CN114225445A - 2-hydroxyethyl hydrazine purification system - Google Patents

2-hydroxyethyl hydrazine purification system Download PDF

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Publication number
CN114225445A
CN114225445A CN202111476920.7A CN202111476920A CN114225445A CN 114225445 A CN114225445 A CN 114225445A CN 202111476920 A CN202111476920 A CN 202111476920A CN 114225445 A CN114225445 A CN 114225445A
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China
Prior art keywords
hydrazine hydrate
ethylene oxide
pipe
storage tank
weighing
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CN202111476920.7A
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Chinese (zh)
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蒋丽君
张雷
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Shi Run Chemical Technology Shanghai Co ltd
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Shi Run Chemical Technology Shanghai Co ltd
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Priority to CN202111476920.7A priority Critical patent/CN114225445A/en
Publication of CN114225445A publication Critical patent/CN114225445A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C241/00Preparation of compounds containing chains of nitrogen atoms singly-bound to each other, e.g. hydrazines, triazanes
    • C07C241/02Preparation of hydrazines

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a purification system of 2-hydroxyethyl hydrazine, which comprises a weighing hopper, a weighing sensor, a hydrazine hydrate storage tank, an ethylene oxide storage tank and a flow controller, wherein in the process of adding hydrazine hydrate and ethylene oxide, the hydrazine hydrate which is liquid at normal temperature is automatically conveyed into the weighing hopper through a hydrazine hydrate feeding pipe, the hydrazine hydrate is automatically weighed through the weighing sensor arranged at the bottom of the weighing hopper, the hydrazine hydrate is quantitatively filled into a reaction kettle when reaching the preset weight, the ethylene oxide is hermetically conveyed and connected with a feed port of the reaction kettle through the ethylene oxide feeding pipe, so that the ethylene oxide is not exposed in the air, then the conveying amount of the ethylene oxide is monitored through the flow controller, and the flow controller is automatically closed under the control of the controller when reaching the preset amount, so that the mass ratio of the hydrazine hydrate and the ethylene oxide entering the reaction kettle can be accurately and automatically controlled, thereby enabling the purification purity of the 2-hydroxyethylhydrazine to be higher.

Description

2-hydroxyethyl hydrazine purification system
Technical Field
The invention relates to the technical field of chemical purification, in particular to a 2-hydroxyethyl hydrazine purification system.
Background
2-hydroxyethyl hydrazine, also called ethanol hydrazine, is a colorless or light yellow viscous oily liquid, is easily soluble in solvents such as water, ethanol and the like, is a strong reducing substance, is an important intermediate raw material for synthesizing furazolidone, and can also be used as a plant growth regulator, a stabilizer for polyurethane and polyacrylonitrile, an oil well corrosion inhibitor, an epoxy resin curing agent, a cross-linking agent and the like.
At present, the preparation method of the 2-hydroxyethyl hydrazine mainly comprises the following three methods at home and abroad;
1. chlorohydrin process
Adding solid NaOH into hydrazine hydrate solution at 80 ℃, and cooling the reaction temperature to normal temperature after the NaOH is completely dissolved; then 2-chloroethanol is added into the reaction liquid, the temperature is controlled below 35 ℃ due to the exothermic reaction, and after the reaction is finished, the excessive hydroxyethylhydrazine is recovered by rotary evaporation. The reaction has been successfully used in industrial production, wherein about 1330kg of chloroethanol (reduced to 100%), about 800kg of hydrazine hydrate (reduced to 100%) and about 2200kg of liquid alkali (mass fraction of 40%) are consumed on average per 1t of 2-hydroxyethylhydrazine (mass fraction is 100%) produced, and although the yield is high, the liquid alkali is easy to corrode a reaction device, and a large amount of NaCl is generated as a by-product.
2. Ethylene oxide process
The ethylene oxide process is to make hydrazine hydrate and ethylene oxide undergo the addition reaction at a certain temperature, after the reaction is completed, the reduced pressure distillation is used to remove most of water and unreacted hydrazine hydrate so as to obtain the product 2-hydroxyethyl hydrazine, and its yield can be up to 80% -90%. The method allows the concentration range of hydrazine hydrate to be wider (the reaction is not influenced by low-concentration hydrazine hydrate), the product yield and purity are higher, and the process is cleaner.
3. Raschig process
The Raschig method mainly comprises the steps of adding newly prepared NH2CI into an ethanolamine solution under the protection of nitrogen, collecting a mixture after the reaction is completed at a certain temperature, and distilling to obtain a product 2-hydroxyethylhydrazine.
In view of the three methods, the most commonly used method in China at present is to obtain ethylene oxide with higher purity, but the existing method is easy to generate side reactions due to the chemical property of ethylene oxide to generate byproducts such as ethylene glycol, ethanol hydrazine and the like, such as 1, 1-bis (2-hydroxyethyl) hydrazine, 1, 2-bis (2-hydroxyethyl) hydrazine, 2- (2-hydroxyethoxy) ethyl hydrazine and the like, in order to reduce the occurrence of side reactions and improve the reaction selectivity, the used hydrazine hydrate must be excessive, and the reaction temperature should be strictly controlled to prepare the purer 2-hydroxyethyl hydrazine, however, the existing purification system has inaccurate and inconvenient control on the amount of ethylene oxide and hydrazine hydrate, often cannot achieve higher ideal purification purity, and is inconvenient to recover the excessive hydrazine hydrate, the recovery rate is low, and therefore, there is a need for a new purification system that solves the above-mentioned problems.
Disclosure of Invention
The invention aims to provide a 2-hydroxyethylhydrazine purification system to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the utility model provides a 2-hydroxyethyl hydrazine purification system, includes reation kettle, evaporating pot, rectifying column, hydrazine hydrate storage tank and ethylene oxide storage tank, reation kettle, evaporating pot and rectifying column set up side by side from a left side to right side and connect gradually, one side of reation kettle is provided with hydrazine hydrate storage tank and ethylene oxide storage tank, be provided with weighing platform under hydrazine hydrate storage tank and the ethylene oxide storage tank, be provided with weighing hopper on the weighing platform, weighing sensor is installed to weighing hopper's both sides, be provided with the take-up (stock) pan under weighing hopper, take-up (stock) pan bottom is connected with the hydrazine hydrate conveying pipe, the other end and the reation kettle feed inlet of hydrazine hydrate conveying pipe are connected, the bottom of ethylene oxide storage tank is connected with the ethylene oxide conveying pipe, install flow controller on the ethylene oxide conveying pipe.
As a further scheme of the invention: a first conveying pipe is installed at the bottom of the reaction kettle, the other end of the first conveying pipe is connected with the upper portion of the evaporating pot, a second conveying pipe is installed at the bottom of the evaporating pot, and the other end of the second conveying pipe is connected with an air inlet of the rectifying tower.
As a still further scheme of the invention: a first-stage feeding pump is mounted in the middle of the hydrazine hydrate feeding pipe, and a second-stage feeding pump is mounted on the first conveying pipe.
As a still further scheme of the invention: and a recovery pipe is installed at the bottom of the rectifying tower, the other end of the recovery pipe is arranged right above the weighing hopper, and a recovery pump is installed in the middle of the recovery pipe.
As a still further scheme of the invention: the bottom of hydrazine hydrate storage tank is installed the discharging pipe, the discharging pipe sets up towards the take-up (stock) pan direction, install the solenoid valve on the discharging pipe.
As a still further scheme of the invention: the discharge valve and the mixture discharge valve are manual control valves, and a temperature sensor is installed on the reaction kettle.
As a still further scheme of the invention: and a controller is installed on one side of the weighing platform and is respectively and electrically connected with the weighing sensor, the electromagnetic valve, the primary feeding pump, the secondary feeding pump, the recovery pump, the flow controller and the temperature sensor through wires.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention automatically conveys hydrazine hydrate which is liquid at normal temperature into the weighing hopper through the hydrazine hydrate feeding pipe in the adding process of the hydrazine hydrate and the ethylene oxide by arranging the weighing hopper, the weighing sensor arranged at the bottom of the weighing hopper automatically weighs the hydrazine hydrate and quantitatively feeds the hydrazine hydrate into the reaction kettle when the preset weight is reached, and similarly, because of the flammable and explosive characteristics of the ethylene oxide and the reason that the ethylene oxide is gaseous at normal temperature, the ethylene oxide is hermetically conveyed and connected with a feed port of the reaction kettle through the ethylene oxide feeding pipe, so the ethylene oxide can not be exposed in the air, then the conveying quantity of the ethylene oxide is monitored through the flow controller and automatically closed under the control of the controller when the preset quantity is reached, so that the mass ratio of the hydrazine hydrate and the ethylene oxide entering the reaction kettle can be accurately and automatically controlled, thereby enabling the purification purity of the 2-hydroxyethylhydrazine to be higher.
2. According to the invention, by arranging the evaporation tank, the rectifying tower and the hydrazine hydrate recovery tower, the evaporation tank and the rectifying tower can evaporate the surplus hydrazine hydrate from the reaction mixture and can recycle the hydrazine hydrate after rectifying and recovering in the rectifying tower, so that the consumption of the hydrazine hydrate can be saved, and the waste amount of raw materials is reduced.
Drawings
FIG. 1 is a schematic diagram of a 2-hydroxyethylhydrazine purification system.
FIG. 2 is an enlarged view of the structure at A in FIG. 1 of a purification system for 2-hydroxyethylhydrazine.
1. A reaction kettle; 2. an evaporator tank; 3. a rectifying tower; 4. a controller; 5. a hydrazine hydrate storage tank; 6. an ethylene oxide storage tank; 7. a weighing hopper; 8. a hydrazine hydrate feed tube; 9. a take-up pan; 10. a weighing platform; 11. a weighing sensor; 12. a discharge valve; 13. an electromagnetic valve; 14. a discharge pipe; 15. an ethylene oxide feed tube; 16. a primary feed pump; 17. a mixture discharge valve; 18. a first delivery pipe; 19. a secondary feed pump; 20. a second delivery pipe; 21. a flow controller; 22. a recovery pipe; 23. a recovery pump; 24. a temperature sensor.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-2, in an embodiment of the present invention, a system for purifying 2-hydroxyethylhydrazine includes a reaction kettle 1, an evaporation tank 2, a rectification tower 3, hydrazine hydrate storage tank 5 and ethylene oxide storage tank 6, reation kettle 1, evaporating pot 2 and rectifying column 3 set up side by side from left to right and connect gradually, one side of reation kettle 1 is provided with hydrazine hydrate storage tank 5 and ethylene oxide storage tank 6, be provided with weighing platform 10 under hydrazine hydrate storage tank 5 and ethylene oxide storage tank 6, be provided with weighing hopper 7 on the weighing platform 10, weighing sensor 11 is installed to weighing hopper 7's both sides, be provided with take-up (stock) pan 9 under weighing hopper 7, take-up (stock) pan 9 bottom is connected with hydrazine hydrate conveying pipe 8, the other end and the reation kettle 1 feed inlet of hydrazine hydrate conveying pipe 8 are connected, the bottom of ethylene oxide storage tank 6 is connected with ethylene oxide conveying pipe 15, install flow controller 21 on the ethylene oxide conveying pipe 15.
A first conveying pipe 18 is installed at the bottom of the reaction kettle 1, a stirring device is installed on the reaction kettle 1, an electromagnetic heating coil is arranged in the reaction kettle 1 and electrically connected with an external electromagnetic controller, the other end of the first conveying pipe 18 is connected with the upper portion of the evaporating pot 2, a second conveying pipe 20 is installed at the bottom of the evaporating pot 2, and the other end of the second conveying pipe 20 is connected with an air inlet of the rectifying tower 3.
A first-stage feeding pump 16 is arranged in the middle of the hydrazine hydrate feeding pipe 8, and a second-stage feeding pump 19 is arranged on the first conveying pipe 18.
A recovery pipe 22 is installed at the bottom of the rectifying tower 3, the other end of the recovery pipe 22 is arranged right above the weighing hopper 7, a recovery pump 23 is installed in the middle of the recovery pipe 22, the recovery pump 23 can suck the hydrazine hydrate recovered in the recovery pipe 22, and the recovered hydrazine hydrate is conveyed into the weighing hopper 7.
A discharge pipe 14 is arranged at the bottom of the hydrazine hydrate storage tank 5, the discharge pipe 14 is arranged towards the receiving disc 9, and an electromagnetic valve 13 is arranged on the discharge pipe 14.
Discharge valve 12 and mixture discharge valve 17 are manual control valves, install temperature sensor 24 on reation kettle 1, and temperature sensor 24 can monitor the mixed material temperature in reation kettle 1 to real-time to controller 4 feedback, the controller 4 of being convenient for control reaction temperature.
The controller 4 is installed on one side of the weighing platform 10, the model of the controller 4 is S7-200, the controller 4 is of an existing programmable control structure, the controller 4 is electrically connected with the weighing sensor 11, the electromagnetic valve 13, the primary feeding pump 16, the secondary feeding pump 19, the recovery pump 23, the flow controller 21 and the temperature sensor 24 through conducting wires, the model of the weighing sensor 11 is PTS124-133G, the model of the flow controller 21 is FQS-25, and the model of the temperature sensor 24 is Pt 100.
The working principle of the invention is as follows:
when in use, the electromagnetic valve 13 is opened, hydrazine hydrate flows out downwards from a hydrazine hydrate storage tank 5 and is discharged into the weighing hopper 7 through the discharge pipe 14, then the hydrazine hydrate is quantitatively weighed by the weighing sensor 11, after the weighing meets the requirement, the electromagnetic valve 13 is closed, the discharge valve 12 is manually opened at the same time, the hydrazine hydrate falls into the material receiving tray 9 and is sent into the reaction kettle 1 through the hydrazine hydrate feeding pipe 8, ethylene oxide enters the reaction kettle 1 through the ethylene oxide feeding pipe 15 after the flow controller 21 is opened, the flow controller 21 automatically monitors the ethylene oxide feeding amount and is automatically closed after the preset amount is reached, then the mixed material is stirred and heated in a memorial manner through the reaction kettle 1, the mixed material is sent into the evaporation tank 2 under the conveying of the primary feeding pump 16, excessive hydrazine hydrate and water are evaporated in the evaporation tank 2 to produce high-purity 2-hydroxyethyl hydrazine, the excessive hydrazine hydrate and the water enter the rectifying tower 3 in a steam form, the water vapor is discharged from the top under the rectification of the rectifying tower 3, and the hydrazine hydrate enters the weighing hopper 7 again from the recovery pipe 22 at the bottom for recycling.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.

Claims (7)

1. The utility model provides a 2-hydroxyethyl hydrazine purification system, includes reation kettle (1), evaporating pot (2), rectifying column (3), hydrazine hydrate storage tank (5) and ethylene oxide storage tank (6), its characterized in that: the reaction kettle (1), the evaporation tank (2) and the rectifying tower (3) are arranged side by side from left to right and are connected in sequence, a hydrazine hydrate storage tank (5) and an ethylene oxide storage tank (6) are arranged on one side of the reaction kettle (1), weighing platforms (10) are arranged under the hydrazine hydrate storage tank (5) and the ethylene oxide storage tank (6), a weighing hopper (7) is arranged on the weighing platform (10), weighing sensors (11) are arranged on two sides of the weighing hopper (7), a material receiving disc (9) is arranged under the weighing hopper (7), the bottom of the material receiving disc (9) is connected with a hydrazine hydrate feeding pipe (8), the other end of the hydrazine hydrate feeding pipe (8) is connected with a feeding hole of the reaction kettle (1), the bottom of the ethylene oxide storage tank (6) is connected with an ethylene oxide feeding pipe (15), and a flow controller (21) is arranged on the ethylene oxide feeding pipe (15).
2. The purification system of 2-hydroxyethylhydrazine according to claim 1, wherein: first conveyer pipe (18) are installed to reation kettle (1) bottom, the other end of first conveyer pipe (18) is connected with the upper portion of evaporating pot (2), second conveyer pipe (20) are installed to the bottom of evaporating pot (2), the second conveyer pipe (20) other end is connected with the air inlet of rectifying column (3).
3. The purification system of 2-hydroxyethylhydrazine according to claim 1, wherein: a primary feeding pump (16) is installed in the middle of the hydrazine hydrate feeding pipe (8), and a secondary feeding pump (19) is installed on the first conveying pipe (18).
4. The purification system of 2-hydroxyethylhydrazine according to claim 1, wherein: a recovery pipe (22) is installed at the bottom of the rectifying tower (3), the other end of the recovery pipe (22) is arranged right above the weighing hopper (7), and a recovery pump (23) is installed in the middle of the recovery pipe (22).
5. The purification system of 2-hydroxyethylhydrazine according to claim 1, wherein: a discharge pipe (14) is installed at the bottom of the hydrazine hydrate storage tank (5), the discharge pipe (14) is arranged towards the direction of the material receiving disc (9), and an electromagnetic valve (13) is installed on the discharge pipe (14).
6. The purification system of 2-hydroxyethylhydrazine according to claim 1, wherein: the discharge valve (12) and the mixture discharge valve (17) are manually controlled valves, and a temperature sensor (24) is installed on the reaction kettle (1).
7. The purification system of 2-hydroxyethylhydrazine according to claim 1, wherein: the weighing device is characterized in that a controller (4) is installed on one side of the weighing platform (10), and the controller (4) is electrically connected with the weighing sensor (11), the electromagnetic valve (13), the primary feeding pump (16), the secondary feeding pump (19), the recovery pump (23), the flow controller (21) and the temperature sensor (24) through wires.
CN202111476920.7A 2021-12-02 2021-12-02 2-hydroxyethyl hydrazine purification system Pending CN114225445A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111476920.7A CN114225445A (en) 2021-12-02 2021-12-02 2-hydroxyethyl hydrazine purification system

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Application Number Priority Date Filing Date Title
CN202111476920.7A CN114225445A (en) 2021-12-02 2021-12-02 2-hydroxyethyl hydrazine purification system

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CN114225445A true CN114225445A (en) 2022-03-25

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4089752A (en) * 1974-04-24 1978-05-16 Sun Ventures, Inc. Distillation column reactor and process
CN101100433A (en) * 2007-07-25 2008-01-09 辽宁华丰化工(集团)有限公司 Method for producing pure triethanolamine containing micro-water
CN104174250A (en) * 2014-08-15 2014-12-03 国家电网公司 Pre-separation device of mixed gas of sulfur hexafluoride and carbon tetrafluoride and pre-separation method of mixed gas of sulfur hexafluoride and carbon tetrafluoride
CN104876833A (en) * 2015-06-16 2015-09-02 杨东 Microreactor device for producing 2-hydroxyethylhydrazine and preparation process
CN207970810U (en) * 2018-01-11 2018-10-16 宜兴市中正化工有限公司 A kind of ethylene oxide feeding system
CN208266098U (en) * 2018-04-20 2018-12-21 厦门路桥翔通建材科技有限公司 A kind of automation polymer production plant
CN210646378U (en) * 2019-08-13 2020-06-02 铜陵瑞莱科技有限公司 Iron oxide coating device
US20200360988A1 (en) * 2019-05-17 2020-11-19 Molten Metal Equipment Innovations, Llc Smart molten metal pump

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4089752A (en) * 1974-04-24 1978-05-16 Sun Ventures, Inc. Distillation column reactor and process
CN101100433A (en) * 2007-07-25 2008-01-09 辽宁华丰化工(集团)有限公司 Method for producing pure triethanolamine containing micro-water
CN104174250A (en) * 2014-08-15 2014-12-03 国家电网公司 Pre-separation device of mixed gas of sulfur hexafluoride and carbon tetrafluoride and pre-separation method of mixed gas of sulfur hexafluoride and carbon tetrafluoride
CN104876833A (en) * 2015-06-16 2015-09-02 杨东 Microreactor device for producing 2-hydroxyethylhydrazine and preparation process
CN207970810U (en) * 2018-01-11 2018-10-16 宜兴市中正化工有限公司 A kind of ethylene oxide feeding system
CN208266098U (en) * 2018-04-20 2018-12-21 厦门路桥翔通建材科技有限公司 A kind of automation polymer production plant
US20200360988A1 (en) * 2019-05-17 2020-11-19 Molten Metal Equipment Innovations, Llc Smart molten metal pump
CN210646378U (en) * 2019-08-13 2020-06-02 铜陵瑞莱科技有限公司 Iron oxide coating device

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Title
王少华: "连续反应器合成β-羟乙基肼" *

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Application publication date: 20220325