Reactor for improving synthesis proportioning precision of methylhydrazine

Abstract

The utility model relates to a reactor capable of improving the synthesis proportioning precision of methylhydrazine, which belongs to the technical field of methylhydrazine production equipment and comprises an ammonia water intermediate tank, a sodium hypochlorite intermediate tank, a first feeding mixer, a second feeding mixer, a third feeding mixer, a fourth feeding mixer, a fourth feeding mixer and a fourth feeding mixer. An inner pipe outlet of the one-step reactor is connected with a second feeding blender through an ultrasonic degassing device, a discharge port of the monomethylamine solution intermediate tank is connected with the second feeding blender, a discharge port of the second feeding blender is connected with a second Venturi tube, a negative pressure port of the second Venturi tube is connected with the ultrasonic degassing device, and a negative pressure port of the second Venturi tube is connected with the ultrasonic degassing device. The outlet of the second venturi tube is connected with the inlet of the inner tube of the two-step reactor, and the outlet of the inner tube of the two-step reactor is connected with the methylhydrazine synthesis liquid storage tank. The device disclosed by the utility model is simple in structure and reasonable in design, and can improve the proportioning precision, the reaction stability and the yield, and the methylhydrazine synthesis proportioning precision.

Description

TECHNICAL FIELD

[0001] The utility model relates to a reactor of improving methylhydrazine synthetic proportioning precision belongs to methylhydrazine production equipment technical field. BACKGROUND

[0002] Methylhydrazine is synthesized by chloramine method, sodium hypochlorite and ammonia are mixed through a mixer, enter the first tubular reactor to react, generate the aqueous solution of chloramine, the reaction liquid is mixed with monomethylamine through a mixer after the reactor, enters the second tubular reactor to react, finally generates the aqueous solution of methylhydrazine, and the reaction formula is as follows:

[0003] NaClO+NH3 NH2+NaOH,

[0004] NH2Cl+NaOH+CH3NH2 CH3NHNH2+NaCl+H2O,

[0005] Among them, in the first step reaction process, there are many side reactions of generating gas:

[0006] 2NaClO 2NaCl+O2 ，

[0007] 3NaCl0+2NH3 3NaCl+3H2O+N2 ，

[0008] 3NH2Cl+3NaOH 3NaCl+3H2O+N2 +NH3 ，

[0009] Especially oxygen and nitrogen, which are insoluble in water, cause the generation of bubbles in the tubular reactor, and the mixing of monomethylamine before the second reactor exists the problem of inaccurate proportioning, which leads to large fluctuation of reaction results and low yield.

[0010] The Chinese patent with publication number CN 103263884 discloses a synthetic reactor and a chloramine method for synthesizing methylhydrazine, which has the characteristics of high yield and selectivity, low energy consumption and less waste. The reaction device only makes a process from solution preparation to cooling after the reaction in the existing production device. High-efficiency mixing fillers are used in the ammonia water preparation unit, the sodium hypochlorite preparation unit and the methylhydrazine generation unit to strengthen the mixing process of the materials, but it cannot be said that it is a catalytic effect, and it cannot discharge the gas generated by the reaction, and it cannot solve the problem of proportioning. It cannot improve the yield and selectivity from the principle. Under the condition of 40℃, the saturation concentration of sodium hydroxide is 56.4%. In the implementation example of the patent, 65% sodium hydroxide is prepared under the condition of 40℃, and there must be a blockage problem in the material conveying process. Moreover, in the combination of the first, second and third embodiments in the implementation example, the concentrations of ammonia water and sodium hydroxide are successively increased, and the content of chloramine is successively decreased. In addition, 30% sodium hydroxide solution absorbs chlorine to generate sodium hypochlorite, and the conversion rate is 100%, and the content of sodium hypochlorite is 22.05%; after the conversion of 47.5% sodium hydroxide solution, the content of sodium hypochlorite is 31.10%. However, the patent states that the content of sodium hypochlorite is 40% and 37.5% respectively. This is completely contrary to the law of conservation of mass and conservation of mass. Therefore, improving the yield and selectivity is just empty talk, and there is no theoretical and practical basis.

[0011] The patent with publication number CN206868207U is entitled as a methylhydrazine synthesis device, the patent with publication number CN206715951U is entitled as a methylhydrazine preparation device, the patent with publication number CN206715925U is entitled as a new reactor for synthesizing methylhydrazine by chloramine method, the patent with publication number CN206951175U is entitled as a reaction device for reducing evaporation energy consumption in the synthesis of methylhydrazine by chloramine method, the patent with publication number CN206715947U is entitled as a reaction kettle for removing trace monomethylamine impurities in 42% methylhydrazine product, and the patent with publication number CN206715924U is entitled as a reaction equipment for removing trace ammonia impurities in 42% methylhydrazine product. The above-mentioned patents only design a reactor which is convenient to clean, and can be considered as a continuous stirred tank reactor in the full mixed flow reactor. For the production of methylhydrazine by chloramine method, the chloramine generated in the first step reaction can be easily and quickly decomposed, and the heat release is large. In order to shorten the residence time, it is necessary to require high heat transfer efficiency. Obviously, such a reactor is not suitable for use in the synthesis reaction of chloramine method, and it is also difficult to improve the efficiency of the reaction. Practical new type

[0012] In order to solve the technical problems existing in the prior art, the utility model provides a reactor which has simple structure, reasonable design, can improve the proportioning accuracy, improve the stability and yield of the reaction, and improve the proportioning accuracy of the methylhydrazine synthesis.

[0013] In order to achieve the above object, the utility model adopts the technical scheme that is a reactor for improving methylamine synthesis matching precision, including ammonia water intermediate tank, sodium hypochlorite intermediate tank, monomethylamine solution intermediate tank, methylamine synthesis liquid storage tank, one step reactor and two step reactor, the one step reactor and two step reactor all internally have inner tubes, the outer portion of the inner tube is equipped with an outer tube, the discharge port of ammonia water intermediate tank, sodium hypochlorite intermediate tank is connected with first feed mixer through control valve, first metering pump respectively, the discharge port of first feed mixer is connected with the inner tube import of one step reactor, the outer tube of one step reactor is provided with refrigerant import and refrigerant export, the inner tube export of one step reactor is connected with the feed end of ultrasonic degassing device, the discharge end of ultrasonic degassing device is connected with second feed mixer, the discharge port of monomethylamine solution intermediate tank is connected with second feed mixer through second metering pump, the discharge port of second feed mixer is connected with second venturi, the negative pressure port of second venturi is connected with ultrasonic degassing device, the outlet of second venturi is connected with the inner tube import of two step reactor, the inner tube export of two step reactor is connected with methylamine synthesis liquid storage tank, the outer tube of two step reactor is provided with heat medium import and heat medium export.

[0014] Preferably, the ultrasonic degassing device includes a housing, a first venturi and an ultrasonic vibrator, the first venturi and the ultrasonic vibrator are installed in the housing, the inlet of the first venturi is connected with the inner tube outlet of the one step reactor through a first hose, the outlet of the first venturi is connected with the inlet pipe of the second feed mixer through a second hose, the negative pressure port of the first venturi is also connected with a third hose, the third hose is connected with the negative pressure port of the second venturi through a connecting pipe.

[0015] Preferably, the negative pressure port pressure of the second venturi is less than that of the first venturi.

[0016] Compared with the prior art, the utility model has the following technical effects: the utility model has simple structure and reasonable design, the liquid from the one step reactor carries gas bubbles, enters the ultrasonic degassing device, the ultrasonic device is used to break the gas bubbles, then the gas is released through the first venturi, and then the gas is sucked into the system through the second venturi, because the generated gas contains ammonia, environmental pollution and material loss are avoided. In this way, after passing through the second feed mixer, the liquid of one step reaction does not carry gas bubbles, and the monomethylamine solution can be accurately matched, and then enters the two step reactor to complete the reaction. In the ultrasonic degassing device, the inlet and outlet pipelines of the liquid are connected with the outside through hoses, which ensures the vibration of the material pipe in the ultrasonic device.

[0017] In addition, the material flow rate of the second Venturi tube is greater than that of the first Venturi tube, generating a pressure difference that can easily suck in the gas removed by ultrasonic waves, reducing material loss. Brief Description of the Drawings

[0018] Figure 1 It is a schematic structural diagram of the present utility model.

[0019] Figure 2 It is a schematic structural diagram of the ultrasonic degassing device in the present utility model. Detailed Embodiment

[0020] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present utility model clearer, the present utility model will be further described in detail below with reference to the drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present utility model and are not used to limit the present utility model.

[0021] As Figure 1 , 2 shown, a reactor for improving the mixing ratio accuracy of methylhydrazine synthesis includes an ammonia water intermediate tank 1, a sodium hypochlorite intermediate tank 2, a monomethylamine solution intermediate tank 3, a methylhydrazine synthesis liquid storage tank 4, a first-stage reactor 5 and a second-stage reactor 6. Inner tubes 7 are provided inside both the first-stage reactor 5 and the second-stage reactor 6, and outer tubes 8 are sleeved outside the inner tubes 7. The discharge ports of the ammonia water intermediate tank 1 and the sodium hypochlorite intermediate tank 2 are respectively connected to a first feed mixer 10 through control valves 16 and a first metering pump 9. The discharge port of the first feed mixer 10 is connected to the inlet of the inner tube of the first-stage reactor 5. A refrigerant inlet 11 and a refrigerant outlet 12 are provided on the outer tube of the first-stage reactor 5. The outlet of the inner tube of the first-stage reactor 5 is connected to the feed end of an ultrasonic degassing device 13. The discharge end of the ultrasonic degassing device 13 is connected to a second feed mixer 14. The discharge port of the monomethylamine solution intermediate tank 3 is connected to the second feed mixer 14 through a second metering pump 15. The discharge port of the second feed mixer 14 is connected to a second Venturi tube 17. The negative pressure port of the second Venturi tube 17 is connected to the ultrasonic degassing device 13. The outlet of the second Venturi tube 17 is connected to the inlet of the inner tube of the second-stage reactor Ⅵ. The outlet of the inner tube of the second-stage reactor 6 is connected to the methylhydrazine synthesis liquid storage tank 4. A heat medium inlet 18 and a heat medium outlet 19 are provided on the outer tube of the second-stage reactor 6.

[0022] The utility model discloses a three raw material storage tanks, namely ammonia water intermediate tank 1, sodium hypochlorite intermediate tank 2, monomethylamine solution intermediate tank 3, methylamine synthesis liquid storage tank 4, the ammonia water intermediate tank 1 and sodium hypochlorite intermediate tank 2 discharge port are connected with first feed mixer 10 through control valve 16, first metering pump 9 respectively, and first feed mixer 10 inputs mixed solution into one step reactor 5 and carries out the reaction, and the material liquid after reaction has gas bubble and enters ultrasonic degassing device 13, and through ultrasonic degassing device 13, the gas bubble is broken and is recovered to second venturi 17, and monomethylamine solution intermediate tank 3 and the material liquid after the reaction of one step reactor 5 are mixed and enter second venturi 17, and second venturi 17 generates negative pressure and inhales the gas released by ultrasonic degassing device 13, and with material liquid enters two step reactor 6, and after two step reactor 6 reaction, enters methylamine synthesis liquid storage tank 4.

[0023] Among them, ultrasonic degassing device 13 includes shell 20, first venturi 21 and ultrasonic vibrator 22, and first venturi 21 and ultrasonic vibrator 22 are installed in shell 20, the inlet of first venturi 21 is connected with the inner pipe outlet of one step reactor 5 through first hose 23, the outlet of first venturi 21 is connected with the inlet pipe of second feed mixer 14 through second hose 24, and the negative pressure port of first venturi 21 is also connected with third hose 25, and the third hose is connected with the negative pressure port of second venturi 17 through connecting pipe 26.Ultrasonic degassing device 13 adopts built-in first venturi 21 and ultrasonic vibrator 22, and the three interfaces of first venturi 21 are connected with the outside through hose, so that under the action of ultrasonic vibrator 22, vibration can be generated, and then the gas bubble of first venturi 21 is broken, the negative pressure port pressure of second venturi 17 is less than that of first venturi 21, the gas generated by first venturi 21 is discharged through the negative pressure outlet of first venturi 21, and is inhaled into second venturi 17, avoiding environmental pollution and material loss.

[0024] The above only is the preferred embodiment of the utility model, and does not limit the utility model, and any modification, equivalent replacement and improvement made within the spirit and principle of the utility model should be included in the utility model range.

Claims

1. A reactor for improving the synthesis ratio accuracy of methyl hydrazine, comprising an ammonia water intermediate tank, a sodium hypochlorite intermediate tank, a monomethylamine solution intermediate tank, a methyl hydrazine synthesis solution storage tank, a one-step reactor, and a two-step reactor, wherein each of the one-step reactor and the two-step reactor is provided with an inner tube, and the outer portion of the inner tube is provided with an outer tube, characterized in that: The discharge outlets of the ammonia water intermediate tank and the sodium hypochlorite intermediate tank are connected with the first feed mixer through control valves and first metering pumps respectively, the discharge outlet of the first feed mixer is connected with the inlet of the inner tube of the one-step reactor, the outer tube of the one-step reactor is provided with a coolant inlet and a coolant outlet, the outlet of the inner tube of the one-step reactor is connected with the feed end of the ultrasonic degassing device, the discharge end of the ultrasonic degassing device is connected with the second feed mixer, the discharge outlet of the monomethylamine solution intermediate tank is connected with the second feed mixer through a second metering pump, the discharge outlet of the second feed mixer is connected with the second Venturi tube, the negative pressure port of the second Venturi tube is connected with the ultrasonic degassing device, the outlet of the second Venturi tube is connected with the inlet of the inner tube of the two-step reactor, the outlet of the inner tube of the two-step reactor is connected with the methylamine synthesis solution storage tank, and the outer tube of the two-step reactor is provided with a heat medium inlet and a heat medium outlet. ​ 2. The reactor for improving the synthesis ratio accuracy of methyl hydride according to claim 1, characterized in that: The ultrasonic degassing device comprises an outer shell, a first Venturi tube and an ultrasonic vibrator, the first Venturi tube and the ultrasonic vibrator are installed in the outer shell, the inlet of the first Venturi tube is connected with the outlet of the inner tube of the one-step reactor through a first hose, the outlet of the first Venturi tube is connected with the inlet pipe of the second feed mixer through a second hose, and the negative pressure port of the first Venturi tube is further connected with a third hose, the third hose is connected with the negative pressure port of the second Venturi tube through a connecting pipe.

3. The reactor for improving the synthesis ratio accuracy of methyl hydride according to claim 1, characterized in that: The negative pressure port of the second Venturi tube has a pressure less than that of the negative pressure port of the first Venturi tube.

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