of the condenser 104 rises, the DCS control system determines that the pressure of the condenser 104 is abnormal, controls the vacuum unit to close, and sends an argon filling and air tightness detection instruction to the condenser pressure detection control unit, so that the second automatic argon filling valve 205 is opened, and argon filling and air tightness detection are performed on the condenser 104. The principle is the same as the pressure control principle in the distiller 201, so it will not be repeated.

[0047] In some embodiments, in step S3, the distillation stage further comprises: S34, regulating the temperature inside the condenser 104: Control the inlet temperature of the cooling water on the condenser 104 to be less than or equal to 25°C. A lower inlet temperature helps to quickly condense the steam into liquid, avoiding pipe blockage or equipment damage due to insufficient condensation. The outlet temperature of the cooling water is 55°C to 60°C, which can not only ensure the condensation effect, but also avoid the long-term stable operation of the system affected by excessive water temperature. When the outlet water temperature detection thermocouple 102 detects that the temperature is too high or too low, the opening and closing degree of the valve 103 is remotely controlled by adjusting the condensate flow rate to control the amount of cooling water entering the condenser 104, thereby affecting the condensation efficiency and the temperature control inside the condenser 104.

[0048] In some embodiments, when the pressure values ​​of the distiller 201 and the condenser 104 are less than 1Pa, and the pressure of the distiller 201 is less than 10Pa for more than a preset time, the DCS control system issues an end distillation instruction, and the distillation furnace 401 is turned off. Specifically, the preset time is set to H, H is equal to furnace weight / ton × 10, unit hour, h.

[0049] When the pressure value of the distiller 201 and the condenser 104 is greater than or equal to 1Pa, or the pressure of the distiller 201 is less than 10Pa for a period less than the preset time, the distillation cycle is controlled according to the preset cycle. The preset cycle is set to M. M is equal to furnace weight / ton × 13 to 19, in hours, and the optimal value is 15.

[0050] In some embodiments, the titanium sponge distillation process control system also includes S4, cooling stage: the DCS control system continuously monitors the pressure of the distiller 201 and the condenser 104. When the pressure of the distiller 201 and the condenser 104 is lower than 5kPa, the DCS control system issues an instruction to control the first automatic argon filling valve 203 and the second automatic argon filling valve 205 to open, and the distiller 201 and the condenser 104 are filled with argon; when the pressure reaches 15kPa, the first automatic argon filling valve 203 and the second automatic argon filling valve 205 are controlled to close, and argon filling is stopped. Specifically, when the pressure is lower than 5kPa, this indicates that the system has reached a higher vacuum degree, and measures need to be taken to protect the equipment and products. As an inert gas, argon can effectively prevent titanium sponge from oxidation or other adverse reactions under high temperature and high vacuum conditions. At the same time, argon can also maintain the stability of the internal pressure of the system to avoid equipment damage or product contamination caused by too low pressure. When the pressure reaches 15 kPa, in order to prevent excessive pressure caused by over-filling with argon, thereby affecting the normal operation of the system and the quality of titanium sponge, the first automatic argon filling valve 203 and the second automatic argon filling valve 205 need to be closed to stop filling with argon. At the same time, the first automatic argon release valve and the second automatic argon release valve 105 can also be opened appropriately.

[0051] The technical features of the above embodiments may be combined arbitrarily. To make the description concise, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0052] The above-mentioned embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for a person of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the patent of the present application shall be subject to the attached claims.

Claims

1. A titanium sponge distillation process control system, comprising a distiller (201), a condenser (104), a distillation electric furnace (401) for heating the distiller (201), and a vacuum unit connected to the condenser (104), It is characterized in that Also includes: a distiller pressure detection control unit and a distiller temperature detection control unit disposed on the distiller (201), a condenser pressure detection control unit and a condenser temperature detection control unit disposed on the condenser (104), and a vacuum unit detection control unit disposed on the vacuum unit; Further including: A human-computer interaction system configured to set the working pressure of the distiller (201), the working temperature of the distiller (201), the working pressure in the condenser (104), and the working temperature in the condenser (104); The DCS control system is configured to receive detection values ​​fed back by the distiller pressure detection control unit, the distiller temperature detection control unit, the condenser pressure detection control unit, and the condenser temperature detection control unit, and to regulate the process parameters of the distiller (201), the condenser (104), and the vacuum unit based on the distiller (201) working pressure, the distiller (201) working temperature, the condenser (104) internal working pressure, and the condenser (104) internal working temperature set in the human-computer interaction system.

2. The titanium sponge distillation process control system according to claim 1, It is characterized in that The vacuum unit comprises a low vacuum unit and a high vacuum unit arranged in parallel; the low vacuum unit and the high vacuum unit are connected via a vacuum pipeline and are connected to a condenser (104); the vacuum unit detection control unit comprises a first vacuum gauge (301) and a remote automatic pneumatic valve arranged on the vacuum pipeline.

3. The titanium sponge distillation process control system according to claim 1, It is characterized in that The distiller pressure detection control unit comprises a second vacuum gauge (202) which is communicatively connected to a DCS control system, a first automatic argon filling valve (203), and a first automatic argon release valve; wherein the second vacuum gauge (202) is installed in the vacuum system of the distiller (201) to monitor the gas pressure in the distiller (201) in real time; the first automatic argon filling valve (203) is installed on the air inlet pipe of the distiller (201) to control the flow rate and timing of argon gas entering the distiller (201); and the first automatic argon release valve is installed on the air outlet pipe of the distiller (201) to control the gas discharge in the distiller (201).

4. The titanium sponge distillation process control system according to claim 1, It is characterized in that The distiller temperature detection control unit comprises a thermocouple (402) and a power regulator (403) which are communicatively connected to a DCS control system. The thermocouples (402) are longitudinally arranged in 5 to 6 groups along the outer wall of the distiller (201), and each group comprises 2 to 4 thermocouples (402) uniformly arranged along the longitudinal direction. The power regulator (403) is installed on the distillation furnace (401) and is used to adjust the heating power of the distillation furnace (401).

5. The titanium sponge distillation process control system according to claim 1, It is characterized in that The condenser pressure detection control unit comprises a third vacuum gauge (204), a second automatic argon filling valve (205) and a second automatic argon release valve (105) which are communicatively connected to a DCS control system; the third vacuum gauge (204) is mounted on the condenser (104); the second automatic argon filling valve (205) is mounted on an air inlet pipe of the condenser (104); and the second automatic argon release valve (105) is mounted on an air outlet pipe of the condenser (104).

6. The titanium sponge distillation process control system according to claim 1, It is characterized in that The condenser temperature detection control unit comprises a condensate flow remote control valve (103) which is communicatively connected to a DCS control system, a water inlet temperature detection thermocouple (101), and a water outlet temperature detection thermocouple (102); the condensate flow remote control valve (103) is installed on the water inlet pipe of the condenser (104); the water inlet temperature detection thermocouple (101) is installed on the water inlet pipe of the condenser (104); the water outlet temperature detection thermocouple (102) is installed on the water outlet pipe of the condenser (104); wherein the condenser (104) is a vertical shell and tube condenser (104), and its cooling water inlet is arranged at the top of the condenser (104).

7. The titanium sponge distillation process control system according to claim 2, It is characterized in that The vacuum pump of the low vacuum unit is a first slide valve pump (307); the vacuum pump of the high vacuum unit is a combination of a second slide valve pump (305) and an oil booster pump (304).

8. A method for controlling the distillation process of titanium sponge, It is characterized in that The following steps are involved: S1, initial stage: the staff sets the working pressure of the distiller (201), the working temperature of the distiller (201), the working pressure inside the condenser (104), and the working temperature inside the condenser (104); S2, reduction stage: turning on the distillation electric furnace (401), causing the distillation electric furnace (401) to heat up according to the set working temperature of the distiller (201), and performing a reduction process on the raw materials in the distiller (201); S3, distillation stage: real-time detection of the pressure inside the distiller (201), the temperature inside the distiller (201), the pressure inside the condenser (104), and the temperature inside the condenser (104), and control of the process parameters of the distiller (201), the condenser (104), and the vacuum unit based on the set working pressure of the distiller (201), the working temperature of the distiller (201), the working pressure inside the condenser (104), and the working temperature inside the condenser (104).

9. The titanium sponge distillation process control method according to claim 8, It is characterized in that In step S2, the reduction stage further comprises: when the pressure in the distiller (201) is 10 5 When the pressure of the distiller (201) is 50Pa~1Pa, the high vacuum unit is turned on to evacuate the air.

10. The titanium sponge distillation process control method according to claim 8, It is characterized in that In step S3, the distillation stage further comprises: S31, regulating the pressure in the distiller (201): when it is detected that the pressure in the distiller (201) is greater than 100 Pa and the pressure drop rate is less than 2 Pa / h, or when the pressure in the distiller (201) is 100-10 Pa and the pressure drop rate is less than 0.5 Pa / h, or when the pressure in the distiller (201) is less than 1 Pa but the pressure in the distiller (201) gradually increases, it is determined that the pressure in the distiller (201) is in an abnormal state, the vacuum unit is controlled to be closed, and the distiller (201) is filled with argon and an air tightness test is performed.

11. The titanium sponge distillation process control method according to claim 10, It is characterized in that In step S3, the distillation stage further comprises: S32, regulating the temperature in the distiller (201): when the pressure in the distiller (201) is 10 5 When the pressure of the distiller (201) is 100-1 Pa, the temperature of the distiller (201) is controlled to be 950-955°C. When the pressure of the distiller (201) is 100-1 Pa, the temperature of the distiller (201) is controlled to be 1000-1005°C.

12. The titanium sponge distillation process control method according to claim 11: It is characterized in that In step S3, the distillation stage further comprises: S33, regulating the pressure in the condenser (104): when it is detected that the pressure in the condenser (104) is greater than 100 Pa and the pressure drop rate is less than 2 Pa / h, or when the pressure in the condenser (104) is between 100 and 10 Pa and the pressure drop rate is less than 0.5 Pa / h, or when the pressure in the condenser (104) is less than 1 Pa but the pressure in the condenser (104) rises, it is determined that the pressure in the condenser (104) is in an abnormal state, the vacuum unit is controlled to be shut down, and an argon filling and air tightness detection instruction is sent to the condenser (104).

13. The titanium sponge distillation process control method according to claim 12: It is characterized in that In step S3, the distillation stage further comprises: S34, regulating the temperature in the condenser (104): controlling the inlet temperature of the cooling water on the condenser (104) to be less than or equal to 25°C, and the outlet temperature of the cooling water to be 55°C to 60°C.

14. The method for controlling the titanium sponge distillation process according to claim 13, It is characterized in that Also includes S35: Distillation Cycle Control: When the pressure values ​​of the distiller (201) and the condenser (104) are less than 1 Pa, and the duration of the pressure of the distiller (201) being less than 10 Pa exceeds a preset time, the distillation is terminated; When the pressure values ​​of the distiller (201) and the condenser (104) are greater than or equal to 1 Pa, or the duration for which the pressure of the distiller (201) is less than 10 Pa is less than a preset time, the distillation cycle is controlled according to the preset cycle.

15. The method for controlling the titanium sponge distillation process according to claim 14, It is characterized in that The process also includes S4, a cooling stage: monitoring the pressure of the distiller (201) and the condenser (104); when the pressure of the distiller (201) and the condenser (104) is lower than 5 kPa, filling the distiller (201) and the condenser (104) with argon; and stopping the filling with argon when the pressure reaches above 15 kPa.

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