Cooling agent WS-5 production line and production process

Abstract

The invention provides a cooling agent WS-5 production line. The cooling agent WS-5 production line comprises a feeding module, a reaction module and a purification module, the feeding module comprises a raw material tank area, an alkaline water ingredient metering tank, a glycine ethyl ester hydrochloride water ingredient metering tank, a petroleum ether metering tank and a menthyl chloride metering tank; the reaction module comprises a multi-stage continuous reactor and a reaction liquid intermediate tank; the purification module comprises extraction equipment and distillation desolvation equipment, the cooling agent WS-5 production line can be used for continuous production of the cooling agent WS-5, and compared with an existing intermittent production mode, the safety and the production efficiency are greatly improved. Meanwhile, the invention further provides a production process of the cooling agent WS-5.

Description

Technical Field

[0001] The present invention relates to a cooling agent production process, in particular to a cooling agent WS-5 production line and production process. Background Art

[0002] The cooling agent WS-5 (also known as N-(ethoxycarbonylmethyl)-para-alkane-3-carboxamide) is the variety with the highest cooling intensity in the WS series. Its cooling sensation is mainly concentrated in the mouth and throat. The cooling intensity is about 3 to 4 times that of menthol. It is mainly used in hard candies, throat lozenges, toothpaste and other products.

[0003] Currently, there are numerous methods for preparing the cooling agent WS-5, but these methods also have certain drawbacks. For example, Chinese Patent CN119080629A discloses a menthamide cooling agent WS-5 and its preparation method. Menthol is oxidized to menthone, and p-methylphenylsulfonylmethyl isocyanide is used as a source of nitrile groups. The nitrile groups are introduced via Van Leusen reduction nitrilation to obtain nitrile menthol. The nitrile menthol is then dissolved in hydrochloric acid and reacted to obtain menthic acid. Menthic acid, ethyl glycine, pyridine, and ethyl acetate are mixed and a condensation reagent is added to obtain the cooling agent WS-5. However, this preparation method uses toxic substances, p-methylphenylsulfonylmethyl isocyanide and pyridine, and currently has not been commercialized. Chinese Patent CN103694130A discloses a high-yield synthesis method for menthamide. Menthamide is prepared by reacting menthonitrile with triethyl phosphate using polyphosphoric acid as a catalyst. However, this method uses the highly toxic substance sodium cyanide, which poses high production risks and is difficult to mass-produce.

[0004] At the same time, most of the production processes of the cooling agent WS-5 on the market currently use an intermittent production process, which not only has a long production cycle, but also requires manual feeding, adjustment and other operations during the production process. It is difficult to accurately control the reaction process, which is not conducive to improving product quality and yield, and is also prone to threatening workers' health.

[0005] In order to solve the above problems, people have been seeking an ideal technical solution. Summary of the Invention

[0006] The purpose of the present invention is to provide a cooling agent WS-5 production line and production process in view of the deficiencies in the prior art.

[0007] In order to achieve the above object, the technical solution adopted by the present invention is:

[0008] A cooling agent WS-5 production line includes a feeding module, a reaction module and a purification module;

[0009] The feeding module includes a raw material tank area, an alkaline water batching metering tank, a glycine ethyl ester hydrochloride batching metering tank, a petroleum ether metering tank, and a menthyl chloride metering tank; the reaction module includes a multi-stage continuous reactor and a reaction liquid intermediate tank; the purification module includes extraction equipment and distillation and desolventizing equipment;

[0010] The raw material storage tanks in the raw material tank area are connected to the alkaline water ingredient metering tank, glycine ethyl ester hydrochloride water ingredient metering tank, petroleum ether metering tank and menthyl chloride metering tank through pipelines; the alkaline water ingredient metering tank, glycine ethyl ester hydrochloride water ingredient metering tank, petroleum ether metering tank and menthyl chloride metering tank are respectively connected to the feed port of the multi-stage continuous reactor, and the discharge port of the multi-stage continuous reactor is connected to the feed port of the reaction liquid intermediate tank; the discharge port of the reaction liquid intermediate tank is connected to the feed port of the extraction equipment, and the organic phase discharge port of the extraction equipment is connected to the distillation and desolventizing equipment.

[0011] The multi-stage continuous reactor includes several reactors connected in series. The height of each reactor decreases in sequence. The reactor with the highest position is the first reactor. The other reactors are the second reactor, the third reactor, etc. from high to low. Each metering tank feeds the first reactor of the multi-stage continuous reactor respectively. The overflow port of the first reactor is connected to the feed port of the second reactor, and the cycle continues until the last reactor.

[0012] The extraction equipment includes a first centrifugal extractor and a second centrifugal extractor; the discharge port of the reaction liquid intermediate tank is connected to the feed port of the first centrifugal extractor; the organic phase discharge port of the first centrifugal extractor is connected to the feed port of the second centrifugal extractor, and the water phase discharge port of the first centrifugal extractor is connected to the feed port of the wastewater intermediate tank; the organic phase discharge port of the second extractor is connected to the feed port of the coarse material intermediate tank.

[0013] The distillation and desolventizing equipment includes two groups of continuous distillation kettles connected in series, the discharge port of the crude material intermediate tank is connected to the first continuous distillation kettle, the bottom discharge port of the first continuous distillation kettle is connected to the feed port of the second continuous distillation kettle, and the top discharge port of the second continuous distillation kettle is connected to the finished product intermediate tank; the top discharge port of the first continuous distillation kettle is connected to the petroleum ether intermediate tank, and a condenser is arranged between the petroleum ether intermediate tank and the first continuous distillation kettle; the bottom discharge port of the second continuous distillation kettle is connected to the high-boiling material intermediate tank.

[0014] The raw material tank area includes menthyl chloride storage tanks, petroleum ether storage tanks and liquid alkali storage tanks.

[0015] The menthyl chloride metering tank, petroleum ether metering tank, alkaline water ingredient metering tank, and glycine ethyl hydrochloride water metering tank are respectively equipped with weighing modules, and the tap water is installed with a metering water meter; the material pump of each raw material storage tank is interlocked with the weighing module of the corresponding metering tank, and the metering water meter is interlocked with the water inlet shut-off valve, and the opening and closing of the material pump of the corresponding raw material storage tank and the water inlet shut-off valve are adjusted according to the information of the weighing module.

[0016] Each reactor is equipped with an online content detector for online monitoring of the ratio and pH value of the three materials in each reactor. The online content detector is interlocked with the parameters of each feed pump of the reactor, and the opening and closing of the feed pump are adjusted according to the detection information of the online content detector.

[0017] A production process of the cooling agent WS-5 is provided, which utilizes the cooling agent WS-5 production line.

[0018] The alkaline water ingredient metering tank, glycine ethyl hydrochloride water ingredient metering tank, petroleum ether metering tank and menthyl chloride metering tank are respectively used to load the multi-stage continuous reactor; then the reaction is carried out at 10-50°C, and the reaction product in the multi-stage continuous reactor enters the reaction liquid intermediate tank, and then enters the extraction equipment for automatic water separation and extraction to obtain WS-5 crude material; the WS-5 crude material enters the distillation and desolventizing equipment for distillation and desolventizing at 90-160°C to obtain WS-5 product.

[0019] Compared to existing technologies, the present invention provides a production line and process for the cooling agent WS-5. This improves upon the existing batch production process for the cooling agent WS-5, enabling continuous production. The WS-5 content in the reaction liquid during the continuous reaction is stable and ≥97%, and the final WS-5 content in the finished product after distillation is ≥99.5%. Specifically, the material is transported through a pipeline, eliminating the need for manual feeding. Menthyl chloride, petroleum ether and liquid alkali materials are transported to the workshop metering tank via a tank area pump, avoiding the safety risk of material transportation; the production process of the present invention adopts a 500L reactor for continuous feeding and continuous discharging, and produces 2 tons of qualified reaction liquid in 24 hours. The annual maximum production capacity reaches 100 tons of finished product production capacity, with an output value of 45 million yuan. Compared with single-kettle production, the production capacity is increased by 3.3 times compared with the reactor batch process, the reaction time is short, and the production efficiency is high; preferably, the glycine ethyl ester hydrochloride and alkaline water ingredient metering tanks are A / B tanks, one for backup and the other for use, and the reactor is continuously fed with a metering pump, the feeding rate is stable, the process control indicators are stable, and the reaction liquid quality is stable. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a simplified flow chart of the cooling agent WS-5 production line of the present invention.

[0021] Figure 2 It is a structural diagram of the cooling agent WS-5 production line of the present invention.

[0022] Figure 3 yes Figure 2 An enlarged schematic diagram of the connection structure of the medium-alkali water ingredient metering tank.

[0023] Figure 4 yes Figure 2 An enlarged schematic diagram of the connection structure of the metering tank for the glycine ethyl ester hydrochloride aqueous solution.

[0024] Figure 5 yes Figure 2 An enlarged schematic diagram of the connection structure of the PetroChina ether metering tank.

[0025] Figure 6 yes Figure 2 An enlarged schematic diagram of the connection structure of the menthyl chloride metering tank.

[0026] Figure 7 yes Figure 2 An enlarged schematic diagram of the connection structure of the first reactor.

[0027] Figure 8 yes Figure 2 An enlarged schematic diagram of the connection structure of the second reactor.

[0028] Figure 9 yes Figure 2 An enlarged schematic diagram of the connection structure of the tail gas absorption tower.

[0029] In the figure: V3001. Alkaline water ingredient metering tank; V3002. Glycine ethyl ester hydrochloride water ingredient metering tank; V3003. Menthyl chloride metering tank; V3004. Petroleum ether metering tank; V3005. Reaction liquid intermediate tank; V3006. Wastewater intermediate tank; V3007. WS-5 crude material intermediate tank; V3008. Petroleum ether intermediate tank; V3009. WS-5 finished product intermediate tank; V3010. High boiling point intermediate tank; R3001. First reactor; R3002. Second reactor; R3003. First continuous distillation kettle; R3004. Second continuous distillation kettle; T3001. Tail gas absorption tower; X3001 First centrifugal extractor; X3002. Second centrifugal extractor; E3001. First condenser; E3002. Second condenser; E3003. Third condenser. DETAILED DESCRIPTION

[0030] The technical solution of the present invention is further described in detail below through specific implementation methods.

[0031] In the description of the invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "provided with", "connected", etc. should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be a communication between the two components. "Installed", "provided with", "connected", etc. can adopt conventional means in the prior art, such as: integral setting, snap-on installation, welding connection, adhesive connection, bolt connection, etc. For ordinary technicians in this field, they can understand the specific meanings of the above terms in the present invention according to specific circumstances and select appropriate connection, setting or installation methods in the prior art.

[0032] like Figure 1-9 As shown, this embodiment provides a cooling agent WS-5 production line, including a feeding module, a reaction module and a purification module;

[0033] The feeding module includes the raw material tank area, alkaline water batching metering tank V3001, glycine ethyl ester hydrochloride batching metering tank V3002, petroleum ether metering tank V3004 and menthyl chloride metering tank V3003; the reaction module includes a multi-stage continuous reactor and a reaction liquid intermediate tank V3005; the purification module includes extraction equipment and distillation and desolventizing equipment;

[0034] The raw material storage tanks in the raw material tank area are connected to the alkaline water ingredient metering tank V3001, the glycine ethyl ester hydrochloride water ingredient metering tank V3002, the petroleum ether metering tank V3004 and the menthyl chloride metering tank V3003 through corresponding pipelines; the alkaline water ingredient metering tank, the glycine ethyl ester hydrochloride water ingredient metering tank, the petroleum ether metering tank V3004 and the menthyl chloride metering tank V3003 are respectively connected to the feed port of the multi-stage continuous reactor, the discharge port of the multi-stage continuous reactor is connected to the feed port of the reaction liquid intermediate tank V3005; the discharge port of the reaction liquid intermediate tank V3005 is connected to the feed port of the extraction equipment, and the organic phase discharge port of the extraction equipment is connected to the distillation and desolventizing equipment. Preferably, the glycine ethyl ester hydrochloride water ingredient metering tank V3002, the alkaline water ingredient metering tank V3001, the petroleum ether metering tank V3004 and the menthyl chloride metering tank V3003 are A / B tanks, one for backup and the other for use, and the reactor is continuously fed with a metering pump.

[0035] In one embodiment, a multi-stage continuous reactor includes several reactors connected in series, and the heights of the reactors decrease in sequence. The reactor with the highest position is the first reactor R3001, and the other reactors are the second reactor R3002, the third reactor, etc. from high to low. Each metering tank feeds the first reactor R3001 of the multi-stage continuous reactor, and the overflow port of the first reactor R3001 is connected to the feed port of the second reactor R3002, and the cycle continues until the last reactor. Specifically, two 500L reactors are set up in this embodiment. The exhaust ports of the first reactor R3001 and the second reactor R3002 are correspondingly connected to the first condenser E3001 and the third condenser E3003E3002. The condensed gas enters the tail gas absorption tower T3001 for spray absorption; the overflow port of the second reactor R3002 is connected to the feed port of the reaction liquid intermediate tank V3005, and the discharge port of the reaction liquid intermediate tank V3005 is connected to the first centrifugal extractor X3001; the reactor adopts a jacketed reactor, which is convenient for temperature adjustment.

[0036] In one embodiment, the extraction equipment includes a first centrifugal extractor X3001 and a second centrifugal extractor X3002; the discharge port of the reaction liquid intermediate tank V3005 is connected to the feed port of the first centrifugal extractor X3001; the organic phase discharge port of the first centrifugal extractor X3001 is connected to the feed port of the second centrifugal extractor X3002, and the water phase discharge port of the first centrifugal extractor X3001 is connected to the feed port of the wastewater intermediate tank V3006; the organic phase discharge port of the second extractor is connected to the feed port of the coarse material intermediate tank.

[0037] In one embodiment, the distillation and desolventizing equipment includes two groups of continuous distillations in series, the discharge port of the crude material intermediate tank is connected to the first continuous distillation kettle R3003, the bottom discharge port of the first continuous distillation kettle R3003 is connected to the feed port of the second continuous distillation kettle R3004, and the top discharge port of the second continuous distillation kettle R3004 is connected to the finished product intermediate tank; the top discharge port of the first continuous distillation kettle R3003 is connected to the petroleum ether intermediate tank V3008, which is convenient for recycling the solvent. A third condenser is arranged between the petroleum ether intermediate tank V3008 and the first continuous distillation kettle R3003; the bottom discharge port of the second continuous distillation kettle R3004 is connected to the high-boiling material intermediate tank V3010.

[0038] In one embodiment, the raw material tank area includes a menthyl chloride storage tank, a petroleum ether storage tank and a liquid caustic soda storage tank.

[0039] In one embodiment, the menthyl chloride metering tank, petroleum ether metering tank V3004, alkaline water ingredient metering tank, and glycine ethyl hydrochloride water metering tank are respectively provided with weighing modules, and the tap water is installed with a metering water meter; the material pump of each raw material storage tank is interlocked with the weighing module of the corresponding metering tank, and the metering water meter is interlocked with the water inlet shut-off valve, and the opening and closing of the material pump of the corresponding raw material storage tank and the water inlet shut-off valve are adjusted according to the information of the weighing module.

[0040] In one embodiment, each reactor is equipped with an online content detector for online monitoring of the ratio and pH value of the three materials in each reactor. The online content detector is interlocked with the parameters of each feed pump of the reactor, and the opening and closing of the feed pump are adjusted according to the detection information of the online content detector.

[0041] It should be noted that in order to facilitate material transportation, conveying pumps and various control valves can be set as needed; for example: metering pumps P3001-P3007 for feeding the reactor; at the same time, the various intelligent chain control adjustments in the present invention are all achieved through the common control circuits in the existing technology and the corresponding controllers, detection elements, etc.

[0042] This embodiment also provides a production process for the cooling agent WS-5, which is produced using the cooling agent WS-5 production line described above.

[0043] The alkaline water ingredient metering tank V3001, the glycine ethyl hydrochloride water ingredient metering tank V3002, the petroleum ether metering tank V3004 and the menthyl chloride metering tank V3003 are respectively used to load the multi-stage continuous reactor; then the reaction is carried out at 10-50°C, and the reaction product in the multi-stage continuous reactor enters the reaction liquid intermediate tank V3005, and then enters the extraction equipment for automatic water separation and extraction to obtain WS-5 crude material; the WS-5 crude material enters the distillation and desolventizing equipment for distillation and desolventizing at 90-160°C to obtain WS-5 product.

[0044] The above embodiments can be combined with each other.

[0045] The best way to use the cooling agent WS-5 production line is as follows:

[0046] 1. Measuring tank feeding steps:

[0047] 1. Check that the alkaline water metering tank V3001 and metering pump P3001, glycine ethyl hydrochloride aqueous solution metering tank V3002 and metering pump P3002, menthyl chloride (CLAG-3) metering tank V3003 and metering pump P3003, petroleum ether metering tank V3004 and metering pump P3004 are intact and ready for feeding.

[0048] 2. Calibrate the alkaline water metering tank V3001 (V3001A / B), glycine ethyl hydrochloride aqueous solution metering tank V3002 (V3002A / B), menthyl chloride metering tank V3003 (V3003A / B), petroleum ether metering tank V3004 (V3004A / B) weighing, liquid level and shut-off valve instruments and valves to ensure they are sensitive and accurate.

[0049] 3. Set the 30% liquid alkali (sodium hydroxide) feed parameters of the alkali water ingredient metering tank V3001 (V3001A / B) and the interlocking parameters of the tank area material pump and the metering tank weighing module in a 1:1 ratio, set the interlocking parameters of the water inlet control valve and the water meter, and the central control room remotely starts the feed pump to feed the workshop metering tank. When the feed volume reaches 400kg in the parameters, the tank area material pump will automatically stop, and when the tap water inflow reaches 400Kg, the water inlet control valve will automatically close. No manual remote operation is required subsequently, and the metering tank will automatically operate intelligently when it reaches the lowest liquid level.

[0050] 4. Set the glycine ethyl ester hydrochloride aqueous solution batching metering tank V3002 (V3002A / B) glycine ethyl ester hydrochloride and tap water feeding parameters as well as the interlocking parameters of the screw feeder, tap water control valve and metering tank weighing module in a ratio of 1:2. The central control room remotely starts the screw feeder and opens the water inlet control valve to feed the workshop metering tank. When the glycine ethyl ester hydrochloride reaches the parameter feed volume of 300kg, the screw feeder automatically stops. When the tap water inlet volume reaches 600Kg, the water inlet control valve automatically closes. No manual remote operation is required subsequently. When the metering tank reaches the lowest liquid level, it will automatically operate intelligently.

[0051] 5. Set the menthyl chloride feeding parameters of the menthyl chloride metering tank V3003 (V3003A / B) and the interlocking parameters of the tank area material pump and the metering tank weighing module. The central control room remotely starts the tank area material pump to feed the workshop metering tank. When the feed volume of 800kg in the parameter is reached, the material pump automatically stops. No manual remote operation is required subsequently. When the metering tank reaches the lowest liquid level, it will automatically operate intelligently.

[0052] 6. Set the petroleum ether feeding parameters of the petroleum ether metering tank V3004 (V3004A / B) and the interlocking parameters of the tank area material pump and the metering tank weighing module. The central control room remotely starts the tank area material pump to feed the metering tank in the workshop. When the feed volume of 600kg in the parameter is reached, the material pump automatically stops. No manual remote operation is required subsequently. When the metering tank reaches the lowest liquid level, it will automatically operate intelligently.

[0053] Second, the reaction kettle reaction steps:

[0054] 1. Check that the equipment reactor (R3001 / R3002) and the reaction liquid intermediate tank V3005 are intact and ready for feeding.

[0055] 2. Calibrate the temperature, liquid level, pressure, current, online pH, automatic regulating valve of the reactor (R3001 / R3002) and the liquid level, temperature, flow meter, shut-off valve and other instruments and valves of the reaction liquid intermediate tank (V3005) to ensure they are sensitive and accurate.

[0056] 3. The central control room remotely starts the alkaline water feed pump (P3001), brine feed pump (P3002), menthyl chloride feed pump (P3003) and petroleum ether feed pump (P3004), and sets the operating frequency of the alkaline water feed pump (P3001) to 30 Hz, flow rate 20-60 kg / h, the operating frequency of the brine feed pump (P3002) to 35 Hz, flow rate 25-80 kg / h, the operating frequency of the menthyl chloride feed pump (P3003) to 30 Hz, 10-30 kg / h, and the operating frequency of the petroleum ether feed pump (P3004) to 35 Hz, 25-80 kg / h, to continuously feed the reactor R3001.

[0057] 5. When the material in reactor R3001 reaches one-third, the central control room remotely starts the stirring of the reactor and opens the jacket regulating valve to cool the reactor (R3001 / R3002): the valve interlocking the reactor temperature is set to 10-50℃, and the cooling water valve will automatically maintain the reactor temperature within the range of 10-50℃ according to the given interlocking value.

[0058] 6. The high alarm of temperature and liquid level in reactor (R3001 / R3002) interlocks the feed pumps P3001~P3004 to stop feeding, ensuring that the reaction temperature and reactor liquid level are automatically controlled within the normal range. When the liquid level of reactor R3001 reaches the overflow outlet, it automatically flows into reactor (R3002).

[0059] 7. When the material in reactor R3002 reaches one-third, the central control room remotely starts the stirring of reactor (R3002) and opens the jacket regulating valve to cool down reactor R3002: the valve interlocking reactor temperature is set to 10-50℃, and the cooling water valve will automatically maintain the reactor temperature within the range of 10-50℃ according to the given interlocking value.

[0060] 8. When the liquid level of the reactor (R3002) reaches the outlet, it automatically flows into the reaction liquid intermediate tank (V3005).

[0061] 9. In this way, the raw materials continuously enter the reactor R3001, then flow into the reactor R3002, and finally continuously flow out of the reactor R3002 into the reaction liquid intermediate tank V3005. The whole process is automatically fed, and the temperature, liquid level, etc. are automatically controlled. Except for the first feeding, no manual operation is required. The whole process is automated and intelligent, with continuous closed reaction and feeding and discharging.

[0062] 10. Both reactors (R3001 and R3002) are equipped with online content detectors that continuously monitor the proportions of each material in each reactor. Based on these proportions, the feed ratios of P3001 to P3004 are intelligently interlocked to adjust, maintaining the material ratios within the normal range. The system also detects product content and any unreacted raw material residues, intelligently interlocking to reduce or increase the feed amounts of P3001 to P3004 to ensure that the intermediate product continuously flowing out of reactor R3002 is of acceptable quality.

[0063] 11. The product contents of reactor R3001 and reactor R3002 are 80% to 90% and 90% to 97% respectively. The product content of reactor R3002 outlet is always above 97%.

[0064] 3. Brine separation, extraction and reaction liquid washing process:

[0065] 1. Separate the organic phase and brine.

[0066] The central control room remotely opens the bottom valve of the reaction liquid intermediate tank V3005, then starts the first centrifugal extractor X3001 [model: CWL350], starts the feed pump (P3005), feeds the first centrifugal extractor X3001, and outputs the organic phase of the material to the centrifugal extractor X3002 at the discharge port, and outputs the sodium chloride brine continuously into the wastewater intermediate tank V3006 at the discharge port.

[0067] 2. Organic phase water washing

[0068] According to the centrifugal extractor operating procedures, start the second centrifugal extractor X3002, control the water inlet regulating valve (regulating valve FV3002; flow meter: FTX3002) to feed water into the second centrifugal extractor X3002, so that the mass ratio of the organic phase from the second centrifugal extractor X3002 to water is 3:1~4:1, and after washing and separation in the second centrifugal extractor X3002, the pH value of the water phase is measured to be 7-8, and the pH meter monitored in the main control room is qualified. The water phase enters the wastewater intermediate tank V3006, and the organic phase is WS-5 coarse material, which enters the WS-5 coarse material intermediate tank V3007 for standby use.

[0069] 4. Continuous distillation and desolventizing process:

[0070] (1) Automated continuous desolventizing:

[0071] The central control room remotely opens the outlet valve (XV-V3007) of the crude material intermediate tank V3007 and the cooling water inlet valve (TV-E3003) of the condenser E3003 in sequence, and remotely starts the feed pump (P3007) to start feeding the (light component) first continuous distillation kettle R3003; the (light component) first continuous distillation kettle R3003 is fed to the liquid level of 30%-50%, and the central control room remotely opens the jacket steam regulating valve (TV-V3003) to control the temperature, raises the temperature in the temperature-controlled kettle to 120-150°C, and maintains the liquid level in the distillation kettle at 60%-80% (while continuously feeding and discharging the material, ensure the liquid level balance), and continuously discharges the material from the bottom of the tower to the second continuous distillation kettle R3004 (WS-5 content ≥98%).

[0072] (2) Automated continuous distillation:

[0073] The central control room remotely opens the cooling water inlet valve (XV-E3004) of the top condenser of the second continuous distillation kettle R3004, and then opens the (light component) bottom discharge valve of the first continuous distillation kettle R3003, and the material from the bottom of the first continuous distillation kettle R3003 continuously enters the second continuous distillation kettle R3004.

[0074] The second continuous distillation kettle R3004 is fed to a liquid level of 30%-50%. The central control room remotely opens the jacket steam regulating valve (TV-R3004a) to control the temperature, raises the temperature in the kettle to 120-160°C, and maintains the liquid level in the distillation kettle at 60%-80%. The finished product of the cooling agent WS-5 is continuously produced from the top of the tower and sent to the product receiving tank V3009. The WS-5 content is ≥99.5%. The regulating valve (TV-R3004b) at the bottom of the kettle continuously produces high-waste and sends it to the high-boiling intermediate tank V3010.

[0075] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to preferred embodiments, ordinary technicians in the field should understand that the specific implementation methods of the present invention can still be modified or some technical features can be replaced by equivalents without departing from the spirit of the technical solutions of the present invention. They should all be included in the scope of the technical solutions claimed for protection by the present invention.

Claims

1. A cooling agent WS-5 production line, characterized by: It includes a feeding module, a reaction module and a purification module; The feeding module includes a raw material tank area, an alkaline water batching metering tank, a glycine ethyl ester hydrochloride batching metering tank, a petroleum ether metering tank, and a menthyl chloride metering tank; the reaction module includes a multi-stage continuous reactor and a reaction liquid intermediate tank; the purification module includes extraction equipment and distillation and desolventizing equipment; The raw material storage tanks in the raw material tank area are connected to the alkaline water ingredient metering tank, glycine ethyl ester hydrochloride water ingredient metering tank, petroleum ether metering tank and menthyl chloride metering tank through pipelines; the alkaline water ingredient metering tank, glycine ethyl ester hydrochloride water ingredient metering tank, petroleum ether metering tank and menthyl chloride metering tank are respectively connected to the feed port of the multi-stage continuous reactor, and the discharge port of the multi-stage continuous reactor is connected to the feed port of the reaction liquid intermediate tank; the discharge port of the reaction liquid intermediate tank is connected to the feed port of the extraction equipment, and the organic phase discharge port of the extraction equipment is connected to the distillation and desolventizing equipment.

2. The cooling agent WS-5 production line according to claim 1, characterized in that: The multi-stage continuous reactor includes several reactors connected in series. The height of each reactor decreases in sequence. The reactor with the highest position is the first reactor. The other reactors are the second reactor, the third reactor, etc. from high to low. Each metering tank feeds the first reactor of the multi-stage continuous reactor respectively. The overflow port of the first reactor is connected to the feed port of the second reactor, and the cycle continues until the last reactor.

3. The cooling agent WS-5 production line according to claim 2, characterized in that: The extraction equipment includes a first centrifugal extractor and a second centrifugal extractor; the discharge port of the reaction liquid intermediate tank is connected to the feed port of the first centrifugal extractor; the organic phase discharge port of the first centrifugal extractor is connected to the feed port of the second centrifugal extractor, and the water phase discharge port of the first centrifugal extractor is connected to the feed port of the wastewater intermediate tank; the organic phase discharge port of the second extractor is connected to the feed port of the coarse material intermediate tank.

4. The cooling agent WS-5 production line according to claim 3, characterized in that: The distillation and desolventizing equipment includes two groups of continuous distillation kettles connected in series, the discharge port of the crude material intermediate tank is connected to the first continuous distillation kettle, the bottom discharge port of the first continuous distillation kettle is connected to the feed port of the second continuous distillation kettle, and the top discharge port of the second continuous distillation kettle is connected to the finished product intermediate tank; the top discharge port of the first continuous distillation kettle is connected to the petroleum ether intermediate tank, and a condenser is arranged between the petroleum ether intermediate tank and the first continuous distillation kettle; the bottom discharge port of the second continuous distillation kettle is connected to the high-boiling material intermediate tank.

5. The cooling agent WS-5 production line according to claim 4, characterized in that: The raw material tank area includes menthyl chloride storage tanks, petroleum ether storage tanks and liquid alkali storage tanks.

6. The cooling agent WS-5 production line according to claim 5, characterized in that: The cooling agent WS-5 production line according to claim 2 is characterized in that: the menthyl chloride metering tank, petroleum ether metering tank, alkaline water ingredient metering tank, and glycine ethyl hydrochloride water metering tank are respectively provided with weighing modules, and the tap water is installed with a metering water meter; the material pump of each raw material storage tank is interlocked with the weighing module of the corresponding metering tank, and the metering water meter is interlocked with the water inlet shut-off valve, and the opening and closing of the material pump of the corresponding raw material storage tank and the water inlet shut-off valve are adjusted according to the information of the weighing module.

7. The cooling agent WS-5 production line according to claim 6, characterized in that: Each reactor is equipped with an online content detector for online monitoring of the ratio and pH value of the three materials in each reactor. The online content detector is interlocked with the parameters of each feed pump of the reactor, and the opening and closing of the feed pump are adjusted according to the detection information of the online content detector.

8. A production process for a cooling agent WS-5, characterized by: The product is produced using the cooling agent WS-5 production line according to any one of claims 1 to 7.

9. The production process of the cooling agent WS-5 according to claim 8, characterized in that: The alkaline water ingredient metering tank, glycine ethyl hydrochloride water ingredient metering tank, petroleum ether metering tank and menthyl chloride metering tank are respectively used to load the multi-stage continuous reactor; then the reaction is carried out at 10-50°C, and the reaction product in the multi-stage continuous reactor enters the reaction liquid intermediate tank, and then enters the extraction equipment for automatic water separation and extraction to obtain WS-5 crude material; the WS-5 crude material enters the distillation and desolventizing equipment for distillation and desolventizing at 90-160°C to obtain WS-5 product.

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