CN211677659U - Tubular reaction production device for diazotization of phenylhydrazine hydrochloride - Google Patents

Tubular reaction production device for diazotization of phenylhydrazine hydrochloride Download PDF

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CN211677659U
CN211677659U CN201921904767.1U CN201921904767U CN211677659U CN 211677659 U CN211677659 U CN 211677659U CN 201921904767 U CN201921904767 U CN 201921904767U CN 211677659 U CN211677659 U CN 211677659U
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tubular reactor
fixedly connected
tubular
reaction
pipe
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李锦山
王海荣
李正健
施柳柳
吴灵燕
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Qidong Asia Pacific Pharmaceutical Co ltd
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Qidong Asia Pacific Pharmaceutical Co ltd
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Abstract

The utility model discloses a tubular reaction apparatus for producing of diazotization of phenylhydrazine hydrochloride, include that liquid holds jar, connecting plate, wriggling measuring pump, electrical control valve, tubular reaction mechanism and tube mixer, liquid holds jar and is equipped with four groups altogether. The utility model discloses it goes on in a tubular reactor to be different from general diazotization reaction, the utility model discloses set up two tubular reactor casings, anterior segment tubular reactor casing is used for the salification reaction of aniline and hydrochloric acid, back end tubular reactor casing is used for the diazotization reaction of sodium nitrite solution with aniline hydrochloride, because two required process temperature of reaction are different, aniline and hydrochloric acid salification reaction are steerable below 10 ℃ in tubular reactor casing, but sodium nitrite and aniline hydrochloride reaction global control are below 20 ℃, owing to set up two tubular reactor casings respectively, frozen salt water can cool off two reactors along separate routes, the exothermic accumulation of two sections reactions has been avoided, can effectively reduce the equipment energy consumption.

Description

Tubular reaction production device for diazotization of phenylhydrazine hydrochloride
Technical Field
The utility model relates to a chemical equipment technical field specifically is a tubular reaction apparatus for producing of hydrochloric acid phenylhydrazine diazotization.
Background
At present, most of users use the traditional kettle type reactor during the diazotization reaction of phenylhydrazine hydrochloride, but the diazotization reaction of phenylhydrazine hydrochloride needs low temperature operation below 5 ℃ in the traditional kettle type reactor, and in order to maintain lower temperature, the energy consumption is higher, and meanwhile, when the diazotization reaction of phenylhydrazine hydrochloride is operated in the traditional 3000L kettle type reactor, the reaction risk level is 5, the explosion risk is higher, so a tubular reaction production device for diazotization reaction of phenylhydrazine hydrochloride is urgently needed to solve the existing problems.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a tubular reaction apparatus for producing of hydrochloric acid phenylhydrazine diazotization to solve the problem that proposes in the above-mentioned background art.
In order to achieve the above object, the utility model provides a following technical scheme: a diazotization tubular reaction production device of phenylhydrazine hydrochloride, which comprises a liquid holding tank, a connecting plate, a peristaltic metering pump, an electric regulating valve, a tubular reaction mechanism and a pipeline mixer,
the liquid containing tank is provided with four groups, the four groups of liquid containing tanks are fixedly connected through a connecting plate, each liquid containing tank comprises a conveying pipe, an overflow pipe, a tank body, a discharge pipe and a measuring meter, the center of the top end face of the tank body is fixedly connected with the conveying pipe for connection, the overflow pipe is fixedly connected at the position, close to the conveying pipe, of the top end face of the tank body, the measuring meter is fixedly connected at the side end face of the tank body, the discharge pipe is fixedly connected at the center of the bottom end face of the tank body,
the bottom end face through connection of the liquid containing tank is provided with a peristaltic metering pump for measurement, the bottom end face of the peristaltic metering pump is fixedly connected with an electric control valve in a through mode, the bottom end face of the electric control valve is fixedly connected with a pipeline mixer for mixing, the electric control valve is fixedly connected with a tubular reaction mechanism through the pipeline mixer in a through mode, the two tubular reactor shells are arranged, the front tubular reactor shell is used for the salt forming reaction of aniline and hydrochloric acid, the rear tubular reactor shell is used for the diazotization reaction of sodium nitrite solution and aniline hydrochloride, the two tubular reactor shells are different in process temperature, the aniline and hydrochloric acid salt forming reaction in the tubular reactor shell can be controlled below 10 ℃, the sodium nitrite and aniline hydrochloride reaction can be controlled below 20 ℃, and the two tubular reactor shells are arranged respectively, the frozen brine can cool the two reactors in a branch way, thereby avoiding the heat release accumulation of two-stage reaction and effectively reducing the energy consumption of equipment.
Preferably, the tubular reaction mechanism comprises a water pipe, tubular reactor shells, a support plate, a fixed plate, a feed inlet, a water outlet and a flow guide pipe, the inner end surfaces of the tubular reactor shells are fixedly connected with the fixed plate, the tubular reactor shells are provided with two groups, the two groups of tubular reactor shells are fixedly connected with the support plate for supporting through the fixed plate, the upper end surfaces of the tubular reactor shells are fixedly connected with the water pipe, the water outlet is fixedly connected with the bottom end surface of the tubular reactor shell, the inner end surfaces of the tubular reactor shells are provided with the feed inlet in a penetrating way, the flow guide pipes are symmetrically and fixedly connected with the inner end surfaces of the tubular reactor shells close to the feed inlet, the material outlets of the two tubular reactor shells and the frozen brine inlet pipe of the thermometer can be provided with regulating valves for interlocking, and the feeding amount of the frozen brine can be automatically regulated according to the, the temperature of the reaction system is kept stable.
Preferably, the inner end face of the tubular reactor shell is provided with a cooling groove close to the outside of the feed inlet, and the cooling groove is communicated with the water delivery pipe and the flow guide pipe.
Preferably, the cooling groove is an annular groove, and the annular groove is arranged on the outer end face of the feeding hole in a surrounding manner, so that the subsequent cooling capacity can be improved.
Preferably, the water pipe comprises a pipe body for supporting and a fixing plate for connecting.
Preferably, the fixed pipe of side fixedly connected with of line mixer, just line mixer passes through fixed pipe carries out fixed connection with tubular reaction mechanism, advances tubular reactor casing at the material before, has set up line mixer for the material has obtained abundant mixture before advancing the reactor, and reaction liquid concentration is balanced, and the material fully reacts in tubular reactor casing.
Compared with the prior art, the beneficial effects of the utility model are as follows:
1. the utility model discloses it goes on in a tubular reactor to be different from general diazotization reaction, the utility model discloses set up two tubular reactor casings, anterior segment tubular reactor casing is used for the salification reaction of aniline and hydrochloric acid, back end tubular reactor casing is used for the diazotization reaction of sodium nitrite solution with aniline hydrochloride, because two required process temperature of reaction are different, aniline and hydrochloric acid salification reaction are steerable below 10 ℃ in tubular reactor casing, but sodium nitrite and aniline hydrochloride reaction global control are below 20 ℃, owing to set up two tubular reactor casings respectively, frozen salt water can cool off two reactors along separate routes, the exothermic accumulation of two sections reactions has been avoided, can effectively reduce the equipment energy consumption.
2. The utility model discloses the material outlet thermometer of two tubular reactor casings advances the pipe with frozen salt solution and can set up the governing valve chain, can be according to the frozen salt solution feeding volume of temperature automatically regulated of reaction, maintains the temperature stability of reaction system.
3. The utility model discloses before the material advances tubular reactor casing, set up the line mixer for the material has obtained abundant mixture before advancing the reactor, and reaction liquid concentration is balanced, and the material fully reacts in the tubular reactor casing.
4. The device takes hydrochloric acid as a bottom material for reaction, and pumps the initial hydrochloric acid back to the raw material storage tank through circulation in a system in the process of cooling, so that the hydrochloric acid material and the cold energy are fully recovered.
Drawings
FIG. 1 is an exploded view of the main body of the present invention;
FIG. 2 is an assembly view of the main body of the present invention;
FIG. 3 is a schematic view of the structure of the storage tank of the present invention;
FIG. 4 is an exploded view of the tubular reaction mechanism of the present invention;
FIG. 5 is an assembly view of the tubular reaction mechanism of the present invention;
fig. 6 is a front view of the tubular reaction mechanism of the present invention;
fig. 7 is a cross-sectional view along the front view a-a of the tubular reactor mechanism of the present invention.
In the figure: 1-liquid holding tank, 2-connecting plate, 3-peristaltic metering pump, 4-electric regulating valve, 5-tubular reaction mechanism, 6-pipeline mixer, 101-conveying pipe, 102-overflow pipe, 103-tank body, 104-discharging pipe, 105-measuring meter, 501-water conveying pipe, 502-tubular reactor shell, 503-supporting plate, 504-fixing plate, 505-feeding hole, 506-water outlet and 507-guide pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Referring to fig. 1-7, the present invention provides an embodiment: a diazotization tubular reaction production device of phenylhydrazine hydrochloride, which comprises a liquid containing tank 1, a connecting plate 2, a peristaltic metering pump 3, an electric regulating valve 4, a tubular reaction mechanism 5 and a pipeline mixer 6,
the liquid containing tank 1 is provided with four groups, the four groups of liquid containing tanks 1 are fixedly connected through a connecting plate 2, the liquid containing tank 1 comprises a material conveying pipe 101, an overflow pipe 102, a tank body 103, a material discharging pipe 104 and a measuring meter 105, the material conveying pipe 101 for connection is fixedly connected at the center of the top end surface of the tank body 103, the overflow pipe 102 is fixedly connected at the position, close to the material conveying pipe 101, of the top end surface of the tank body 103, the measuring meter 105 is fixedly connected at the side end surface of the tank body 103, the material discharging pipe 104 is fixedly connected at the center of the bottom end surface of the tank body 103,
the bottom end face of the liquid containing tank 1 is connected with a peristaltic metering pump 3 for measurement in a penetrating way, the bottom end face of the peristaltic metering pump 3 is fixedly connected with an electric regulating valve 4 in a penetrating way, the bottom end face of the electric regulating valve 4 is fixedly connected with a pipeline mixer 6 for mixing, the electric regulating valve 4 is fixedly connected with a tubular reaction mechanism 5 in a penetrating way through the pipeline mixer 6, the two tubular reactor shells 502 are arranged, the front tubular reactor shell 502 is used for the salt forming reaction of aniline and hydrochloric acid, the rear tubular reactor shell 502 is used for the diazotization reaction of sodium nitrite solution and aniline hydrochloride, the two tubular reactor shells 502 are different in required process temperature, the salt forming reaction of aniline and hydrochloric acid in the tubular reactor shell 502 can be controlled below 10 ℃, the total temperature of the reaction of sodium nitrite and aniline hydrochloride can be controlled below 20 ℃, and the two tubular reactor shells 502 are respectively arranged, the frozen brine can cool the two reactors in a branch way, thereby avoiding the heat release accumulation of two-stage reaction and effectively reducing the energy consumption of equipment.
The tubular reaction mechanism 5 comprises a water pipe 501, a tubular reactor shell 502, a support plate 503, a fixing plate 504, a feed inlet 505, a water outlet 506 and a flow guide tube 507, the fixing plate 504 is fixedly connected to the inner end surface of the tubular reactor shell 502, two groups of tubular reactor shells 502 are arranged, the support plate 503 for supporting is fixedly connected to the two groups of tubular reactor shells 502 through the fixing plate 504, the water pipe 501 is fixedly connected to the upper end surface of the tubular reactor shell 502, the water outlet 506 is fixedly connected to the bottom end surface of the tubular reactor shell 502, the feed inlet 505 is formed in the inner end surface of the tubular reactor shell 502 in a penetrating manner, the flow guide tube 507 is symmetrically and fixedly connected to the inner end surface of the tubular reactor shell 502 close to the feed inlet 505, regulating valves can be arranged on material outlet thermometers of the two tubular reactor shells 502 and a frozen brine inlet pipe for interlocking, and the feeding amount of the, the temperature of the reaction system is maintained stable.
The inside end face of tubular reactor shell 502 is close to the outside of feed inlet 505 and has seted up the cooling tank, and the cooling tank all carries out through connection with raceway 501 and honeycomb duct 507.
The cooling groove is an annular groove, and the annular groove is arranged on the outer end surface of the feed inlet 505 in a surrounding manner, so that the subsequent cooling capacity can be improved.
The water pipe 501 includes a pipe body for supporting and a fixing plate for connection, so that subsequent connection is facilitated.
The fixed pipe of side fixedly connected with of line mixer 6, and line mixer 6 carries out fixed connection through fixed pipe and tubular reaction mechanism 5, advances tubular reactor casing 502 at the material before, has set up line mixer 6 for the material has obtained abundant mixture before advancing tubular reactor casing 502, and reaction solution concentration is balanced, and the material fully reacts in tubular reactor casing 502.
The working principle is as follows: respectively filling hydrochloric acid, aqueous solution, aniline and sodium nitrite solution into a liquid containing tank 1, opening an external hydrochloric acid loop valve, closing a discharge valve outside the diazo liquid, opening a hydrochloric acid peristaltic metering pump 3 and a valve on a pipe section to allow the hydrochloric acid to flow, opening frozen saline water to reduce the temperature of the hydrochloric acid in the system to be below 10 ℃, opening the external discharge valve outside the diazo liquid, closing the external hydrochloric acid loop valve, opening a water and aniline peristaltic metering pump 3 and an electric regulating valve 4 of the pipe section, opening the electric regulating valve 4 of the pipe section of the sodium nitrite solution peristaltic metering pump 3 relative to the opening time of the water and aniline valves for 10 seconds to avoid the direct reaction of the sodium nitrite and the hydrochloric acid to generate nitrogen oxide gas, obtaining aniline salt solution after the materials are reacted by two tubular reactor shells 502, externally monitoring the temperature of the inlet and the outlet of the tubular reactor shells 502 in the whole process, when the temperature is abnormal, the electric adjusting valve 4 of the frozen brine can be controlled, or the raw material feeding pump and the valves are closed, so that the thermal danger caused by the decomposition of products due to overhigh temperature is avoided, meanwhile, the one-way valve can be arranged on the guide pipe in the tubular reaction mechanism 5, when the required temperature is not too low, a user can open the one-way valve and close the water conveying pipe 501 on the other side, so that the two groups of tubular reactor shells 502 share the cooling liquid, and the energy consumption is reduced.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (6)

1. The tubular reaction production device for diazotization of phenylhydrazine hydrochloride is characterized in that: comprises a liquid containing tank (1), a connecting plate (2), a peristaltic metering pump (3), an electric regulating valve (4), a tubular reaction mechanism (5) and a pipeline mixer (6),
the liquid is contained and is contained tank (1) and is equipped with four groups altogether, and four groups liquid is contained and carry out fixed connection through connecting plate (2) between the tank (1), liquid is contained and is contained tank (1) and include conveying pipeline (101), overflow pipe (102), jar body (103), row material pipe (104) and measurement meter (105), the top face center department fixedly connected with of jar body (103) is used for the conveying pipeline (101) of connecting, and is located the top face of jar body (103) is close to conveying pipeline (101) department fixedly connected with overflow pipe (102), the side end face fixedly connected with measurement meter (105) of jar body (103), and is located the bottom face center department fixedly connected with row material pipe (104) of jar body (103),
liquid holds bottom face through connection who receives jar (1) has been used for measuring wriggling measuring pump (3), and is located the bottom face of wriggling measuring pump (3) link up fixedly connected with electric control valve (4), the bottom face fixedly connected with of electric control valve (4) is used for pipeline mixer (6) of mixing, just electric control valve (4) pass through pipeline mixer (6) link up fixedly connected with tubular reaction mechanism (5).
2. The tubular reaction production device for diazotizing phenylhydrazine hydrochloride according to claim 1, characterized in that: the tubular reaction mechanism (5) comprises a water delivery pipe (501), a tubular reactor shell (502), a supporting plate (503), a fixing plate (504), a feed inlet (505), a water outlet (506) and a draft tube (507), the inner end surface of the tubular reactor shell (502) is fixedly connected with a fixing plate (504), the tubular reactor shell (502) is provided with two groups, and the two groups of tubular reactor shells (502) are fixedly connected with supporting plates (503) for supporting through the fixing plates (504), the upper end surface of the shell (502) of the tubular reactor is fixedly connected with a water delivery pipe (501), and a water outlet (506) is fixedly connected with the bottom end surface of the tubular reactor shell (502), a feed inlet (505) is arranged on the inner end surface of the tubular reactor shell (502) in a penetrating way, and draft tubes (507) are symmetrically and fixedly connected to the inner end surface of the tubular reactor shell (502) close to the feed inlet (505).
3. The tubular reaction production device for diazotizing phenylhydrazine hydrochloride according to claim 2, characterized in that: the inner end face of the tubular reactor shell (502) is close to the outer portion of the feed inlet (505), and is provided with a cooling groove which is communicated with the water delivery pipe (501) and the flow guide pipe (507).
4. The tubular reaction production device for diazotizing phenylhydrazine hydrochloride according to claim 3, characterized in that: the cooling groove is an annular groove, and the annular groove is arranged on the outer end face of the feed port (505) in a surrounding manner.
5. The tubular reaction production device for diazotizing phenylhydrazine hydrochloride according to claim 2, characterized in that: the water conveying pipe (501) comprises a pipe body for supporting and a fixing plate for connecting.
6. The tubular reaction production device for diazotizing phenylhydrazine hydrochloride according to claim 1, characterized in that: the side end of the pipeline mixer (6) is fixedly connected with a fixed pipe, and the pipeline mixer (6) is fixedly connected with the tubular reaction mechanism (5) through the fixed pipe.
CN201921904767.1U 2019-11-07 2019-11-07 Tubular reaction production device for diazotization of phenylhydrazine hydrochloride Active CN211677659U (en)

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CN201921904767.1U CN211677659U (en) 2019-11-07 2019-11-07 Tubular reaction production device for diazotization of phenylhydrazine hydrochloride

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Application Number Priority Date Filing Date Title
CN201921904767.1U CN211677659U (en) 2019-11-07 2019-11-07 Tubular reaction production device for diazotization of phenylhydrazine hydrochloride

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113470757A (en) * 2021-04-16 2021-10-01 甘肃省化工研究院有限责任公司 Thermal risk analysis method of diazotization process

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113470757A (en) * 2021-04-16 2021-10-01 甘肃省化工研究院有限责任公司 Thermal risk analysis method of diazotization process

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