CN103801248A - Synthesis device and method of gaseous extinguishing agent - Google Patents
Synthesis device and method of gaseous extinguishing agent Download PDFInfo
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- CN103801248A CN103801248A CN201410040281.3A CN201410040281A CN103801248A CN 103801248 A CN103801248 A CN 103801248A CN 201410040281 A CN201410040281 A CN 201410040281A CN 103801248 A CN103801248 A CN 103801248A
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Abstract
The invention discloses a synthesis device and method of a gaseous extinguishing agent. The synthesis device is characterized in that a reaction still is connected with an agitator, a trifluoropropene storage tank, a liquid bromine storage tank, an alkali liquor storage tank and a fractional distillation tube, the tail end of a branch tube of the fractional distillation tube goes into a collecting bottle, the adding order of raw materials can be controlled through a plurality of switching valves, and halon is synthesized by one step to substitute for a clean gaseous extinguishing agent. Three operation steps of addition, elimination and fractionation can be performed in the synthesis device, and the whole synthesis flow is free from transferring of any intermediate product from the step of feeding materials to the step of obtaining the target product, so that the material loss is avoided, the reaction yield is improved, the reaction time is saved, and the reaction efficiency is improved.
Description
Technical field
The invention belongs to the synthetic field of extinguishing chemical, be specifically related to be applicable to breathe out synthetic method and the device of the alternative clean gas extinguishing chemical of dragon.
Background technology
Along with eliminating gradually of halon fire agent, various Kazakhstan dragon substitutes extinguishing chemical product and continues to bring out.2-is bromo-3,3, and 3-trifluoro propene (2-BTP) is considered to most potential and a kind ofly cleanly breathes out efficiently dragon and substitute firing-fighting medium.The preparation method of 2-BTP adopts bromine and trifluoro propene addition, then by the cancellation of alcohol aqueous slkali, obtains target product through fractionation.Because alcohol aqueous slkali viscosity is larger, in cancellation process, there is more alkali bromide slaine to generate, in fractional distillation process, need precipitation to separate from mother liquor, therefore existing synthesizer is that three steps are separately carried out in different reactors, in building-up process, reaction intermediates is separated and is shifted, and this not only can cause the loss of material, reduce synthetic yield, also can increase operating procedure, reduce reaction efficiency, increase in addition manufacturing cost and the floor space of synthesizer.
Summary of the invention
The present invention is the problem of cannot one-step synthesis breathing out dragon and substitute clean gas extinguishing chemical for solving, and a kind of synthesizer and synthetic method thereof of gas extinguishing agent of integrated, simple and effective is provided.
The present invention is that technical solution problem adopts following technical scheme:
The present invention breathes out the synthesizer of the alternative clean gas extinguishing chemical of dragon, and its design feature is: a reactor is set, is provided with intensification chuck on the sidewall of described reactor; Be provided with agitator insert port, gas feed, bromine charge door, alkali lye charge door, gas vent and thermometer socket at the top of described reactor; Be provided with the discharging opening sealing by sealing-plug in the bottom of described reactor;
Agitator is inserted into reactor inside by agitator insert port, the bottom of agitator, is positioned at reactor inside center lower position and is connected with paddle;
One end of gas feed conduit is inserted in reactor by described gas feed, and the other end is connected with outside trifluoro propene storage tank by the first switch valve; On the sidewall of the bottom of described gas feed conduit, be provided with venthole;
One end of bromine conduit is inserted in reactor by described bromine charge door, and the other end is connected with the bromine storage tank that is positioned at reactor top by second switch valve;
One end of alkali lye conduit is inserted in reactor by described alkali lye charge door, and the other end is connected with the alkali lye storage tank that is positioned at reactor top by the 3rd switch valve;
One end of outtake tube is inserted in reactor by gas vent, and the other end is connected with the fractionating column that is positioned at reactor top by the 4th switch valve; The arm end of fractionating column passes into receiving flask, is inserted with the first thermometer in described fractionating column; Described receiving flask is placed in beaker;
The second thermometer is inserted in reactor by thermometer socket;
Be outside equipped with radiation source at described intensification chuck.
Synthesizer of the present invention, its design feature is also: described bromine conduit and described gas feed conduit are inserted into the bottom of reactor, described outtake tube and described alkali lye conduit are inserted into the top of reactor.
Described reactor is take clear glass as material.
Described venthole is one or more.
The contact position place of the contact position place of the contact position place of the contact position place of described gas feed place and gas feed conduit and described gas feed, described bromine charge door place and bromine conduit and described bromine charge door, described alkali lye charge door place and the contact position place of alkali lye conduit and described alkali lye charge door, described gas outlet and outtake tube and described gas vent, described the second thermometer and described thermometer socket is all take ground glass as material; The contact position place of described agitator and described agitator insert port is provided with the sealing ring take polytetrafluoroethylene (PTFE) as material.
Utilize the Kazakhstan dragon of synthesizer of the present invention to substitute the synthetic method of clean gas extinguishing chemical, its feature is to carry out as follows:
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, the trifluoro propene in trifluoro propene storage tank and bromine are passed in reactor by the amount of 1.01～1.15 times of stoichiometric proportions,, after waiting to ventilate, close the first switch valve; In intensification chuck and beaker, pass into temperature and be the cold water of-5～20 ℃, open the 4th switch valve;
The 3rd, the KOH that preparation mass concentration is 15～45% or the aqueous solution of NaOH, join in alkali lye storage tank, open the 3rd switch valve, the aqueous solution of the KOH in alkali lye storage tank or NaOH and bromine are joined in reactor by alkali lye conduit by the amount of 1.05～1.20 times of stoichiometric proportions; After treating the aqueous solution interpolation of KOH or NaOH, close the 3rd switch valve;
Finally, in reacting kettle jacketing, pass into temperature and be the hot water of 30～80 ℃, in receiving flask, collect target product; After collection, stop passing into hot water, after device is cooled to room temperature, open sealing-plug, emit salvage stores by discharge port, described target product is breathes out the alternative clean gas extinguishing chemical of dragon.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, in synthesizer of the present invention, can carry out addition, cancellation and three operating procedures of fractionation, whole synthesis flow obtains target product from being fed to, do not need through shifting any intermediate product, not only avoid loss of material, improve reaction yield, and save the reaction time, improved reaction efficiency;
2, the socket of reactor of the present invention top is connected with it conduit and interface are all glass frosted or teflon seal connection, do not use any rubber seal, have avoided the corrosion of bromine to sealing ring; In course of reaction without poisonous gas leakage, to operating personnel and Environmental security;
3, the end of air induction conduit of the present invention arranges multiple ventholes, is conducive to the abundant reaction between trifluoro propene gas and bromine;
4, synthesizer of the present invention has realized the unlatching of synthetic different phase or has cut out by multiple switch valves;
5, synthesizer simplicity of design of the present invention, compact conformation, easy to manufacture, cost is low, and floor space is little;
6, each parts regulation and control of synthesizer of the present invention are convenient, are easy to installing/dismounting and clean and preserve;
7, reactor of the present invention is colourless transparent glass manufacture, is convenient to observing response process.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Number in the figure: 1 reactor; 2 intensification chucks; 3 agitator insert ports; 4 agitators; 5 paddles; 6 gas feeds; 7 air induction conduits; 8 ventholes; 9 first switch valves; 10 trifluoro propene storage tanks; 11 bromine charge doors; 12 bromine conduits; 13 second switch valves; 14 bromine storage tanks; 15 alkali lye charge doors; 16 alkali lye conduits; 17 the 3rd switch valves; 18 alkali lye storage tanks; 19 gas vents; 20 outtake tubes; 21 the 4th switch valves; 22 fractionating columns; 23 first thermometers; 24 receiving flasks; 25 beakers; 26 discharging openings; 27 sealing-plugs; 28 thermometer sockets; 29 second thermometers; 30 radiation sources.
Specific embodiment
As shown in Figure 1, the synthesizer that the present embodiment is breathed out the alternative clean gas extinguishing chemical of dragon is that a reactor 1 is set, and is provided with intensification chuck 2 on the sidewall of reactor 1; Be provided with agitator insert port 3, gas feed 6, bromine charge door 11, alkali lye charge door 15, gas vent 19 and thermometer socket 28 at the top of reactor 1; Be provided with the discharging opening 26 sealing by sealing-plug 27 in the bottom of reactor 1;
One end of gas feed conduit 7 is inserted in reactor 1 by gas feed 6, and the other end is connected with outside trifluoro propene storage tank 10 by the first switch valve 9; On the sidewall of the bottom of gas feed conduit 7, be provided with venthole 8;
One end of bromine conduit 12 is inserted in reactor 1 by bromine charge door 11, and the other end is connected with the bromine storage tank 14 that is positioned at reactor top by second switch valve 13;
One end of alkali lye conduit 16 is inserted in reactor 1 by alkali lye charge door 15, and the other end is connected with the alkali lye storage tank 18 that is positioned at reactor top by the 3rd switch valve 17;
One end of outtake tube 20 is inserted in reactor 1 by gas vent 19, and the other end is connected with the fractionating column 22 that is positioned at reactor top by the 4th switch valve 21; The arm end of fractionating column 22 passes into receiving flask 24, is inserted with the first thermometer 23 in fractionating column 22; Receiving flask 24 is placed in beaker 25;
The second thermometer 29 is inserted in reactor 1 by thermometer socket 28; Be outside equipped with irradiation source 30 at intensification chuck 2.
In concrete enforcement, bromine conduit 12 and gas inlet ducts 7 are inserted into the bottom of reactor 1, and alkali lye conduit 16 and outtake tube 20 are inserted into the top of reactor 1, can reduce like this volatilization of bromine, and the contact area of augmenting response thing improves reaction efficiency.
Venthole 8 is set to multiple, is conducive to the abundant reaction between trifluoro propene gas and bromine.
The contact position place of contact position place, the second thermometer 29 and the thermometer socket 28 of contact position place, gas vent 19 places and outtake tube 20 and the gas vent 19 of contact position place, alkali lye charge door 15 places and alkali lye conduit 16 and the alkali lye charge door 15 of contact position place, bromine charge door 11 places and bromine conduit 12 and the bromine charge door 11 of gas feed 6 places and gas feed conduit 7 and gas feed 6 is all take ground glass as material; Agitator 4 is provided with the sealing ring take polytetrafluoroethylene (PTFE) as material with the contact position place of agitator insert port 3.
Utilizing the Kazakhstan dragon of the synthesizer of the present embodiment to substitute the synthetic method of clean gas extinguishing chemical, 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, start agitator 4;
Then, open radiation source 30, then open the first switch valve 9, the trifluoro propene in trifluoro propene storage tank 10 and bromine are passed in reactor 1 by the amount of 1.01～1.15 times of stoichiometric proportions,, after waiting to ventilate, close the first switch valve 9; In intensification chuck 2 and beaker 25, pass into temperature and be the cold water of-5～20 ℃, open the 4th switch valve 21;
The 3rd, the KOH that preparation mass concentration is 15～45% or the aqueous solution of NaOH, join in alkali lye storage tank 18, open the 3rd switch valve 17, the aqueous solution of the KOH in alkali lye storage tank 18 or NaOH and bromine are joined in reactor by alkali lye conduit 16 by the amount of 1.05～1.20 times of stoichiometric proportions; After treating the aqueous solution interpolation of KOH or NaOH, close the 3rd switch valve 17;
Finally, in reacting kettle jacketing 2, pass into temperature and be the hot water of 30～80 ℃, in receiving flask 24, collect target product; After collection, stop passing into hot water, after device is cooled to room temperature, open sealing-plug 27, emit salvage stores by discharge port 26, target product is breathes out the alternative clean gas extinguishing chemical of dragon.
Claims (6)
1. a synthesizer for gas extinguishing agent, is characterized in that: a reactor (1) is set, is provided with intensification chuck (2) on the sidewall of described reactor (1); Be provided with agitator insert port (3), gas feed (6), bromine charge door (11), alkali lye charge door (15), gas vent (19) and thermometer socket (28) at the top of described reactor (1); Be provided with in the bottom of described reactor (1) by the discharging opening (26) of sealing-plug (27) sealing;
Agitator (4) is inserted into reactor (1) inside by agitator insert port (3), the bottom of described agitator (4), is positioned at reactor (1) inside center lower position and is connected with paddle (5);
One end of gas feed conduit (7) is inserted in reactor (1) by described gas feed (6), and the other end is connected with outside trifluoro propene storage tank (10) by the first switch valve (9); On the sidewall of the bottom of described gas feed conduit (7), 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 connected with the bromine storage tank (14) that is positioned at reactor top by second switch valve (13);
One end of alkali lye conduit (16) is inserted in reactor (1) by described alkali lye charge door (15), and the other end is connected with the alkali lye storage tank (18) that is positioned at reactor top by the 3rd switch valve (17);
One end of outtake tube (20) is inserted in reactor (1) by gas vent (19), and the other end is connected with the fractionating column (22) that is positioned at reactor top by the 4th switch valve (21); The arm end of described fractionating column (22) passes into receiving flask (24), is inserted with the first thermometer (23) in described fractionating column (22); Described receiving flask (24) is placed in beaker (25);
The second thermometer (29) is inserted in reactor (1) by thermometer socket (28);
Be outside equipped with radiation source (30) at described intensification chuck (2).
2. synthesizer according to claim 1, it is characterized in that: described bromine conduit (12) and described gas feed conduit (7) are inserted into the bottom of reactor (1), described outtake tube (20) and described alkali lye conduit (16) are inserted into the top of reactor (1).
3. synthesizer according to claim 1, is characterized in that: described reactor (1) is take clear glass as material.
4. synthesizer according to claim 1, is characterized in that: described venthole (8) is for one or more.
5. synthesizer according to claim 1, it is characterized in that: described gas feed (6) is located and the contact position place of gas feed conduit (7) and described gas feed (6), described bromine charge door (11) is located and the contact position place of bromine conduit (12) and described bromine charge door (11), described alkali lye charge door (15) is located and the contact position place of alkali lye conduit (16) and described alkali lye charge door (15), described gas vent (19) is located and the contact position place of outtake tube (20) and described gas vent (19), the contact position place of described the second thermometer (29) and described thermometer socket (28) is all take ground glass as material, described agitator (4) is provided with the sealing ring take polytetrafluoroethylene (PTFE) as material with the contact position place of described agitator insert port (3).
6. a synthetic method of utilizing the gas extinguishing agent of synthesizer described in claim 1,2,3,4 or 5, is characterized in that carrying 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), start agitator (4);
Then, open radiation source (30), open again the first switch valve (9), the trifluoro propene in trifluoro propene storage tank (10) and bromine are passed in reactor (1) by the amount of 1.01～1.15 times of stoichiometric proportions, after waiting to ventilate, close the first switch valve (9); In intensification chuck (2) and beaker (25), pass into temperature and be the cold water of-5～20 ℃, open the 4th switch valve (21);
The 3rd, the KOH that preparation mass concentration is 15～45% or the aqueous solution of NaOH, join in alkali lye storage tank (18), open the 3rd switch valve (17), the aqueous solution of the KOH in alkali lye storage tank (18) or NaOH and bromine are joined in reactor by alkali lye conduit (16) by the amount of 1.05～1.20 times of stoichiometric proportions; After treating the aqueous solution interpolation of KOH or NaOH, close the 3rd switch valve (17);
Finally, in reacting kettle jacketing (2), pass into temperature and be the hot water of 30～80 ℃, in receiving flask (24), collect target product; After collection, stop passing into hot water, after device is cooled to room temperature, open sealing-plug (27), emit salvage stores by discharge port (26), described target product is gas extinguishing agent.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| CN103801248A true CN103801248A (en) | 2014-05-21 |
| CN103801248B CN103801248B (en) | 2016-08-17 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109516464A (en) * | 2019-01-21 | 2019-03-26 | 尹金彦 | A kind of brominated activated carbon process units |
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| 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 |
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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 |
Non-Patent Citations (2)
| Title |
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| 李丽娟: "《化工实验及开发技术》", 31 July 2002, 化学工业出版社, article "加热方式", pages: 13-16 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109516464A (en) * | 2019-01-21 | 2019-03-26 | 尹金彦 | A kind of brominated activated carbon process units |
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| CN103801248B (en) | 2016-08-17 |
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