CN117732095A - Method for treating sodium azide by adopting triple-effect evaporation system - Google Patents

Method for treating sodium azide by adopting triple-effect evaporation system Download PDF

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CN117732095A
CN117732095A CN202410190352.1A CN202410190352A CN117732095A CN 117732095 A CN117732095 A CN 117732095A CN 202410190352 A CN202410190352 A CN 202410190352A CN 117732095 A CN117732095 A CN 117732095A
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effect
effect evaporator
triple
evaporator
sodium azide
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CN117732095B (en
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陈潇
杨卓华
邓超
陈语
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Gongxian Huajie Hazardous Waste Treatment Co ltd Chengdu Branch
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Gongxian Huajie Hazardous Waste Treatment Co ltd Chengdu Branch
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Abstract

The invention provides a method for treating sodium azide by adopting a three-effect evaporation system, and relates to the technical field of hazardous waste treatment. According to the method for treating sodium azide by adopting the three-effect evaporation system, provided by the invention, the liquid level of the evaporation cabin is controlled, the pressure and flow of the circulating hot water are controlled, the temperature of the circulating hot water is controlled, the liquid phase temperature and the gas phase pressure of the evaporation cabin are controlled, the liquid phase pH value and the ORP value of the evaporation cabin are controlled, and the parameters of the three-effect evaporation system which normally operates can be adjusted to the technological parameters capable of treating sodium azide within 1 hour through the DCS control system, so that the time cost and the labor cost are greatly saved. The method for treating sodium azide by adopting the triple-effect evaporation system provided by the invention can treat sodium azide in batches, and personnel only need to add sodium azide into the triple-effect evaporation crystallizer, so that the personnel do not participate in reaction operation, and the safety coefficient is high.

Description

Method for treating sodium azide by adopting triple-effect evaporation system
Technical Field
The invention relates to the technical field of hazardous waste treatment, in particular to a method for treating sodium azide by adopting a three-effect evaporation system.
Background
Sodium azide (Sodium azide), molecular formula NaN 3 Colorless hexagonal crystals, which are easily soluble in water and liquid ammonia, slightly soluble in ethanol, and insoluble in diethyl ether. Sodium azide may explode when heated, exposed to open fire, or subjected to friction, shock, or impact, and react violently with acids to produce explosive hydrazoic acid. The compound which is very sensitive to heavy metals and salts thereof is a dangerous chemical with explosiveness.
At present, sodium hypochlorite and potassium permanganate are mostly used for oxidizing the waste water in an alkaline environment, and the danger is eliminated through the reaction.
The existing treatment technology is only suitable for treating very small amount of sodium azide, is not suitable for large-batch (more than 10 kg) treatment, has high participation degree of personnel in the treatment process, has high risk coefficient, and is highly likely to cause hypoxia or poisoning of operators due to generated nitrogen or ammonia.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims at providing a method for treating sodium azide by adopting a three-effect evaporation system, which can treat sodium azide on a large scale, is not limited to the scale of tens or hundreds of grams abandoned in a laboratory, and has practical significance for treating enterprises on a scale of tens of kilograms; the personnel participation degree is small, the personnel contact is not needed for the reaction and the desalination, and the safety of the staff is greatly improved.
Embodiments of the invention may be implemented as follows:
in a first aspect, the present invention provides a method of treating sodium azide using a triple effect evaporation system comprising:
s110, starting solvent material supply of a first-effect evaporator, a second-effect evaporator and a third-effect evaporator step by step, controlling liquid levels by using liquid level monitors arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator, and starting a first-effect circulating pump of the first-effect evaporator, a second-effect circulating pump of the second-effect evaporator and a third-effect circulating pump of the third-effect evaporator for internal circulation;
s120, starting the water replenishing of the circulating hot water tank, controlling the liquid level by using a liquid level monitor arranged on the circulating hot water tank, and starting the circulating hot water system in an interlocking manner;
s130, after the pressure and the flow of the circulating hot water system meet the requirements, starting the fully premixed gas boiler in an interlocking way, adjusting the gas flow in an interlocking way according to the temperature of circulating hot water in the circulating hot water system, and establishing heat source supply of a three-effect evaporation system for normal operation;
s140, controlling the temperature of the circulating hot water system through a temperature monitor and a pressure monitor which are respectively arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator, so that the liquid phase temperature in the first-effect evaporator is 60-65 ℃, the gas phase pressure is-50 to-60 kPa, the liquid phase temperature in the second-effect evaporator is 45-50 ℃, the gas phase pressure is-70 to-80 kPa, and the liquid phase temperature in the third-effect evaporator is 35-38 ℃, and the gas phase pressure is-87 to-90 kPa;
s150, controlling the addition amounts of sodium hypochlorite solution and sodium hydroxide solution through a pH monitor and an ORP value detector which are respectively arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator, so that the pH value of a liquid phase in the first-effect evaporator is more than or equal to 8, the ORP value is more than or equal to 400mv, the pH value of the liquid phase in the second-effect evaporator is more than or equal to 7.5, the ORP value is more than or equal to 200mv, and the pH value of the liquid phase in the third-effect evaporator is more than or equal to 9, and the ORP value is more than or equal to 650mv;
and S160, after the requirements of the step S140 and the step S150 are met, introducing sodium azide into the triple-effect evaporation crystallizer for reaction, and conveying the reacted salt-containing wastewater into the first-effect evaporator and the double-effect evaporation crystallizer for desalting through a feeding mechanism.
In an alternative embodiment, the upper limit of the pH value of the liquid phase in the first-effect evaporator is 10, the upper limit of the ORP value is 500 mv, the upper limit of the pH value of the liquid phase in the second-effect evaporator is 8.5, the upper limit of the ORP value is 300mv, and the upper limit of the pH value of the liquid phase in the third-effect evaporator is 10, the upper limit of the ORP value is 750 mv.
In an alternative embodiment, the triple effect evaporation crystallizer is provided with a feeding chute for feeding the sodium azide and a negative pressure suction mechanism, a damping spring is arranged at the bottom of the feeding chute, one end of the negative pressure suction mechanism is communicated with the feeding chute, and the other end of the negative pressure suction mechanism is communicated with the inside of the triple effect evaporation crystallizer.
In an alternative embodiment, the suction gas flow rate of the negative pressure suction mechanism is 1-2 m/s.
In an alternative embodiment, the weight of sodium azide added to the feed chute at a time is 1 to 1000g.
In an alternative embodiment, an effective heater is arranged between the first-effect evaporator and the first-effect circulating pump, a second-effect heater is arranged between the second-effect evaporation crystallizer and the second-effect circulating pump, and a third-effect heater is arranged between the third-effect evaporation crystallizer and the third-effect circulating pump;
and the gas outlet of the first-effect evaporator is communicated with the second-effect heater for heat gradient recovery, and the gas outlet of the second-effect evaporation crystallizer is communicated with the third-effect heater for heat gradient recovery.
In an alternative embodiment, the circulating water discharged from the circulating hot water tank is heated by the fully premixed gas boiler, then is introduced into the first-effect heater, the second-effect preheater and the third-effect preheater, and is circulated and returned to the circulating hot water tank.
In an optional embodiment, the feeding mechanism comprises a salt-containing wastewater pipeline, the salt-containing wastewater in the salt-containing wastewater pipeline is wastewater or industrial wastewater after salt water separation of a three-effect evaporation system, the salt-containing wastewater is preheated by a three-effect preheater and then exchanges heat with the three-effect heater, and is discharged to the first-effect evaporator and fed to the pipeline connected with the first-effect circulating pump.
In an optional embodiment, the feeding mechanism further comprises a second-effect material transferring pump arranged between the first-effect circulating pump and the second-effect circulating pump, an inlet of the second-effect material transferring pump is connected to a pipeline between the first-effect circulating pump and the first-effect heater, an outlet of the second-effect material transferring pump is divided into two paths, one path of the second-effect material transferring pump is connected to the pipeline between the second-effect circulating pump and the second-effect heater, and the other path of the second-effect material transferring pump is connected to an inlet pipeline of the first-effect circulating pump.
In an alternative embodiment, the sodium hypochlorite solution has a concentration of 40-60wt% and the sodium hydroxide solution has a concentration of 20-40wt%.
The beneficial effects of the embodiment of the invention include, for example:
the method for treating sodium azide by adopting the three-effect evaporation system does not need to construct a new production operation device, can be completed by technical improvement of the existing mature three-effect evaporation system device, and reduces equipment investment; for example, the method can be completed by technical transformation of the existing titanium alloy material three-effect evaporation system, special materials are not required to be additionally researched and developed or special equipment is not required to be built, and investment of production equipment is reduced. The personnel participation degree is small, and the safety aspect can be better ensured; the sodium azide can be treated in a large scale, and the problem can be solved from the practical production; the production operation can be carried out on the existing operation three-effect evaporation system by adjusting the technological parameters, the system is not required to be subjected to drainage replacement, the time interval for switching the operation functions of the equipment is reduced, and the production cost is reduced. In the present invention, the process control includes: the liquid level control system of the evaporation chamber (a first-effect evaporator, a second-effect evaporator and a third-effect evaporator), the circulating hot water pressure and flow control system, the circulating hot water temperature control system, the liquid phase temperature and the gas phase pressure of the evaporation chamber (the first-effect evaporator, the second-effect evaporator and the third-effect evaporator) are controlled, and the liquid phase pH value and the ORP value of the evaporation chamber (the first-effect evaporator, the second-effect evaporator and the third-effect evaporator) are controlled. The material water supply and stable adjustment of the one-key starting three-effect system can be realized, the step-by-step water supplementing and the circulating pump starting are not required to be operated by personnel, only the operation parameters are required to be monitored, and the workload of operators is reduced. According to the method for treating sodium azide by adopting the three-effect evaporation system, provided by the invention, the parameters of the three-effect evaporation system which is in normal operation can be adjusted to the technological parameters capable of treating sodium azide by the DCS control system within 1 hour, so that the time cost and the labor cost are greatly saved. The method for treating sodium azide by adopting the three-effect evaporation system provided by the invention can treat sodium azide in batches, and personnel only need to place the sodium azide at the feeding chute, and the personnel do not participate in reaction operation, so that the safety coefficient is high.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of a triple-effect evaporation system used in a method for treating sodium azide using the triple-effect evaporation system according to an embodiment of the present application;
FIG. 2 is a process flow diagram of a method for treating sodium azide using a triple effect evaporation system according to an embodiment of the present application;
FIG. 3 is a logic diagram (A) and a logic diagram (B) of a control program for one-effect feed interlock in a method for treating sodium azide using a triple effect evaporation system according to an embodiment of the present application;
fig. 4 is a logic diagram (a) and a logic diagram (B) of a control program for liquid level interlocking of a circulating hot water tank in a method for treating sodium azide by using a triple effect evaporation system according to an embodiment of the present application;
FIG. 5 is a logic diagram (A) and a logic diagram (B) of a control program for temperature control interlock in a method for treating sodium azide using a triple effect evaporation system according to an embodiment of the present application;
FIG. 6 is a logic diagram (A) and a logic diagram (B) of a control program for one-effect pH adjustment in a method for treating sodium azide using a triple effect evaporation system according to an embodiment of the present application;
FIG. 7 is a logic diagram (A) and a logic diagram (B) of control program for one-effect ORP adjustment in a method for treating sodium azide using a triple effect evaporation system according to an embodiment of the present application;
fig. 8 is a schematic structural diagram of a feed chute in a method for treating sodium azide using a triple effect evaporation system according to an embodiment of the present application.
Icon: a 100-triple effect evaporation system;
110-a first effect evaporator; 111-a first-effect circulating pump; 112-a one-effect heater;
120-double effect evaporation crystallizer; 121-a two-way circulation pump; 122-a dual effect heater; 123-a two-effect preheater;
130-a triple effect evaporative crystallizer; 131-a triple-effect circulating pump; 132-a triple effect heater; 133-triple effect preheater; 134-a feed chute; 135-a damping spring;
140-circulating a hot water tank; 141-a circulating hot water pump; 142-a fully premixed gas boiler;
150-a feeding mechanism; 151-a saline wastewater conduit; 152-a double-effect transfer pump;
201-a liquid level monitor; 202-a temperature monitor; 203-a pressure monitor; 204-a pH monitor; 205-ORP value detector.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
In the description of the present invention, it should be noted that, if the terms "upper", "lower", "inner", "outer", and the like indicate an azimuth or a positional relationship based on the azimuth or the positional relationship shown in the drawings, or the azimuth or the positional relationship in which the inventive product is conventionally put in use, it is merely for convenience of describing the present invention and simplifying the description, and it is not indicated or implied that the apparatus or element referred to must have a specific azimuth, be configured and operated in a specific azimuth, and thus it should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, if any, are used merely for distinguishing between descriptions and not for indicating or implying a relative importance.
It should be noted that the features of the embodiments of the present invention may be combined with each other without conflict.
Referring to fig. 1 and 2, the present invention provides a method for treating sodium azide using a triple effect evaporation system, comprising:
s110, operation linkage.
Referring to fig. 1 and 3, solvent material replenishment of the first-effect evaporator 110, the second-effect evaporator 120 and the third-effect evaporator 130 is started step by step, liquid level is controlled to 600 mm-1000 mm by using a liquid level monitor 201 arranged on the first-effect evaporator 110, the second-effect evaporator 120 and the third-effect evaporator 130, and an internal circulation is performed by starting a first-effect circulation pump 111 of the first-effect evaporator 110, a second-effect circulation pump 121 of the second-effect evaporator 120 and a third-effect circulation pump 131 of the third-effect evaporator 130. Fig. 3 shows a feed control process of the first-effect evaporator 110, and a feed control process of the second-effect evaporator-crystallizer 120 and the third-effect evaporator-crystallizer 130 is the same as that of the first-effect evaporator 110, so that a detailed description thereof will be omitted.
The solvent material can be tap water, salt-containing wastewater or other industrial wastewater, and is mainly used as a solvent for dissolving subsequent sodium hypochlorite solution, sodium hydroxide solution and sodium azide and providing an aqueous reaction environment.
S120, interlocking the liquid level of the circulating hot water tank.
Referring to fig. 1 and 4, the circulating hot water tank 140 is started to replenish water, and the liquid level parallel lock is controlled by the liquid level monitor 201 arranged on the circulating hot water tank 140 to start the circulating hot water system. The process ensures the normal circulation of the circulating hot water system.
S130, temperature control interlocking.
Referring to fig. 1 and 5, after the pressure and flow rate of the circulating hot water system reach the requirements, the fully premixed gas boiler 142 is started in an interlocking manner, and the gas flow rate is adjusted in an interlocking manner according to the temperature of the circulating hot water in the circulating hot water system, so that the heat source supply of the triple effect evaporation system 100 is established, and the triple effect evaporation system operates normally. The pressure of the circulating hot water system is 0.4-0.6 MPa, and the flow is 10-15 m/h.
A first-effect heater 112 is arranged between the first-effect evaporator 110 and the first-effect circulating pump 111, a second-effect heater 122 is arranged between the second-effect evaporation crystallizer 120 and the second-effect circulating pump 121, and a third-effect heater 132 is arranged between the third-effect evaporation crystallizer 130 and the third-effect circulating pump 131; meanwhile, the two-effect evaporative crystallizer 120 is also equipped with a two-effect preheater 123, and the three-effect evaporative crystallizer 130 is also equipped with a three-effect preheater 133.
The circulating water discharged from the circulating hot water tank 140 enters the full premix gas boiler 142 through the circulating hot water pump 141 to be heated, is introduced into the first-effect heater 112, the second-effect preheater 123 and the third-effect preheater 133, and is circulated and returned to the circulating hot water tank 140, the gas outlet of the first-effect evaporator 110 is communicated with the second-effect heater 122 to perform heat gradient recovery, and the gas outlet of the second-effect evaporator 120 is communicated with the third-effect heater 132 to perform heat gradient recovery.
The circulating hot water exchanges heat with the first-effect heater 112, so that the solvent in the first-effect evaporator 110 is heated, the temperature in the first-effect evaporator 110 is regulated and controlled, further, the second-effect evaporation crystallizer 120 exchanges heat with the solvent in the second-effect heater 122 by utilizing the high-temperature gas of the first-effect evaporator 110, and the third-effect heater 132 exchanges heat with the solvent in the third-effect heater 132 by utilizing the high-temperature gas of the second-effect evaporator.
S140, controlling the temperature and the gas phase pressure of each effective liquid phase.
Because sodium azide is heated, it can explode when exposed to open fire, or when rubbed, vibrated, or impacted. In order to avoid the risk of thermal flash explosion of sodium azide when the sodium azide enters the triple-effect evaporation crystallizer 130, the temperature of each liquid phase and the pressure of gas phase are adjusted in advance through a temperature control interlock, a feeding/discharging control interlock and a negative pressure suction mechanism control interlock.
The temperature of the circulating hot water system is controlled by a temperature monitor 202 and a pressure monitor 203 which are respectively arranged on the first-effect evaporator 110, the second-effect evaporator 120 and the third-effect evaporator 130, so that the liquid phase temperature in the first-effect evaporator 110 is 60-65 ℃, the gas phase pressure is minus 50-minus 60kPa, the liquid phase temperature in the second-effect evaporator 120 is 45-50 ℃, the gas phase pressure is minus 70-minus 80kPa, and the liquid phase temperature in the third-effect evaporator 130 is 35-38 ℃ and the gas phase pressure is minus 87-minus 90kPa.
Wherein, the material of the first-effect evaporator 110 is from the three-effect evaporation crystallizer 130, the main purpose of the first-effect evaporator 110 is to obtain heat from the outside, evaporate water in large quantity, provide heat sources for the two-effect evaporation crystallizer 120 and the three-effect evaporation crystallizer 130, and increase the salt solution concentration; the secondary purpose of the first-effect evaporator 110 is to escape unreacted sodium azide from the triple-effect evaporator 130, after the reaction is finished, the temperature is controlled to save the heat source cost and ensure that the sodium azide does not have safety risks under the condition that the triple-effect evaporator 130 escapes too much, if the temperature is too high, the risk of violent reaction and even flash explosion occurs, the cost consumption of distilled water condensation is increased, and the pressure is controlled to ensure the power consumption of a negative pressure suction mechanism and improve the evaporation efficiency, so that the liquid phase temperature in the first-effect evaporator 110 is controlled to be 60-65 ℃ and the gas phase pressure is controlled to be-50 to-60 kPa.
The two-effect evaporation crystallizer 120 is mainly used for separating out salt crystals, so that the desalting function of the three-effect evaporation crystallizer 130 system is realized, and the temperature control at the stage ensures that the temperature of discharged salt is not too high, and the effect of salt water separation is affected; because the heating source of the triple-effect evaporation crystallizer 130 is from double-effect steam, if the temperature of the double-effect evaporation crystallizer 120 is controlled to be too high, the temperature of the triple-effect evaporation crystallizer 130 is too high, so that the flash explosion risk of the triple-effect evaporation crystallizer 130 for treating sodium azide is increased, the pressure control is used for ensuring the power consumption of a negative pressure suction mechanism and improving the evaporation efficiency, and therefore, the liquid phase temperature in the double-effect evaporation crystallizer 120 is controlled to be 45-50 ℃ and the gas phase pressure is controlled to be-70 to-80 kPa.
The triple effect evaporative crystallizer 130 is the main reaction chamber of sodium azide, the temperature of the section must be controlled below the flash explosion temperature limit, but the control is too low, which affects the reaction efficiency and the efficiency of the whole system of the triple effect evaporative crystallizer 130; because the triple-effect evaporative crystallizer 130 is directly communicated with the negative pressure suction mechanism, the vacuum degree is highest, and the advantages are that the gas released by the reaction can be quickly pumped away and balanced, the safety of the operation process is ensured, the minimum triple-effect temperature is achieved, the greater the vacuum degree is, the more favorable for water evaporation, and the production energy consumption is saved. Therefore, the liquid phase temperature in the triple effect evaporative crystallizer 130 is controlled to be 35-38 ℃ and the gas phase pressure is controlled to be-87 to-90 kPa.
S150, controlling the pH value and ORP value of each effective liquid phase.
Referring to fig. 1, 6 and 7, the addition amounts of sodium hypochlorite solution and sodium hydroxide solution are controlled by a pH monitor 204 and an ORP value detector 205 respectively arranged on the first-effect evaporator 110, the second-effect evaporator 120 and the third-effect evaporator 130, wherein the concentration of the sodium hypochlorite solution is 40-60wt%, and the concentration of the sodium hydroxide solution is 20-40wt%, so that the pH value of a liquid phase in the first-effect evaporator 110 is more than or equal to 8, the ORP value is more than or equal to 400mv, the pH value of a liquid phase in the second-effect evaporator 120 is more than or equal to 7.5, the ORP value is more than or equal to 200mv, the pH value of a liquid phase in the third-effect evaporator 130 is more than or equal to 9, and the ORP value is more than or equal to 650mv.
The upper limit of the liquid phase pH value in the first-effect evaporator 110 is 10, the upper limit of the ORP value is 500 and mv, the upper limit of the liquid phase pH value in the second-effect evaporator 120 is 8.5, the upper limit of the ORP value is 300 and mv, the upper limit of the liquid phase pH value in the third-effect evaporator 130 is 10, and the upper limit of the ORP value is 750 and mv.
Wherein, the pH value of the liquid phase in the first-effect evaporator 110 is more than or equal to 8, the upper limit of the pH value is 10, unnecessary waste of sodium hydroxide can be caused if the control is too high, the pH value possibly causing the second-effect salt to be too high, and the risk of alkali corrosion exists for operators; ORP value is more than or equal to 400mv, upper limit is 500 mv, sodium hypochlorite waste is caused when the control is too high, electrochemical corrosion of equipment is aggravated, and sodium azide concentration entering a two-effect system cannot be ensured to be lower than 0.01% when the control is too low.
The pH value of the liquid phase in the two-effect evaporation crystallizer 120 is more than or equal to 7.5, the upper limit is 8.5, sodium hydroxide is unnecessarily wasted if the control is too high, the pH value of salt is possibly caused to be too high, alkali corrosion risks exist for operators, the ORP value is more than or equal to 200mv, the upper limit is 300mv, the section is only used for dealing with the escape of sodium azide under extremely special conditions, sodium hypochlorite is wasted if the control is too high, and electrochemical corrosion of equipment is aggravated.
The pH value of the liquid phase in the triple effect evaporation crystallizer 130 is more than or equal to 9, the upper limit is 10, and sodium hydroxide is unnecessarily wasted if the control is too high; the ORP value is more than or equal to 650mv, the upper limit is 750mv, the addition of sodium azide is controlled quantity addition, sodium hypochlorite waste is caused if the ORP value is too high, electrochemical corrosion of equipment can be aggravated, and if the ORP value is too low, more than 99% of sodium azide can not be ensured to complete the reaction at the same time, and the sodium azide can escape to an effective system.
Since it cannot be ensured that sodium azide does not escape from the triple-effect evaporative crystallizer 130 to the first-effect evaporative crystallizer 110 and even extremely little escape to the double-effect evaporative crystallizer 120 due to some special reasons during actual operation, in order to ensure that salt and steam condensate discharged from the triple-effect evaporative system 100 are free of sodium azide, it is ensured that ORPs in the first-effect evaporative crystallizer 110, the double-effect evaporative crystallizer 120 and the triple-effect evaporative crystallizer 130 are set parameters in real time (the higher the ORP value is, the stronger the oxidability is, the more favorable the reaction of sodium azide is, but the higher the ORP value is, the cost of sodium hypochlorite cannot be, the equipment cannot be increased, and the sodium azide may generate explosive azidic acid when meeting acid, so that the safety of the disposal process can be ensured and the unnecessary waste of sodium hydroxide can be avoided under the condition that the first-effect evaporator 110, the double-effect evaporative crystallizer 120 and the triple-effect evaporative crystallizer 130 are alkaline.
S160, feeding reaction.
After step S140 and step S150 meet the requirements, sodium azide is introduced into the triple-effect evaporation crystallizer 130 to react, and the reacted salt-containing wastewater is conveyed into the first-effect evaporator 110 and the double-effect evaporation crystallizer 120 to be desalted through the feeding mechanism 150.
Referring to fig. 8, the triple effect evaporative crystallizer 130 is provided with a feed chute 134 for feeding sodium azide and a negative pressure suction mechanism (not shown), one end of which is communicated with the feed chute 134 and the other end of which is communicated with the inside of the triple effect evaporative crystallizer 130.
In this embodiment, the negative pressure suction mechanism is used for feeding, so that the sodium azide can be prevented from diffusing outside the triple-effect evaporation crystallizer 130, the trend of the sodium azide can be ensured to be led into the triple-effect evaporation crystallizer 130 by adopting a negative pressure suction mode, the highly toxic substances are prevented from drifting into the environment, the gas friction and the generated vibration can be ignored, and the safety of the feeding process can be ensured, wherein the negative pressure suction mechanism adopts a negative pressure system matched with the triple-effect evaporation system 100, the suction feeding is completed by utilizing the vacuum degree of the triple-effect evaporation crystallizer 130, the suction gas flow is 1-2 m/s, the suction flow is too large, the vacuum degree in the triple-effect evaporation crystallizer 130 is unbalanced, the sodium azide cannot enter the triple-effect evaporation crystallizer 130 due to the too small suction flow, the weight of the sodium azide which is fed into the chute each time is 1-1000 g, the reaction in the triple-effect evaporation crystallizer 130 is severe due to the too large addition amount, and even the risk of the vacuum degree unbalance of the triple-effect evaporation crystallizer 130 occurs.
Specifically, the feeding chute 134 in this embodiment is obliquely provided with a certain gradient, so that sodium azide can conveniently enter the triple-effect evaporation crystallizer 130, the damping spring 135 is arranged at the bottom of the feeding chute 134, and the damping spring 135 can reduce vibration during feeding, so that the safety of the feeding process is effectively ensured.
The feeding mechanism 150 comprises a salt-containing wastewater pipeline 151, wherein salt-containing wastewater in the salt-containing wastewater pipeline 151 is wastewater or industrial wastewater after salt water separation of a three-effect evaporation system, the salt-containing wastewater is preheated by a three-effect preheater 133 and then exchanges heat with a three-effect heater 132, and is discharged to a pipeline connected with the one-effect evaporator 110 and the one-effect circulating pump 111 to feed the one-effect evaporator 110.
Since the salt-containing wastewater discharged from the triple effect evaporation crystallizer 130 may have escaped sodium azide, the sodium azide can be reacted again by using sodium hypochlorite solution and sodium hydroxide solution inside the triple effect evaporation crystallizer 110 and the triple effect evaporation crystallizer 120 by sequentially entering the triple effect evaporation crystallizer 110 and the triple effect evaporation crystallizer 120, and as can be seen from the liquid phase pH value and ORP value of the triple effect evaporation crystallizer 110, the triple effect evaporation crystallizer 130 is used as a main reaction chamber, the pH value and ORP value of the triple effect evaporation crystallizer 130 are higher, the single effect evaporation crystallizer 110 is used for a plurality of times, and the pH value and ORP value of the double effect evaporation crystallizer 120 are the lowest.
The salt-containing wastewater entering the first-effect evaporator 110 realizes the feeding of the solvent of the first-effect evaporator 110, so that the continuous evaporation of the first-effect evaporator 110 is avoided, the liquid level of the solvent in the first-effect evaporator 110 is reduced to the minimum, in addition, the feeding mechanism 150 further comprises a second-effect transfer pump 152 arranged between the first-effect circulation pump 111 and the second-effect circulation pump 121, an inlet of the second-effect transfer pump 152 is connected to a pipeline between the first-effect circulation pump 111 and the first-effect heater 112, an outlet of the second-effect transfer pump 152 is divided into two paths, one path is connected to a pipeline between the second-effect circulation pump 121 and the second-effect heater 122, and the other path is connected to an inlet pipeline of the first-effect circulation pump 111. By setting the two-effect transfer pump 152, selective material feeding to the two-effect evaporation crystallizer 120 can be realized, and the two-effect transfer pump 152 can be started only when material feeding is needed, but not when material feeding is not needed.
By detecting the concentration of azide ions in the first-effect evaporator 110, the second-effect evaporator 120 and the third-effect evaporator 130 by adopting an ion chromatography method, the treatment effect of sodium azide under the set of process technology is very good, the reaction of sodium azide with the addition amount of more than 99% in the third-effect evaporator 130 is realized, sodium azide is not detected by the second-effect evaporator 120, and the vacuum degree and the temperature of the system are not influenced.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The embodiment provides a method for treating sodium azide by adopting a three-effect evaporation system, which comprises the following steps:
s110, starting solvent material supply of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator step by step, controlling the liquid level to 650-750 mm by using liquid level monitors arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator, and starting a first-effect circulating pump of the first-effect evaporator, a second-effect circulating pump of the second-effect evaporator and a third-effect circulating pump of the third-effect evaporator for internal circulation;
s120, starting the water replenishing of the circulating hot water tank, controlling the liquid level to 1000-1200 mm by using a liquid level monitor arranged on the circulating hot water tank, and then starting the circulating hot water system in an interlocking manner;
s130, after the pressure of the circulating hot water system reaches 0.45MPa and the flow reaches 12 m/h, setting the temperature of circulating hot water in the circulating hot water system to be 85 ℃, starting the fully premixed gas boiler in an interlocking manner, adjusting the gas flow in an interlocking manner according to the temperature of the circulating hot water in the circulating hot water system, and establishing heat source supply of a triple effect evaporation system to run normally;
s140, controlling the temperature of a circulating hot water system through a temperature monitor and a pressure monitor which are arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator respectively, so that the liquid phase temperature in the first-effect evaporator is 60-62 ℃, the gas phase pressure is-55 to-60 kPa, the liquid phase temperature in the second-effect evaporator is 45-48 ℃, the gas phase pressure is-75 to-80 kPa, and the liquid phase temperature in the third-effect evaporator is 35-36 ℃ and the gas phase pressure is-87 to-89 kPa;
s150, controlling the addition amount of the 50wt% sodium hypochlorite solution and the 30wt% sodium hydroxide solution through a pH monitor and an ORP value detector which are arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator respectively, so that the pH value of a liquid phase in the first-effect evaporator is 8-9, the ORP value is 400-450 mv, the pH value of the liquid phase in the second-effect evaporator is 7.5-8, the ORP value is 200-250 mv, the pH value of the liquid phase in the third-effect evaporator is 9-9.5, and the ORP value is 650-700 mv.
S160, after the requirements of the step S140 and the step S150 are met, 500g of sodium azide is sucked by a negative pressure suction mechanism (2 m through a feeding chute with a damping spring arranged at the bottom 3 And/s) introducing the salt-containing wastewater into a three-effect evaporation crystallizer for reaction under the action of the catalyst, and conveying the reacted salt-containing wastewater into the one-effect evaporator and the two-effect evaporation crystallizer for desalting through a feeding mechanism.
Example 2
The embodiment provides a method for treating sodium azide by adopting a three-effect evaporation system, which comprises the following steps:
s110, starting solvent material supply of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator step by step, controlling the liquid level to 750-850 mm by using liquid level monitors arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator, and starting a first-effect circulating pump of the first-effect evaporator, a second-effect circulating pump of the second-effect evaporator and a third-effect circulating pump of the third-effect evaporator for internal circulation;
s120, starting the water replenishing of the circulating hot water tank, controlling the liquid level to 1200-1500 mm by using a liquid level monitor arranged on the circulating hot water tank, and then starting the circulating hot water system in an interlocking manner;
s130, after the pressure of the circulating hot water system reaches 0.5MPa and the flow reaches 15 m/h, setting the temperature of circulating hot water in the circulating hot water system to 90 ℃, starting the fully premixed gas boiler in an interlocking manner, adjusting the gas flow in an interlocking manner according to the temperature of the circulating hot water in the circulating hot water system, and establishing heat source supply of a triple effect evaporation system for normal operation;
s140, controlling the temperature of a circulating hot water system through a temperature monitor and a pressure monitor which are arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator respectively, so that the liquid phase temperature in the first-effect evaporator is 62-65 ℃, the gas phase pressure is-50 to-55 kPa, the liquid phase temperature in the second-effect evaporator is 48-50 ℃, the gas phase pressure is-70 to-75 kPa, and the liquid phase temperature in the third-effect evaporator is 36-38 ℃ and the gas phase pressure is-87 to-89 kPa;
s150, controlling the addition amounts of 50wt% sodium hypochlorite solution and 30wt% sodium oxide solution through a pH monitor and an ORP value detector which are respectively arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator, so that the pH value of a liquid phase in the first-effect evaporator is 9-10, the ORP value is 450-500 mv, the pH value of the liquid phase in the second-effect evaporator is 8-8.5, the ORP value is 250-300 mv, and the pH value of the liquid phase in the third-effect evaporator is 9.5-10, and the ORP value is 700-750 mv;
s160, after the requirements of the step S140 and the step S150 are met, 500g of sodium azide is sucked by a negative pressure suction mechanism (1.5 m through a feeding chute with a damping spring arranged at the bottom 3 And/s) introducing the salt-containing wastewater into a three-effect evaporation crystallizer for reaction under the action of the catalyst, and conveying the reacted salt-containing wastewater into the one-effect evaporator and the two-effect evaporation crystallizer for desalting through a feeding mechanism.
Comparative example 1
This comparative example is substantially the same as example 1 except that the liquid phase temperature and the gas phase pressure are different in step S140. Specifically, in the comparative example, the temperature of a circulating hot water system is controlled through a temperature monitor and a pressure monitor which are arranged on a first-effect evaporator, a second-effect evaporator and a third-effect evaporator respectively, so that the liquid phase temperature in the first-effect evaporator is 55-60 ℃, the gas phase pressure is minus 60 to minus 65 kPa, the liquid phase temperature in the second-effect evaporator is 40-45 ℃, the gas phase pressure is minus 80 to minus 85 kPa, and the liquid phase temperature in the third-effect evaporator is 30-35 ℃ and the gas phase pressure is minus 87 to minus 89 kPa.
Finally, tracking, monitoring and statistics show that under the process parameters, although the system runs without abnormal conditions, the time required for processing 500g of sodium azide is 65 minutes longer than that under the conditions of the parameters in the embodiment 1 (the sodium azide content in the one-effect evaporator is monitored, the sodium azide content is not detected as the cut-off time), the consumed fuel gas cost is 11 percent higher, and the electricity consumption cost is 18 percent higher.
Comparative example 2
This comparative example is substantially the same as example 1 except that the liquid phase temperature and the gas phase pressure are different in step S140. Specifically, in the comparative example, the temperature of a circulating hot water system is controlled through a temperature monitor and a pressure monitor which are arranged on a first-effect evaporator, a second-effect evaporator and a third-effect evaporator respectively, so that the liquid phase temperature in the first-effect evaporator is 65-70 ℃, the gas phase pressure is-40 to-50 kPa, the liquid phase temperature in the second-effect evaporator is 50-55 ℃, the gas phase pressure is-60 to-70 kPa, and the liquid phase temperature in the third-effect evaporator is 38-40 ℃ and the gas phase pressure is-83 to-86 kPa.
Finally, tracking, monitoring and statistics show that under the process parameters, although the system runs without obvious variation, the time required for treating 500g of sodium azide is not obviously prolonged compared with the conditions of the parameters in the embodiment 1, but the same amount of salt-containing wastewater is evaporated, the time is 33 minutes more, the consumed fuel gas cost is 16 percent, the electricity consumption cost is 17 percent, and bubble bursting sounds are occasionally generated in the triple-effect evaporation crystallizer (after monitoring and research, the extremely small amount of sodium azide is found to appear in the triple-effect evaporation crystallizer to be similar to small firecrackers due to temperature and collision.
Comparative example 3
This comparative example is substantially the same as example 1, except that the pH and ORP values are different in step S140. Specifically, in the comparative example, the addition amounts of sodium hypochlorite solution and sodium hydroxide solution are controlled by a pH monitor and an ORP value detector arranged on a first-effect evaporator, a second-effect evaporator and a third-effect evaporator respectively, so that the pH value of a liquid phase in the first-effect evaporator is 7.5-8, the ORP value is 350-400 mv, the pH value of the liquid phase in the second-effect evaporator is 7-7.5, the ORP value is 150-200 mv, and the pH value of the liquid phase in the third-effect evaporator is 8.5-9 and the ORP value is 600-650 mv.
Finally, tracking, monitoring and statistics show that under the process parameters, although the system runs without abnormal conditions, the time required for processing 500g of sodium azide is 73 minutes longer than that under the conditions of the parameters in the example 1 (the sodium azide content in the one-effect evaporator is monitored, the sodium azide content is not detected as the cut-off time), the consumed fuel gas cost is 14.5 percent higher, and the electricity consumption cost is 21 percent higher.
Comparative example 4
This comparative example is substantially the same as example 1, except that the pH and ORP values are different in step S140. Specifically, in the comparative example, the addition amounts of sodium hypochlorite solution and sodium hydroxide solution are controlled by a pH monitor and an ORP value detector arranged on a first-effect evaporator, a second-effect evaporator and a third-effect evaporator respectively, so that the pH value of a liquid phase in the first-effect evaporator is 10-11, the ORP value is 500-550 mv, the pH value of the liquid phase in the second-effect evaporator is 8.5-9.5, the ORP value is 300-400 mv, and the pH value of the liquid phase in the third-effect evaporator is 10-11 and the ORP value is 750-850 mv.
Finally, tracking, monitoring and statistics show that under the process parameters, although the system runs without abnormal conditions, and the time required for processing 500g of sodium azide is 15 minutes less than that under the conditions of the parameters in the embodiment 1 (the sodium azide content in the first-effect evaporator is monitored, the sodium azide content is not detected as the cut-off time), the ORP value and the pH value are detected to be almost unchanged in the second-effect crystal slurry, the proportion of sodium azide in the material which is fed into the first-effect crystal slurry in the same time is not obviously reduced, the total auxiliary material cost is increased by 19 percent by simply increasing the pH value and the oxidizing property and can not ensure that the sodium azide cannot escape, and the corrosion rate is found to be increased by 5 percent by tracking the corrosion amount of the same steel materials in the first-effect evaporator, the second-effect evaporator and the third-effect evaporator respectively.
Experimental example
The sample detection was performed on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator in the methods of examples 1-2 and comparative examples 1-4, and the specific detection method was spectrophotometry.
From the above table, it can be seen that examples 1-2 fall within the optimal process parameter selection range in order to achieve the goal of ensuring less escape of sodium azide in each effect, less time consumed, less auxiliary materials, less fuel gas and less electric power. It should be noted that, since the point values of the examples and the comparative examples of the present invention are not controllable, only the parameter ranges can be controlled.
The method for treating sodium azide by adopting the three-effect evaporation system does not need to construct a new production operation device, can be completed by technical improvement of the existing mature three-effect evaporation system 100 device, and reduces equipment investment; for example, the three-effect evaporation system 100 can be technically modified by the existing titanium alloy material, special materials are not required to be additionally developed or special equipment is not required to be built, and the investment of production equipment is reduced. The personnel participation degree is small, and the safety aspect can be better ensured; the sodium azide can be treated in a large scale, and the problem can be solved from the practical production; production operation can be performed on the existing operating triple-effect evaporation system 100 by adjusting process parameters, drainage replacement is not needed for the system, time intervals for switching equipment operation functions are reduced, and production cost is reduced. In the present invention, the process control includes: the liquid level control system of the evaporation chambers (the first-effect evaporator 110, the second-effect evaporator 120 and the third-effect evaporator 130), the circulating hot water pressure and flow control system, the circulating hot water temperature control system, the liquid phase temperature and the gas phase pressure of the evaporation chambers (the first-effect evaporator 110, the second-effect evaporator 120 and the third-effect evaporator 130) are controlled, and the liquid phase pH value and the ORP value of the evaporation chambers (the first-effect evaporator 110, the second-effect evaporator 120 and the third-effect evaporator 130) are controlled. The material water supply and stable adjustment of the one-key starting three-effect system can be realized, the step-by-step water supplementing and the circulating pump starting are not required to be operated by personnel, only the operation parameters are required to be monitored, and the workload of operators is reduced. The method for treating sodium azide by adopting the three-effect evaporation system provided by the invention can adjust the parameters of the three-effect evaporation system 100 which normally operates to the technological parameters capable of treating sodium azide through the DCS control system within 1 hour, thereby greatly saving the time cost and the labor cost. The method for treating sodium azide by adopting the three-effect evaporation system provided by the invention can treat sodium azide in batches, and personnel only need to place the sodium azide at the feeding chute 134, and the personnel do not participate in reaction operation, so that the safety coefficient is high.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present invention should be included in the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (10)

1. A method of treating sodium azide using a triple effect evaporation system comprising:
s110, starting solvent material supply of a first-effect evaporator, a second-effect evaporator and a third-effect evaporator step by step, controlling liquid levels by using liquid level monitors arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator, and starting a first-effect circulating pump of the first-effect evaporator, a second-effect circulating pump of the second-effect evaporator and a third-effect circulating pump of the third-effect evaporator for internal circulation;
s120, starting the water replenishing of the circulating hot water tank, controlling the liquid level by using a liquid level monitor arranged on the circulating hot water tank, and starting the circulating hot water system in an interlocking manner;
s130, after the pressure and the flow of the circulating hot water system meet the requirements, starting the fully premixed gas boiler in an interlocking way, adjusting the gas flow in an interlocking way according to the temperature of circulating hot water in the circulating hot water system, and establishing heat source supply of a three-effect evaporation system for normal operation;
s140, controlling the temperature of the circulating hot water system through a temperature monitor and a pressure monitor which are respectively arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator, so that the liquid phase temperature in the first-effect evaporator is 60-65 ℃, the gas phase pressure is-50 to-60 kPa, the liquid phase temperature in the second-effect evaporator is 45-50 ℃, the gas phase pressure is-70 to-80 kPa, and the liquid phase temperature in the third-effect evaporator is 35-38 ℃, and the gas phase pressure is-87 to-90 kPa;
s150, controlling the addition amounts of sodium hypochlorite solution and sodium hydroxide solution through a pH monitor and an ORP value detector which are respectively arranged on the first-effect evaporator, the second-effect evaporator and the third-effect evaporator, so that the pH value of a liquid phase in the first-effect evaporator is more than or equal to 8, the ORP value is more than or equal to 400mv, the pH value of the liquid phase in the second-effect evaporator is more than or equal to 7.5, the ORP value is more than or equal to 200mv, and the pH value of the liquid phase in the third-effect evaporator is more than or equal to 9, and the ORP value is more than or equal to 650mv;
and S160, after the requirements of the step S140 and the step S150 are met, introducing sodium azide into the triple-effect evaporation crystallizer for reaction, and conveying the reacted salt-containing wastewater into the first-effect evaporator and the double-effect evaporation crystallizer for desalting through a feeding mechanism.
2. The method of claim 1, wherein the upper limit of the pH of the liquid phase in the one-effect evaporator is 10, the upper limit of the ORP is 500 and mv, the upper limit of the pH of the liquid phase in the two-effect evaporator is 8.5, the upper limit of the ORP is 300 and mv, and the upper limit of the pH of the liquid phase in the three-effect evaporator is 10 and the upper limit of the ORP is 750 and mv.
3. The method for treating sodium azide by using a triple effect evaporation system according to claim 1, wherein the triple effect evaporation crystallizer is provided with a feeding chute for feeding the sodium azide and a negative pressure suction mechanism, a damping spring is arranged at the bottom of the feeding chute, one end of the negative pressure suction mechanism is communicated with the feeding chute, and the other end of the negative pressure suction mechanism is communicated with the inside of the triple effect evaporation crystallizer.
4. A method for treating sodium azide by using a triple effect evaporation system according to claim 3, wherein the suction gas flow rate of the negative pressure suction mechanism is 1-2 m 3 /s。
5. A method of treating sodium azide with a triple effect evaporation system according to claim 3, wherein the weight of sodium azide added to the feed chute at a time is 1 to 1000g.
6. The method for treating sodium azide by using a triple effect evaporation system according to claim 1, wherein an effective heater is arranged between the first effect evaporator and the first effect circulating pump, a double effect heater is arranged between the double effect evaporation crystallizer and the double effect circulating pump, and a triple effect heater is arranged between the triple effect evaporation crystallizer and the triple effect circulating pump;
and the gas outlet of the first-effect evaporator is communicated with the second-effect heater for heat gradient recovery, and the gas outlet of the second-effect evaporation crystallizer is communicated with the third-effect heater for heat gradient recovery.
7. The method for treating sodium azide by using a triple effect evaporation system according to claim 6, wherein the circulating water discharged from the circulating hot water tank is circulated back to the circulating hot water tank after being heated by the fully premixed gas boiler and then introduced into the first effect heater, the second effect preheater and the triple effect preheater.
8. The method for treating sodium azide by using a triple-effect evaporation system according to claim 6, wherein the feeding mechanism comprises a salt-containing wastewater pipeline, the salt-containing wastewater in the salt-containing wastewater pipeline is from wastewater or industrial wastewater after salt water separation of the triple-effect evaporation system, the salt-containing wastewater is preheated by a triple-effect preheater and then exchanges heat with the triple-effect heater, and the salt-containing wastewater is discharged to a pipeline connected with the first-effect evaporator and the first-effect circulating pump to feed the first-effect evaporator.
9. The method according to claim 6, wherein the feeding mechanism further comprises a two-effect transfer pump arranged between the one-effect circulation pump and the two-effect circulation pump, an inlet of the two-effect transfer pump is connected to a pipeline between the one-effect circulation pump and the one-effect heater, an outlet of the two-effect transfer pump is divided into two paths, one path is connected to the pipeline between the two-effect circulation pump and the two-effect heater, and the other path is connected to an inlet pipeline of the one-effect circulation pump.
10. The method of treating sodium azide with a triple effect evaporation system according to claim 1, wherein the concentration of sodium hypochlorite solution is 40-60wt% and the concentration of sodium hydroxide solution is 20-40wt%.
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