CN216890498U - Thiocarbazine production system - Google Patents
Thiocarbazine production system Download PDFInfo
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- CN216890498U CN216890498U CN202220361915.5U CN202220361915U CN216890498U CN 216890498 U CN216890498 U CN 216890498U CN 202220361915 U CN202220361915 U CN 202220361915U CN 216890498 U CN216890498 U CN 216890498U
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Abstract
The utility model provides a production system of thiocarbohydrazide, belonging to the technical field of organic synthesis. The system comprises a synthesis unit, a hydrogen sulfide absorption unit and a filtrate treatment unit. The synthesis unit comprises a reaction device and a filtering device, the reaction device is provided with a hydrazine hydrate feeding pipe and a tail gas discharging pipe, and the filtering device is provided with a filtrate outlet pipe. The hydrogen sulfide absorption unit comprises a hydrogen sulfide absorption device, and the hydrogen sulfide absorption device is provided with an absorption liquid feeding pipe. The filtrate processing unit comprises a neutralization tank and a hydrazine hydrate distillation tower, wherein the feed end of the neutralization tank is connected with a filtrate outlet pipe, a condensate recovery assembly is arranged on the top of the hydrazine hydrate distillation tower, and the discharge end of the condensate recovery assembly is connected with a hydrazine hydrate feed pipe. A tower kettle of the hydrazine hydrate distillation tower is provided with a wastewater discharge pipe which is connected with an absorption liquid feed pipe. By adopting the thiocarbazide production system, the conversion rate of hydrazine hydrate is improved, sulfur-containing substances in wastewater are recovered, the discharge capacity of the wastewater is reduced, and clean production is realized.
Description
Technical Field
The utility model belongs to the technical field of organic synthesis, and particularly relates to a thio-carbazide production system.
Background
Thiocarbohydrazide (TCH), english name: thiocarbazide, CAS. No.: 2231-57-4, formula: CH (CH)6N4S, is widely used for organic synthesis and is an important production raw material of the high-efficiency broad-spectrum herbicide metribuzin.
An important synthetic route for thiocarbohydrazide is: carbon disulfide and hydrazine hydrate react at a lower temperature to generate dithiocarbazinate (HDTC), then the dithiocarbazinate (HDTC) is heated and decomposed to release hydrogen sulfide, and reaction liquid is cooled to separate and prepare TCH. The production wastewater generated by synthesizing thiocarbazone by adopting the route contains about 3-10% of hydrazine hydrate and a small amount of sodium sulfide, hydrogen sulfide, thiocarbazone and the like. Generally, the part of wastewater is mixed with other wastewater and is discharged after qualified biochemical treatment, on one hand, the conversion rate of hydrazine hydrate is directly reduced, and the yield of thiocarbazone is reduced, on the other hand, sulfur-containing substances in the wastewater enter a biochemical system, so that the difficulty of water treatment is increased, and the waste of sulfur resources is caused.
SUMMERY OF THE UTILITY MODEL
Based on the above, the utility model provides a thiocarbohydrazine production system, which aims to solve the technical problem of low resource utilization efficiency of partial components in wastewater in a thiocarbohydrazine production process in the prior art.
The technical scheme for solving the technical problems is as follows:
a thiocarbohydrazide production system, comprising:
the device comprises a synthesis unit and a gas-liquid separation unit, wherein the synthesis unit comprises a reaction device and a filtering device, the reaction device is provided with a hydrazine hydrate feeding pipe and a tail gas discharging pipe, and the filtering device is provided with a filtrate outlet pipe;
the hydrogen sulfide absorption unit comprises a hydrogen sulfide absorption device, and the hydrogen sulfide absorption device is provided with an absorption liquid feeding pipe; and
the filtrate treatment unit comprises a neutralization tank and a hydrazine hydrate distillation tower connected with the discharge end of the neutralization tank, the feed end of the neutralization tank is connected with the filtrate outlet pipe, the top of the hydrazine hydrate distillation tower is provided with a condensate recovery assembly, and the discharge end of the condensate recovery assembly is connected with the hydrazine hydrate feed pipe; and a tower kettle of the hydrazine hydrate distillation tower is provided with a wastewater discharge pipe, and the wastewater discharge pipe is connected with the absorption liquid feed pipe.
Preferably, the hydrogen sulfide absorption device includes:
a main absorption tank; a first tail gas inlet pipe and a first tail gas outlet pipe are arranged on the main absorption tank, one end of the first tail gas inlet pipe is connected with the tail gas outlet pipe, and the other end of the first tail gas inlet pipe extends into the bottom of the main absorption tank; the first tail gas outlet pipe is communicated with the top of the main absorption tank; a first discharging pump is arranged at the bottom of the main absorption tank; and
at least one secondary canister; a third tail gas inlet pipe and a third tail gas outlet pipe are arranged on the secondary absorption tank, one end of the third tail gas inlet pipe is connected with the first tail gas outlet pipe, and the other end of the third tail gas inlet pipe extends into the bottom of the secondary absorption tank; the third tail gas outlet pipe is communicated with the top of the secondary absorption tank; a third discharge pump is arranged at the bottom of the secondary absorption tank, and the outlet end of the third discharge pump is connected with the main absorption tank; the secondary absorption tank is provided with the absorption liquid feeding pipe.
Preferably, the hydrogen sulfide absorption device further comprises a monitoring tank; a second tail gas inlet pipe and a second tail gas outlet pipe are arranged on the monitoring tank, one end of the second tail gas inlet pipe is connected with the first tail gas outlet pipe, and the other end of the second tail gas inlet pipe extends into the bottom of the monitoring tank; the second tail gas outlet pipe is connected with the third tail gas inlet pipe; the monitoring tank is also provided with a temperature sensor for monitoring the liquid phase temperature in the monitoring tank; the bottom of monitoring jar is provided with the second discharge pump, the exit end of second discharge pump is connected main absorption tank.
Preferably, the filtrate treatment unit further comprises a settling tank, an inlet end of the settling tank is connected with the filtrate outlet pipe, a clear liquid overflow pipe is arranged in the middle of the settling tank, and the neutralization tank is connected with the clear liquid overflow pipe; the bottom of the settling tank is connected with a sulfur card recovery pump, and the outlet end of the sulfur card recovery pump is connected with the inlet end of the filtering device.
Preferably, the hydrogen sulfide absorption unit still includes exhaust emission device, exhaust emission device includes negative pressure pump, active carbon adsorption subassembly and exhaust chimney, the entry linkage of negative pressure pump the third tail gas outlet duct, exit linkage the active carbon adsorption subassembly, the exit end of active carbon adsorption subassembly is connected the exhaust chimney.
Preferably, the hydrogen sulfide absorption unit further comprises a sodium hydrosulfide storage tank, and a feed end of the sodium hydrosulfide storage tank is connected with an outlet end of the first discharge pump; a circulating discharge pump is arranged at the bottom of the sodium hydrosulfide storage tank, a pre-absorption tower is arranged at the top of the sodium hydrosulfide storage tank, and the bottom of the pre-absorption tower is communicated with the sodium hydrosulfide storage tank; the pre-absorption tower is provided with a reaction kettle tail gas inlet pipe and at least one spray pipe, the reaction kettle tail gas inlet pipe is connected with the tail gas discharging pipe, and the spray pipe is connected with the outlet end of the circulating discharging pump.
Preferably, the condensate recovery assembly comprises at least one stage of condenser, a condensate tank and a reflux pump which are connected in sequence, and the discharge end of the reflux pump is respectively connected with the upper part of the distillation tower and the hydrazine hydrate feeding pipe.
Preferably, the condensate recovery assembly further comprises a condensate cooler, wherein the feed end of the condensate cooler is connected with the outlet end of the reflux pump, and the discharge end of the condensate cooler is connected with the hydrazine hydrate feed pipe.
Compared with the prior art, the utility model has at least the following advantages:
the method comprises the steps of setting a synthesis unit, a hydrogen sulfide absorption unit and a filtrate treatment unit, wherein the synthesis unit is used for producing crude thiocarbohydrazide liquid by taking hydrazine hydrate and carbon disulfide as raw materials, filtering and separating a thiocarbohydrazide product from the crude thiocarbohydrazide liquid, and obtaining a filtrate. And (3) treating the filtrate by the filtrate treatment unit, neutralizing hydrogen sulfide and part of acidic sulfur-containing substances contained in the filtrate by excessive alkali liquor, and then feeding the neutralized solution into a hydrazine hydrate distillation tower for distillation. Recovering 20-40% hydrazine hydrate solution from the top of a hydrazine hydrate distillation tower, and the residual Na-containing solution in the bottom of the hydrazine hydrate distillation tower2S and part of the impurity is used as H2S absorbent, absorbing H produced by the synthesis unit2And S, finally forming the NaHS solution.
The thiocarbohydrazide production system neutralizes wastewater generated in the thiocarbohydrazide synthesis process by alkali liquor, and then recovers hydrazine hydrate in the thiocarbohydrazide wastewater by distillation of a hydrazine hydrate distillation tower, thereby improving the conversion rate of the hydrazine hydrate. The hydrazine hydrate distillation tower bottom liquid is used as H2The S absorbent not only recovers sulfur-containing substances in the wastewater, but also reduces the discharge capacity of the wastewater, realizes the near zero discharge of the wastewater, and realizes the clean production of the thiocarbohydrazide.
Drawings
FIG. 1 is a schematic view of an embodiment of a process flow of a thiocarbohydrazine production system.
Fig. 2 is a schematic flow diagram of an apparatus of a synthesis unit in an embodiment.
Fig. 3 is a schematic flow chart of the apparatus of the hydrogen sulfide absorption unit according to an embodiment.
Fig. 4 is a schematic view showing the flow of the hydrogen sulfide absorption unit according to still another embodiment.
Fig. 5 is a schematic apparatus flow diagram of a filtrate processing unit according to an embodiment.
In the figure: the device comprises a thiocarbohydrazide production system 10, a synthesis unit 100, a reaction device 110, a hydrazine hydrate feed pipe 111, a tail gas discharge pipe 112, a filter device 120, a filtrate outlet pipe 121, a hydrogen sulfide absorption unit 200, a hydrogen sulfide absorption device 210, an absorption liquid feed pipe 201, a main absorption tank 211, a first tail gas inlet pipe 2111, a first tail gas outlet pipe 2112, a first discharge pump 2113, a tail gas distributor 2114, a secondary absorption tank 212, a third tail gas inlet pipe 2121, a third tail gas outlet pipe 2122, a third discharge pump 2123, a monitoring tank 213, a second tail gas inlet pipe 2131, a second tail gas outlet pipe 2132, a temperature sensor 2133, a second discharge pump 2134, a tail gas discharge device 220, a negative pressure pump 221, an activated carbon adsorption component 222, an exhaust chimney 223, a sodium hydrosulfide storage tank 230, a circulating discharge pump 231, a pre-absorption tower 232, a reaction kettle tail gas inlet pipe 2321, a spray pipe 2322, an atomization spray nozzle 2323, a filtrate treatment unit 300, The system comprises a settling tank 310, a clear liquid overflow pipe 311, a sulfur card recovery pump 312, an overflow partition 313, a neutralization tank 320, a hydrazine hydrate distillation tower 330, a waste water discharge pipe 331, a condensate recovery assembly 340, a condenser 341, a condensate tank 342, a reflux pump 343, a condensate cooler 344, a p-aminobenzamide production device 400 and a concentration device 500.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The technical solutions of the present invention will be further described below with reference to the accompanying drawings of the embodiments of the present invention, and the present invention is not limited to the following specific embodiments.
It should be understood that the same or similar reference numerals in the drawings of the embodiments correspond to the same or similar parts. In the description of the present invention, it should be understood that if there are terms such as "upper", "lower", "front", "rear", "left", "right", "top", "bottom", etc., indicating orientations or positional relationships based on the orientations or positional relationships shown in the drawings, it is only for convenience of description and simplicity of description, but does not indicate or imply that the equipment or elements referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationships in the drawings are only used for illustrative purposes and are not to be construed as limiting the patent, and the specific meanings of the terms will be understood by those skilled in the art according to specific situations.
In one embodiment, referring to fig. 1 to 5, a thiocarbohydrazine production system 10 for clean production of thiocarbohydrazine includes a synthesis unit 100, a hydrogen sulfide absorption unit 200, and a filtrate treatment unit 300. The synthesis unit 100 comprises a reaction device 110 and a filtering device 120, wherein the reaction device 110 is provided with a hydrazine hydrate feeding pipe 111 and a tail gas discharging pipe 112, and the filtering device 120 is provided with a filtrate outlet pipe 121. The hydrogen sulfide absorption unit 200 includes a hydrogen sulfide absorption device 210, and the hydrogen sulfide absorption device 210 is provided with an absorption liquid feed pipe 201. The filtrate processing unit 300 comprises a neutralization tank 320 and a hydrazine hydrate distillation tower 330 connected with the discharge end of the neutralization tank 320, the feed end of the neutralization tank 320 is connected with the filtrate outlet pipe 121, a condensate recovery assembly 340 is arranged at the top of the hydrazine hydrate distillation tower 330, and the discharge end of the condensate recovery assembly 340 is connected with the hydrazine hydrate feed pipe 111. A waste water discharge pipe 331 is arranged at the bottom of the hydrazine hydrate distillation tower 330, and the waste water discharge pipe 331 is connected with the absorption liquid feed pipe 201.
In the reaction apparatus 110, hydrazine hydrate and CS2Firstly reacting at a lower temperature to generate dithiocarbazic acid (HDTC), then heating up, decomposing the HDTC to generate thiocarbohydrazide, and releasing hydrogen sulfide. And cooling and filtering the reaction solution, washing and drying solid substances to obtain the product thiocarbohydrazide.
Mother liquor obtained by filtering the reaction solution and washing solution generated in the washing process are sent into the neutralization tank 320, liquid alkali is added, and H in the filtrate is neutralized2S and other acidic substances to obtain Na-containing2Dilute alkali solution of S. Containing Na2The dilute alkali liquor of S is sent into the hydrazine hydrate distillation tower 330, 20-40% of hydrazine hydrate solution is recovered from the tower top, and the tower bottom liquid is used as H2The S-absorbed solution is sent to the hydrogen sulfide absorption device 210 to absorb H generated in the reaction device 1102And S, finally forming the NaHS solution.
The NaHS solution can be separated to obtain industrial NaHS salt, preferably, the NaHS solution is used as a raw material for producing the p-aminobenzamide, the p-nitrobenzamide is used as a raw material for producing the p-aminobenzamide, and low discharge and zero discharge of sulfur-containing wastewater are realized.
The thiocarbohydrazide production system 10 firstly neutralizes wastewater generated in the thiocarbohydrazide synthesis process through alkali liquor, and then recovers hydrazine hydrate in the thiocarbohydrazide wastewater through distillation in the hydrazine hydrate distillation tower 330, thereby improving the conversion rate of the hydrazine hydrate. The bottom liquid of the hydrazine hydrate distillation tower 330 is used as H2The S absorbent not only recovers sulfur-containing substances in the wastewater, but also reduces the discharge capacity of the wastewater, realizes the near zero discharge of the wastewater, and realizes the clean production of the thiocarbohydrazide.
In one preferred embodiment, please refer to fig. 3, the hydrogen sulfide absorption apparatus 210 includes a main absorption tank 211 and at least one secondary absorption tank 212, a first tail gas inlet pipe 2111 and a first tail gas outlet pipe 2112 are disposed on the main absorption tank 211, one end of the first tail gas inlet pipe 2111 is connected to the tail gas outlet pipe 112, and the other end extends into the bottom of the main absorption tank 211. The first tail gas outlet pipe 2112 is communicated with the top of the main absorption tank 211, and a first discharge pump 2113 is arranged at the bottom of the main absorption tank 211. A third tail gas inlet pipe 2121 and a third tail gas outlet pipe 2122 are arranged on the secondary absorption tank 212, one end of the third tail gas inlet pipe 2121 is connected with the first tail gas outlet pipe 2112, and the other end of the third tail gas inlet pipe extends into the bottom of the secondary absorption tank 212. The third tail gas outlet pipe 2122 is communicated with the top of the secondary absorption tank 212. The bottom of the secondary absorption tank 212 is provided with a third discharge pump 2123, and the outlet end of the third discharge pump 2123 is connected with the primary absorption tank 211. The absorption liquid feeding pipe 201 is arranged on the secondary absorption tank 212.
Further, to facilitate monitoring H within the primary absorber tank 2112S, the hydrogen sulfide absorption device 210 further includes a monitoring tank 213. The monitoring tank 213 is provided with a second tail gas inlet pipe 2131 and a second tail gas outlet pipe 2132, one end of the second tail gas inlet pipe 2131 is connected with the first tail gas outlet pipe 2112, and the other end extends into the bottom of the monitoring tank 213. The second tail gas outlet pipe 2132 is connected with the third tail gas inlet pipe 2121. The monitoring tank 213 is also provided with a device for monitoring the liquid phase temperature in the monitoring tank 213A temperature sensor 2133, wherein a second discharging pump 2134 is arranged at the bottom of the monitoring tank 213, and the outlet end of the second discharging pump 2134 is connected with the main absorption tank 211.
In the above embodiment, a main absorption tank 211, a monitoring tank 213, and at least one secondary absorption tank 212 are provided, tail gas of the thiocarbohydrazide reaction kettle containing high-concentration hydrogen sulfide is firstly introduced into the main absorption tank 211 through the first tail gas inlet pipe 2111, most of the hydrogen sulfide contacts and reacts with the dilute alkali solution in the main absorption tank 211 or the dilute alkali solution containing sodium sulfide to generate sodium hydrosulfide (NaHS), and the generated sodium hydrosulfide is recycled. A small part of hydrogen sulfide overflows through the first tail gas inlet pipe 2112 at the top of the main absorption tank 211, and sequentially passes through the monitoring tank 213 and the secondary absorption tank 212 to react with dilute alkali liquor in a contact manner to generate sodium sulfide (Na)2S). Tail gas emissions through the secondary absorber 212.
As the dilute alkali liquor in the main absorption tank 211 is gradually absorbed and saturated, a large amount of hydrogen sulfide enters the monitoring tank 213 to react with the dilute alkali liquor to release heat. When the temperature sensor 210 detects that the temperature of the liquid phase in the monitoring tank 213 rises, the solution saturated in absorption in the main absorption tank 211 is discharged through the first discharge pump 2113 for further treatment and resource utilization of sodium hydrosulfide therein. Then the dilute alkali liquor in the monitoring tank 213 is sent into the main absorption tank 211, the dilute alkali liquor in the secondary absorption tank 212 is sent into the monitoring tank 213, and fresh alkali liquor and tower bottom liquor from the tower bottom of the hydrazine hydrate distillation tower 330 are supplemented into the secondary absorption tank 212.
On one hand, dilute alkali liquor and tower bottom liquid from the tower bottom of the hydrazine hydrate distillation tower 330 are adopted to absorb hydrogen sulfide gas generated in the synthetic reaction process of thiocarbohydrazide to prepare sodium hydrosulfide solution, so that the recycling of sulfur is realized, the utilization rate of liquid alkali is improved, and the discharge amount of waste water is reduced. On the other hand, under the guarantee of at least one-stage secondary absorption tank 212, hydrogen sulfide can be contacted with nearly fresh alkali liquor all the time, so that the hydrogen sulfide is absorbed, the comprehensive removal efficiency of the hydrogen sulfide exceeds 99%, and the high removal efficiency can be maintained for a long time.
It is worth mentioning that the secondary absorption tank 212 is provided with at least one, a plurality of secondary absorption tanks 212 are connected in series, and the third discharge pump 2123 of the subsequent stage can pump the dilute alkali liquor in the corresponding secondary absorption tank 212 to the secondary absorption tank 212 of the previous stage. Preferably, the secondary absorption tank 212 is provided to secure the removal efficiency of hydrogen sulfide in the offgas.
In some embodiments, in order to reduce the influence of the discharged tail gas on the environment, the hydrogen sulfide absorption unit 200 further includes a tail gas discharge device 220, the tail gas discharge device 220 includes a negative pressure pump 221, an activated carbon adsorption component 222 and an exhaust chimney 223, an inlet of the negative pressure pump 221 is connected to the third tail gas outlet pipe 2122, an outlet of the negative pressure pump is connected to the activated carbon adsorption component 222, and an outlet of the activated carbon adsorption component 222 is connected to the exhaust chimney 223. Preferably, the height of the exhaust stack 223 is not less than 25 m. The tail gas of the thiocarbazide reaction kettle is extracted by the negative pressure pump 221 after hydrogen sulfide is removed by the main absorption tank 211, the monitoring tank 213 and the secondary absorption tank 212, and is sent to the activated carbon adsorption component 222, so that the content of VOCs in the tail gas is further reduced, and the tail gas is discharged through the exhaust chimney 223.
In some embodiments, the hydrogen sulfide absorption unit 200 further comprises a sodium hydrosulfide storage tank 230, wherein a feed end of the sodium hydrosulfide storage tank 230 is connected to an outlet end of the first discharge pump 2113. The solution saturated in absorption in the main absorption tank 211 is discharged to the sodium hydrosulfide storage tank 230 through the first discharge pump 2113 for further treatment.
In some preferred embodiments, the discharge end of the sodium hydrosulfide storage tank 230 is connected with a p-aminobenzamide production device 400. The sodium hydrosulfide solution produced by absorbing the tail gas of the thiocarbohydrazide reaction kettle is directly used as a reducing agent to reduce the paranitrobenzamide to prepare the paraaminobenzamide, thereby reducing the separation process of the sodium hydrosulfide and reducing the discharge amount of wastewater.
Further, the discharge end of the sodium hydrosulfide storage tank 230 is also connected with a concentration device 500 to perform evaporation concentration on the obtained sodium hydrosulfide solution, so as to adjust the concentration of the sodium hydrosulfide solution on the one hand, and recover part of condensed water on the other hand, thereby reducing the discharge amount of wastewater.
In some preferred embodiments, in order to improve the absorption efficiency of hydrogen sulfide in the primary absorption tank 211, please refer to fig. 4 together, a tail gas distributor 2114 is disposed in the primary absorption tank 211, and the feed end of the tail gas distributor 2114 is connected to the first tail gas inlet pipe 2111. The tail gas from the thiocarbohydrazide reaction device 110 enters the tail gas distributor 2114 through the first tail gas inlet pipe 2111, is diffused from the air holes and contacts with the dilute alkali solution, so that the contact area of the tail gas and the dilute alkali solution is enlarged, and the absorption efficiency of the dilute alkali solution on hydrogen sulfide is improved.
In some preferred embodiments, in order to further reduce the content of sodium sulfide in the obtained sodium hydrosulfide solution and improve the purity of the prepared sodium hydrosulfide solution, please refer to fig. 3 together, a circulating discharge pump 231 is disposed at the bottom of the sodium hydrosulfide storage tank 230, a pre-absorption tower 232 is disposed at the top of the sodium hydrosulfide storage tank, and the bottom of the pre-absorption tower 232 is communicated with the sodium hydrosulfide storage tank 230. The pre-absorption tower 232 is provided with a reaction kettle tail gas inlet pipe 2321 and at least one spray pipe 2322, and the spray pipe 2322 is connected with the outlet end of the circulating discharge pump 231.
In the above embodiment, the tail gas of the thiocarbohydrazide reaction kettle containing high concentration hydrogen sulfide is firstly sent to the bottom of the pre-absorption tower 232, the sodium hydrosulfide solution which is stored in the sodium hydrosulfide storage tank 230 and is saturated in absorption is pumped by the circulating discharge pump 231, and is sprayed from the top of the pre-absorption tower 232 through the spray pipe 2322 to contact with the tail gas of the thiocarbohydrazide reaction kettle containing high concentration hydrogen sulfide, so that a small amount of sodium sulfide contained in the sodium hydrosulfide solution is further converted into sodium hydrosulfide, and the purity of the prepared sodium hydrosulfide solution is improved.
Further, an atomizing spray head 2323 connected with the spray pipe 2322 is arranged in the pre-absorption tower 232. For example, three atomizing nozzles 2323 are arranged in the pre-absorption tower 232 from top to bottom. The sodium hydrosulfide solution containing a small amount of sodium sulfide passes through the atomizing spray head 2323 to form a fog shape, and is in countercurrent contact with the tail gas containing hydrogen sulfide, so that the conversion efficiency of the sodium sulfide is improved.
In one preferred embodiment, referring to fig. 5 together, the filtrate processing unit 300 further comprises a settling tank 310, wherein the inlet end of the settling tank 310 is connected with the filtrate outlet pipe 121, a clear liquid overflow pipe 311 is arranged in the middle of the settling tank 310, and the neutralization tank 320 is connected with the clear liquid overflow pipe 311. The bottom of the settling tank 310 is connected with a sulfur card recovery pump 312, and the outlet end of the sulfur card recovery pump 312 is connected with the inlet end of the filtering device 120.
Mother liquor obtained by filtering reaction liquid and washing liquid generated in the washing process are sent into the settling tank 310, and a small amount of solid contained in the filtrate is settled at the bottom of the settling tank 310. When the filtering device 120 is operating, the bottom liquid settled in the settling tank 310 for a certain time is pumped to the front end of the filtering device 120, and is mixed with the reaction liquid from the synthesizing device 110 and then filtered, so that part of the thiocarbohydrazide product is recovered, and the yield of the thiocarbohydrazide product is improved. In order to improve the settling effect of the wastewater generated in the thiocarbohydrazide production in the settling tank 310, an overflow baffle 313 is arranged in the settling tank 310.
In some embodiments, the condensate recovering assembly 340 includes at least one stage of condenser 341, a condensate tank 342 and a reflux pump 343, which are connected in sequence, and a discharge end of the reflux pump 343 is connected to an upper portion of the hydrazine hydrate distillation column 330 and a feed end of the reaction device 110, respectively.
Further, the condensate recovering assembly 340 further comprises a condensate cooler 344, wherein a feed end of the condensate cooler 344 is connected to an outlet end of the reflux pump 343, and a discharge end of the condensate cooler 344 is connected to the hydrazine hydrate feed pipe 111.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A thiocarbohydrazide production system, comprising:
the device comprises a synthesis unit and a gas-liquid separation unit, wherein the synthesis unit comprises a reaction device and a filtering device, the reaction device is provided with a hydrazine hydrate feeding pipe and a tail gas discharging pipe, and the filtering device is provided with a filtrate outlet pipe;
the hydrogen sulfide absorption unit comprises a hydrogen sulfide absorption device, and the hydrogen sulfide absorption device is provided with an absorption liquid feeding pipe; and
the filtrate treatment unit comprises a neutralization tank and a hydrazine hydrate distillation tower connected with the discharge end of the neutralization tank, the feed end of the neutralization tank is connected with the filtrate outlet pipe, the tower top of the hydrazine hydrate distillation tower is provided with a condensate recovery assembly, and the discharge end of the condensate recovery assembly is connected with the hydrazine hydrate feed pipe; and a tower kettle of the hydrazine hydrate distillation tower is provided with a wastewater discharge pipe, and the wastewater discharge pipe is connected with the absorption liquid feed pipe.
2. The thiocarbohydrazine-producing system according to claim 1, wherein the hydrogen sulfide-absorbing means comprises:
a main absorption tank; a first tail gas inlet pipe and a first tail gas outlet pipe are arranged on the main absorption tank, one end of the first tail gas inlet pipe is connected with the tail gas outlet pipe, and the other end of the first tail gas inlet pipe extends into the bottom of the main absorption tank; the first tail gas outlet pipe is communicated with the top of the main absorption tank; a first discharging pump is arranged at the bottom of the main absorption tank; and
at least one secondary canister; a third tail gas inlet pipe and a third tail gas outlet pipe are arranged on the secondary absorption tank, one end of the third tail gas inlet pipe is connected with the first tail gas outlet pipe, and the other end of the third tail gas inlet pipe extends into the bottom of the secondary absorption tank; the third tail gas outlet pipe is communicated with the top of the secondary absorption tank; a third discharge pump is arranged at the bottom of the secondary absorption tank, and the outlet end of the third discharge pump is connected with the main absorption tank; the secondary absorption tank is provided with the absorption liquid feeding pipe.
3. The thiocarbohydrazine-producing system of claim 2, wherein the hydrogen sulfide-absorbing device further comprises a monitoring tank; a second tail gas inlet pipe and a second tail gas outlet pipe are arranged on the monitoring tank, one end of the second tail gas inlet pipe is connected with the first tail gas outlet pipe, and the other end of the second tail gas inlet pipe extends into the bottom of the monitoring tank; the second tail gas outlet pipe is connected with the third tail gas inlet pipe; the monitoring tank is also provided with a temperature sensor for monitoring the liquid phase temperature in the monitoring tank; the bottom of monitoring jar is provided with the second discharge pump, the exit end of second discharge pump is connected main absorption tank.
4. The thiocarbazosin production system as claimed in any one of claims 1 to 3, wherein the filtrate treatment unit further comprises a settling tank, the inlet end of the settling tank is connected with the filtrate outlet pipe, and the middle part of the settling tank is provided with a clear liquid overflow pipe, and the neutralization tank is connected with the clear liquid overflow pipe; the bottom of the settling tank is connected with a sulfur card recovery pump, and the outlet end of the sulfur card recovery pump is connected with the inlet end of the filtering device.
5. The thiocarbohydrazine production system as claimed in claim 3, wherein the hydrogen sulfide absorption unit further comprises a tail gas discharge device, the tail gas discharge device comprises a negative pressure pump, an activated carbon adsorption component and an exhaust chimney, an inlet of the negative pressure pump is connected with the third tail gas outlet pipe, an outlet of the negative pressure pump is connected with the activated carbon adsorption component, and an outlet of the activated carbon adsorption component is connected with the exhaust chimney.
6. The thiocarbohydrazine-producing system of claim 5, wherein the hydrogen sulfide absorption unit further comprises a sodium hydrosulfide tank, a feed end of the sodium hydrosulfide tank being connected to an outlet end of the first discharge pump; a circulating discharge pump is arranged at the bottom of the sodium hydrosulfide storage tank, a pre-absorption tower is arranged at the top of the sodium hydrosulfide storage tank, and the bottom of the pre-absorption tower is communicated with the sodium hydrosulfide storage tank; the pre-absorption tower is provided with a reaction kettle tail gas inlet pipe and at least one spray pipe, the reaction kettle tail gas inlet pipe is connected with the tail gas discharging pipe, and the spray pipe is connected with the outlet end of the circulating discharging pump.
7. The thiocarbohydrazine production system of claim 4, wherein the condensate recovery assembly comprises at least one stage of condenser, a condensate tank and a reflux pump connected in sequence, and the discharge end of the reflux pump is respectively connected with the upper part of the distillation tower and the hydrazine hydrate feeding pipe.
8. The thiocarbohydrazine production system of claim 7, wherein the condensate recovery assembly further comprises a condensate cooler, a feed end of the condensate cooler is connected to an outlet end of the reflux pump, and a discharge end of the condensate cooler is connected to the hydrazine hydrate feed pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202220361915.5U CN216890498U (en) | 2022-02-22 | 2022-02-22 | Thiocarbazine production system |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220361915.5U CN216890498U (en) | 2022-02-22 | 2022-02-22 | Thiocarbazine production system |
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| CN216890498U true CN216890498U (en) | 2022-07-05 |
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| CN202220361915.5U Active CN216890498U (en) | 2022-02-22 | 2022-02-22 | Thiocarbazine production system |
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