CN103801248B - The synthesizer of a kind of gas extinguishing agent and synthetic method thereof - Google Patents
The synthesizer of a kind of gas extinguishing agent and synthetic method thereof Download PDFInfo
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- CN103801248B CN103801248B CN201410040281.3A CN201410040281A CN103801248B CN 103801248 B CN103801248 B CN 103801248B CN 201410040281 A CN201410040281 A CN 201410040281A CN 103801248 B CN103801248 B CN 103801248B
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Abstract
The invention discloses synthesizer and the synthetic method thereof of a kind of gas extinguishing agent, it is characterized in that: connecting on a reactor has agitator, trifluoro propene storage tank, bromine storage tank, alkali liquor storage tank and fractionating column, the arm end of fractionating column is passed through receiving flask, the addition sequence of each raw material is controlled, it is achieved one-step synthesis Halon Replacement clean coal power system by multiple switch valves.Addition, cancellation and three operating procedures of fractional distillation can be carried out in the synthesizer of the present invention, whole synthesis flow obtains target product from being fed to, need not move through any intermediate product of transfer, not only avoid loss of material, improve reaction yield, and save the response time, improve reaction efficiency.
Description
Technical field
The invention belongs to extinguishing chemical synthesis field, be specifically related to be applicable to synthetic method and the dress of Halon Replacement clean coal power system
Put.
Background technology
Along with gradually eliminating of halon fire agent, various Halon Replacement extinguishing chemical products continue to bring out.2-bromo-3,3,3-trifluoro propene
(2-BTP) it is considered as most potential a kind of clean efficient Halon Replacement firing-fighting medium.The preparation method of 2-BTP is mainly
Use bromine and trifluoro propene addition, then eliminated by alcohol aqueous slkali, be fractionated into obtaining target product.Due to alcohol aqueous slkali viscosity
Relatively big, there is more alkali bromide slaine to generate during eliminating, need from mother solution, separate precipitation in fractional distillation process,
The most existing synthesizer is to be divided among in different reactors carrying out, by reaction intermediates in building-up process by three steps
Separating and shift, this not only results in the loss of material, reduces synthetic yield, also can increase operating procedure, reduces reaction
Efficiency, additionally adds manufacturing cost and the floor space of synthesizer.
Summary of the invention
The present invention is for solve cannot the problem of one-step synthesis Halon Replacement clean coal power system, it is provided that a kind of integration, letter
Just the synthesizer of efficient gas extinguishing agent and synthetic method thereof.
The present invention solves that technical problem adopts the following technical scheme that
The synthesizer of Halon Replacement clean coal power system of the present invention, its construction features is: arrange a reactor, described
Intensification chuck it is provided with on the sidewall of reactor;The top of described reactor is provided with agitator insert port, gas feed, liquid
Bromine charge door, alkali liquor charge door, gas outlet and thermometer socket;It is provided with sealing-plug close in the bottom of described reactor
The discharging opening of envelope;
Agitator is inserted into inside reactor by agitator insert port, the bottom of agitator, is positioned at below reactor inside center
Position connects stirring paddle;
One end of gas feed conduit is inserted in reactor by described gas feed, and the other end is by the first switch valve and outside
Trifluoro propene storage tank be connected;The sidewall of the bottom of described gas feed conduit is provided with venthole;
One end of bromine conduit is inserted in reactor by described bromine charge door, and the other end passes through second switch valve and is positioned at instead
The bromine storage tank above still is answered to be connected;
One end of alkali liquor conduit is inserted in reactor by described alkali liquor charge door, and the other end passes through the 3rd switch valve and is positioned at instead
The alkali liquor storage tank above still is answered to be connected;
One end of outtake tube is inserted in reactor by gas outlet, and the other end passes through the 4th switch valve and is positioned on reactor
The fractionating column of side is connected;The arm end of fractionating column is passed through receiving flask, and described fractionating column has been inserted into the first thermometer;Described receipts
Collection bottle is placed in beaker;
Second thermometer is inserted in reactor by thermometer socket;
It is outside equipped with radiation source at described intensification chuck.
The synthesizer of the present invention, its construction features lies also in: described bromine conduit and described gas feed conduit are inserted into reaction
The bottom of still, described outtake tube and described alkali liquor conduit are inserted into the top of reactor.
Described reactor is with clear glass as material.
Described venthole is one or more.
At described gas feed and at the contact position of gas feed conduit and described gas feed, at described bromine charge door and liquid
At the contact position of bromine conduit and described bromine charge door, at described alkali liquor charge door and alkali liquor conduit and described alkali liquor charge door
At contact position, at described gas outlet and outtake tube and the contact position of described gas outlet, described second thermometer with
All with ground glass as material at the contact position of described thermometer socket;Described agitator contacts with described agitator insert port
Position is provided with the sealing ring with politef as material.
Utilizing the synthetic method of the Halon Replacement clean coal power system of the synthesizer of the present invention, its feature is as follows
Carry out:
First, open second switch valve, the bromine in bromine storage tank is joined in reactor, close second switch valve, start
Agitator;
Then, open radiation source, then open the first switch valve, by the trifluoro propene in trifluoro propene storage tank with bromine based on chemistry
The amount amount than 1.01~1.15 times is passed in reactor, close the first switch valve after waiting to ventilate;In intensification chuck and burning
It is passed through the cold water that temperature is-5~20 DEG C in Bei, opens the 4th switch valve;
3rd, preparation mass concentration is the aqueous solution of KOH or NaOH of 15~45%, joins in alkali liquor storage tank, opens the
Three switch valves, lead to the aqueous solution of KOH or NaOH in alkali liquor storage tank and the bromine stoichiometrically amount of 1.05~1.20 times
Cross alkali liquor conduit to join in reactor;After treating the aqueous solution interpolation of KOH or NaOH, close the 3rd switch valve;
Finally, reacting kettle jacketing is passed through the hot water that temperature is 30~80 DEG C, receiving flask is collected target product;Collect
Bi Hou, stops being passed through hot water, after device is cooled to room temperature, opens sealing-plug, releases salvage stores by discharge port, described
Target product is Halon Replacement clean coal power system.
Compared with the prior art, beneficial effects of the present invention is embodied in:
1, can carry out addition, cancellation and three operating procedures of fractional distillation in the synthesizer of the present invention, whole synthesis flow is from charging
To obtaining target product, it is not necessary to through shifting any intermediate product, not only avoid loss of material, improve reaction yield,
And save the response time, improve reaction efficiency;
2, the socket above reactor of the present invention is connected with it conduit and interface are all glass frosted or teflon seal company
Connect, do not use any rubber seal, it is to avoid the bromine corrosion to sealing ring;Without poisonous gas leakage in course of reaction, right
Operator and Environmental security;
3, the end of air induction conduit of the present invention arranges multiple venthole, the beneficially abundant reaction between trifluoro propene gas and bromine;
4, the synthesizer of the present invention achieves being turned on and off of synthesis different phase by multiple switch valves;
5, the synthesizer design of the present invention is simple, and compact conformation, easy to manufacture, low cost, floor space is little;
6, each parts regulation and control of the synthesizer of the present invention are convenient, it is easy to installing/dismounting cleans and preserves;
7, the reactor of the present invention is colourless transparent glass manufacture, it is simple to observing response process.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention;
Label in figure: 1 reactor;2 intensification chucks;3 agitator insert ports;4 agitators;5 stirring paddles;6 gases enter
Mouthful;7 air induction conduits;8 ventholes;9 first switch valves;10 trifluoro propene storage tanks;11 bromine charge doors;12 bromines are led
Pipe;13 second switch valves;14 bromine storage tanks;15 alkali liquor charge doors;16 alkali liquor conduits;17 the 3rd switch valves;18 alkali
Liquid storage tank;19 gas outlets;20 outtake tubes;21 the 4th switch valves;22 fractionating columns;23 first thermometeies;24 collect
Bottle;25 beakers;26 discharging openings;27 sealing-plugs;28 thermometer sockets;29 second thermometeies;30 radiation sources.
Specific embodiment
As it is shown in figure 1, the synthesizer of the present embodiment Halon Replacement clean coal power system is to arrange a reactor 1, in reaction
Intensification chuck 2 it is provided with on the sidewall of still 1;Agitator insert port 3, gas feed 6, liquid it is provided with at the top of reactor 1
Bromine charge door 11, alkali liquor charge door 15, gas outlet 19 and thermometer socket 28;It is provided with in the bottom of reactor 1
The discharging opening 26 that sealing-plug 27 seals;
It is internal that agitator 4 is inserted into reactor 1 by agitator insert port 3, the bottom of agitator 4, is positioned at reactor 1
Central lower position, portion connects stirring paddle 5;Agitator insert port 3 is arranged on the center at reactor top, so may be used
To ensure that agitator is positioned at the axis line of reactor, improve stirring efficiency.
One end of gas feed conduit 7 is inserted in reactor 1 by gas feed 6, the other end by the first switch valve 9 with
Outside trifluoro propene storage tank 10 is connected;The sidewall of the bottom of gas feed conduit 7 is provided with venthole 8;
One end of bromine conduit 12 is inserted in reactor 1 by bromine charge door 11, the other end by second switch valve 13 with
It is positioned at the bromine storage tank 14 above reactor to be connected;
One end of alkali liquor conduit 16 is inserted in reactor 1 by alkali liquor charge door 15, the other end by the 3rd switch valve 17 with
It is positioned at the alkali liquor storage tank 18 above reactor to be connected;
One end of outtake tube 20 is inserted in reactor 1 by gas outlet 19, and the other end passes through the 4th switch valve 21 and position
Fractionating column 22 above reactor is connected;The arm end of fractionating column 22 is passed through receiving flask 24, and fractionating column 22 has been inserted into
First thermometer 23;Receiving flask 24 is placed in beaker 25;
Second thermometer 29 is inserted in reactor 1 by thermometer socket 28;It is outside equipped with irradiation source 30 at intensification chuck 2.
In being embodied as, bromine conduit 12 and gas inlet ducts 7 are inserted into the bottom of reactor 1, alkali liquor conduit 16 and going out
Airway 20 is inserted into the top of reactor 1, so can reduce the volatilization of bromine, increases the contact area of reactant, improves
Reaction efficiency.
Reactor 1, with clear glass as material, coordinates transparent intensification chuck 2, it is ensured that radiation source energy Net long wave radiation, the most just
In observing response process.
Venthole 8 is set to multiple, beneficially the abundant reaction between trifluoro propene gas and bromine.
At gas feed 6 and at gas feed conduit 7 and the contact position of gas feed 6, at bromine charge door 11 and bromine is led
At pipe 12 and the contact position of bromine charge door 11, at alkali liquor charge door 15 and the connecing of alkali liquor conduit 16 and alkali liquor charge door 15
Touch at position, gas outlet 19 and at outtake tube 20 and the contact position of gas outlet 19, the second thermometer 29 and temperature
All with ground glass as material at the contact position of degree meter socket 28;Agitator 4 sets at the contact position of agitator insert port 3
It is equipped with the sealing ring with politef as material.
Utilize the synthetic method of the Halon Replacement clean coal power system of the synthesizer of the present embodiment, be to carry out as follows:
First, open second switch valve 13, the bromine in bromine storage tank 14 is joined in reactor 1, close second switch
Valve 13, starts agitator 4;
Then, open radiation source 30, then open the first switch valve 9, the trifluoro propene in trifluoro propene storage tank 10 is pressed with bromine
The amount of stoichiometric proportion 1.01~1.15 times is passed in reactor 1, close the first switch valve 9 after waiting to ventilate;Rising
Temperature chuck 2 and beaker 25 are passed through the cold water that temperature is-5~20 DEG C, open the 4th switch valve 21;
3rd, preparation mass concentration is the aqueous solution of KOH or NaOH of 15~45%, joins in alkali liquor storage tank 18, beats
Drive the 3rd switch valve 17, by the aqueous solution of KOH or NaOH in alkali liquor storage tank 18 and bromine stoichiometrically 1.05~1.20
Amount again is joined in reactor by alkali liquor conduit 16;After treating the aqueous solution interpolation of KOH or NaOH, close the 3rd
Switch valve 17;
Finally, reacting kettle jacketing 2 is passed through the hot water that temperature is 30~80 DEG C, receiving flask 24 is collected target product;Receive
After collection, stop being passed through hot water, after device is cooled to room temperature, open sealing-plug 27, release remnants by discharge port 26
Material, target product is Halon Replacement clean coal power system.
Claims (6)
1. the synthesizer of a gas extinguishing agent, it is characterised in that: a reactor (1) is set, in described reactor (1)
Sidewall on be provided with intensification chuck (2);The top of described reactor (1) is provided with agitator insert port (3), gas enters
Mouth (6), bromine charge door (11), alkali liquor charge door (15), gas outlet (19) and thermometer socket (28);Described
The bottom of reactor (1) is provided with the discharging opening (26) that sealing-plug (27) seals;
It is internal that agitator (4) is inserted into reactor (1) by agitator insert port (3), the bottom of described agitator (4),
It is positioned at the connection of reactor (1) inside center lower position and has stirring paddle (5);
One end of gas feed conduit (7) is inserted in reactor (1) by described gas feed (6), and the other end is by the
One switch valve (9) is connected with outside trifluoro propene storage tank (10);Sidewall in the bottom of described gas feed conduit (7)
On be provided with venthole (8);
One end of bromine conduit (12) is inserted in reactor (1) by described bromine charge door (11), and the other end is by the
Two switch valves (13) are connected with the bromine storage tank (14) being positioned at above reactor;
One end of alkali liquor conduit (16) is inserted in reactor (1) by described alkali liquor charge door (15), and the other end is by the
Three switch valves (17) are connected with the alkali liquor storage tank (18) being positioned at above reactor;
One end of outtake tube (20) is inserted in reactor (1) by gas outlet (19), and the other end is by the 4th switch
Valve (21) is connected with the fractionating column (22) being positioned at above reactor;The arm end of described fractionating column (22) is passed through receiving flask
(24), described fractionating column (22) has been inserted into the first thermometer (23);Described receiving flask (24) is placed in beaker (25)
In;
Second thermometer (29) is inserted in reactor (1) by thermometer socket (28);
It is outside equipped with radiation source (30) described intensification chuck (2).
Synthesizer the most according to claim 1, it is characterised in that: described bromine conduit (12) and described gas feed
Conduit (7) is inserted into the bottom of reactor (1), described outtake tube (20) and described alkali liquor conduit (16) and is inserted into instead
Answer the top of still (1).
Synthesizer the most according to claim 1, it is characterised in that: described reactor (1) is with clear glass as material.
Synthesizer the most according to claim 1, it is characterised in that: described venthole (8) is one or more.
Synthesizer the most according to claim 1, it is characterised in that: described gas feed (6) place and gas feed are led
At the contact position of pipe (7) and described gas feed (6), described bromine charge door (11) place and bromine conduit (12) with
At the contact position of described bromine charge door (11), described alkali liquor charge door (15) place and alkali liquor conduit (16) and described alkali
At the contact position of liquid charge door (15), (19) place of described gas outlet and outtake tube (20) and described gas outlet (19)
Contact position at, at the contact position of described second thermometer (29) and described thermometer socket (28) all with ground glass
For material;Described agitator (4) is provided with politef as material at the contact position of described agitator insert port (3)
The sealing ring of matter.
6. utilize a synthetic method for the gas extinguishing agent of synthesizer, its feature described in claim 1,2,3,4 or 5
It is to carry out as follows:
First, open second switch valve (13), the bromine in bromine storage tank (14) is joined in reactor (1), close
Second switch valve (13), starts agitator (4);
Then, open radiation source (30), then open the first switch valve (9), by the trifluoropropyl in trifluoro propene storage tank (10)
Alkene and the bromine stoichiometrically amount of 1.01~1.15 times is passed in reactor (1), closes the first switch after waiting to ventilate
Valve (9);It is passed through, in intensification chuck (2) and beaker (25), the cold water that temperature is-5~20 DEG C, opens the 4th switch valve (21);
3rd, preparation mass concentration is the aqueous solution of KOH or NaOH of 15~45%, joins in alkali liquor storage tank (18),
Open the 3rd switch valve (17), by the aqueous solution of KOH or NaOH in alkali liquor storage tank (18) with bromine stoichiometrically
Amount than 1.05~1.20 times is joined in reactor by alkali liquor conduit (16);Treat that the aqueous solution of KOH or NaOH has added
Bi Hou, closes the 3rd switch valve (17);
Finally, reacting kettle jacketing (2) is passed through the hot water that temperature is 30~80 DEG C, receiving flask (24) is collected target and produces
Thing;After collection, stop being passed through hot water, after device is cooled to room temperature, open sealing-plug (27), by discharge port (26)
Releasing salvage stores, described target product is gas extinguishing agent.
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CN201410040281.3A CN103801248B (en) | 2014-01-27 | 2014-01-27 | The synthesizer of a kind of gas extinguishing agent and synthetic method thereof |
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CN201410040281.3A CN103801248B (en) | 2014-01-27 | 2014-01-27 | The synthesizer of a kind of gas extinguishing agent and synthetic method thereof |
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CN103801248B true CN103801248B (en) | 2016-08-17 |
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH08247554A (en) * | 1995-03-13 | 1996-09-27 | Matsushita Electric Ind Co Ltd | Electric hot water heater |
CN102247789A (en) * | 2011-06-24 | 2011-11-23 | 威海新元化工有限公司 | Device and method for synthesizing 2-chloro-3,3,3-trifluoropropene |
CN202516542U (en) * | 2012-03-06 | 2012-11-07 | 美药星(南京)制药有限公司 | PH and temperature automatic control system for reaction kettle |
CN102964207A (en) * | 2012-12-22 | 2013-03-13 | 威海新元化工有限公司 | Preparation method of 2-bromo-3,3,3-trifluoropropene |
CN202909714U (en) * | 2012-10-17 | 2013-05-01 | 联化科技股份有限公司 | Device for photocatalysis bromination reaction |
-
2014
- 2014-01-27 CN CN201410040281.3A patent/CN103801248B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH08247554A (en) * | 1995-03-13 | 1996-09-27 | Matsushita Electric Ind Co Ltd | Electric hot water heater |
CN102247789A (en) * | 2011-06-24 | 2011-11-23 | 威海新元化工有限公司 | Device and method for synthesizing 2-chloro-3,3,3-trifluoropropene |
CN202516542U (en) * | 2012-03-06 | 2012-11-07 | 美药星(南京)制药有限公司 | PH and temperature automatic control system for reaction kettle |
CN202909714U (en) * | 2012-10-17 | 2013-05-01 | 联化科技股份有限公司 | Device for photocatalysis bromination reaction |
CN102964207A (en) * | 2012-12-22 | 2013-03-13 | 威海新元化工有限公司 | Preparation method of 2-bromo-3,3,3-trifluoropropene |
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