CN209721581U - Improve the hydrogen chloride synthesis system of product purity - Google Patents

Improve the hydrogen chloride synthesis system of product purity Download PDF

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Publication number
CN209721581U
CN209721581U CN201821948469.8U CN201821948469U CN209721581U CN 209721581 U CN209721581 U CN 209721581U CN 201821948469 U CN201821948469 U CN 201821948469U CN 209721581 U CN209721581 U CN 209721581U
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hydrogen chloride
hot water
microreactor
hydrogen
synthesis system
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文仕敏
邓敏
王政强
徐慧远
缑可贞
谢濠江
佘国华
高在平
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Yibin Tianyuan Group Co Ltd
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Yibin Tianyuan Group Co Ltd
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Abstract

The utility model discloses a kind of hydrogen chloride synthesis systems for improving product purity, it is characterized in that substituting synthetic furnace with microreactor.The utility model has the advantages that: 1) compared with prior art hydrogen chloride product purity significantly improve, and embodiment according to the present utility model, hydrogen chloride product purity can reach 98% or more;2) micro- reaction system structure that the utility model uses is simple, and only needing same unit device to be arranged in juxtaposition can reach scale mass production purpose, produce it is easy to control, using industrially promoting.

Description

Improve the hydrogen chloride synthesis system of product purity
Technical field
The utility model relates to a kind of hydrogen chloride synthesis devices.
Background technique
Hydrogen chloride, molecular formula HCl are a kind of gas of colourless irritant smell, are made of chlorine atom and hydrogen atom.Its Aqueous solution is commonly called as hydrochloric acid, relative molecular mass 36.5.Mainly for the preparation of dyestuff, drug, fragrance, organic-inorganic chloride etc..
Usual hydrogen chloride gas is prepared using synthetic furnace, there is steel synthetic furnace, graphitic synthetic furnace, the free air cooling of heat transfer type But formula and two kinds of water-cooling jacket.Steel synthetic furnace holds corrosion-vulnerable at the top and bottom of furnace, and service life is short, few at present Enterprise uses.And graphitic synthetic furnace has many advantages, such as corrosion-resistant, high temperature resistant, is the mainstream synthetic furnace of current synthesising hydrogen.Example As the patent document of the production method of the entitled reagent grade hydrochloric acid of Publication No. CN1640813A describes a kind of compare more typically The method using graphitic synthetic furnace synthesising hydrogen.Using hydrogen chloride gas purity prepared by graphitic synthetic furnace be usually 91~ 94%.
Utility model content
For the purity for improving chlorination hydrogen production, the utility model provides a kind of hydrogen chloride synthesis system for improving product purity System.
The technical scheme adopted by the utility model is improving the hydrogen chloride synthesis system of product purity, it is characterised in that: Including microreactor, synthetic reaction carries out in microreactor.
The gaseous mixture of hydrogen and chlorine is a kind of explosive gaseous mixture, and explosion limit is 5%~87.5% (volume hundred Divide ratio), range is very wide.In prior art, the lamp cap that chlorine and hydrogen are passed through graphite furnace simultaneously mixed after with igniting dress Igniting is set, and since two kinds of gases are there are biggish density variation, it cannot accomplish absolutely to be sufficiently mixed, and graphite furnace volume is big, Hydrogen molecule is more, chlorine molecule is also more, and contact area is big, and the heat that when burning generates is more, while the production of hydrogen chloride at present Journey is continuous production process, and hydrogen and chlorine, which constantly enter graphite furnace also, causes the risk of mixed gas part inhomogeneities to increase Add, if within the scope of explosion limit, the rapid spatial expansion of mixed gas in the confined space is easy to happen explosion.Currently The generation that technical staff is exploded in order to prevent, generally use the hydrogen that is passed through it is much more excessive than chlorine (molar ratio hydrogen: chlorine= 1.1~1.2:1) mode, in practice it has proved that the program can effectively prevent that safety accident occurs, but this scheme causes simultaneously Hydrogen content is high and lead to the reduction of chlorination hydrogen purity in chlorination hydrogen production.
In the present invention, inventor is using microreactor substitution graphitic synthetic furnace as synthesizer, due to micro- reaction The hydraulic diameter of the microchannel of device is only 0.1~5mm, therefore microreactor device hydrogen is lacked by what pipeline was discharged, with chlorine The contact area very little of gas is scattered and disappeared quickly even if the heat of generation is few within the scope of explosion limit, will not be exploded;Cause This is without ensuring hydrogen much excessive the problem of also there is no security risks, it is only necessary to maintain stable reaction to carry out, omit hydrogen A micro- excess, as described above, the reduction of hydrogen ratio is so that therefore product purity is also improved, to realize practical Novel purpose.React the hydrogen chloride gas generated can enter after hydrogen chloride cooler is cooling hydrogen chloride buffer tank storage to With.
In above scheme, since the hydraulic diameter of the microchannel of microreactor is only 0.1~5mm, it is difficult to realize hydrogen Gas and chlorine are passed through microchannel simultaneously and guarantee that the uniformity in microchannel can stablize progress to guarantee to react, because This utility model is also provided with micro-mixer, by hydrogen and chlorine are passed through in micro-mixer simultaneously by certain flow ratio into Microreactor is entered back into after row premixing uniformly, to overcome the above problem.
To prevent the temperature of microreactor excessively high, corresponding heat-exchange system can be set, reaction temperature is controlled, hold Intelligible, the common all kinds of heat-exchange systems in this field, such as circulation can be used in heat-exchange system, and specific arragement construction can To be designed according to the structure of microreactor, such as a kind of preferred scheme is inventors herein proposed in the present invention: this The microreactor of utility model may include air-tight chamber and the reaction zone that is arranged in air-tight chamber, the reaction zone It is provided at least one microchannel, and hot water cyclesystem is set simultaneously, hot water cyclesystem includes and microreactor The circulating hot water upper hose and circulating hot water return pipe of air-tight chamber connection.In the equipment course of work, circulating hot water passes through The circulating hot water upper hose of hot water cyclesystem enters in the air-tight chamber of microreactor, in the microchannel of reaction zone Indirect heat exchange occurs for portion's reactant, by the hot temperature of control loop and flow by reaction temperature control at 1500~2500 DEG C, with It is carried out conducive to reaction and ensures safety.Hot water cyclesystem can also further be improved, such as increase the separation of liquid vapour Equipment, the circulating hot water after heat exchange form steam mixture and pass through hot water cyclesystem recovery section heat as a vapor, Circulating hot water, which then returns to microreactor by water supply pipeline, to be continued to take away heat of reaction, and the heat of recycling can be used for needing steam The workshop section heated.
It is respectively arranged on the inlet duct and outlet conduit of micro-mixer as a further improvement of the utility model, Temperature monitor and pressure sensor;On-line detector, temperature monitor and pressure are provided on the microreactor outlet conduit Force snesor, the on-line detector include hydrogen chloride purity detecting instrument and free chlorine contents detector;The hydrogen chloride buffering Tank is provided with pressure sensor;In order to be monitored to production process.
The invention also discloses a kind of methods using micro- reaction system production hydrogen chloride, comprising the following steps:
A, by dry hydrogen and chlorine according to the molar ratio hydrogen of flows per unit time: chlorine=1.01~1.05:1 Ratio is passed through in micro-mixer is sufficiently mixed simultaneously, obtains mixed gas;
B, enter microreactor from the mixed gas that micro-mixer comes out, pass through igniter provocative reaction, mixed gas Reaction generates hydrogen chloride gas in microchannel, while circulating hot water passes through the circulating hot water upper hose of hot water cyclesystem Into in the air-tight chamber of microreactor, indirect heat exchange occurs with the microchannel internal-response object of reaction zone, passes through control Circulating hot water temperature processed and flow control reaction temperature at 1500~2500 DEG C;The mixed gas is in microchannel It is 5~20s by the time;
C, the hydrogen chloride gas that reaction generates obtains chlorination hydrogen production after cooling.
The production that micro- reaction system based on the utility model carries out hydrogen chloride can be realized using this method.
The beneficial effects of the utility model are: 1) hydrogen chloride product purity significantly improves compared with prior art, according to this The embodiment of utility model, hydrogen chloride product purity can reach 98% or more;2) micro- reaction system knot that the utility model uses Structure is simple, and only needing same unit device to be arranged in juxtaposition can reach scale mass production purpose, and production is easy to control, conducive to producing It is promoted in industry.
Detailed description of the invention
Fig. 1 is the hydrogen chloride synthesis system structure diagram of the raising product purity of the utility model.
In the figure, it is marked as 1- micro-mixer, 2- microreactor, 201- air-tight chamber, 202- reaction zone, 3- chlorination are hydrogen-cooled But device, 4- hydrogen chloride buffer tank, 5- hot water cyclesystem, 501- circulating hot water upper hose, 502- circulating hot water return pipe, 6- point Fiery device, 7- circulation, 8- hydrogen gas tank, 9- chlorine pot, PI01- hydrogen pressure tank, PI02- chlorine pressure tank, PI03- are micro- Mixer outlet gas pressure, PI04- microreactor outlet gas pressure, PI05- hydrogen chloride buffer tank pressure;TI01- hydrogen Temperature, TI02- chlorine temperature, TI03- micro-mixer Outlet Gas Temperature, TIC04- microreactor Outlet Gas Temperature, TIC05- hydrogen chloride cooler outlet pipe temp;FQIC01- hydrogen flowmeter, FQIC02- cl gas flow meter;FV01- hydrogen stream Adjustable valve, FV02- chlorine flowrate regulating valve, TV01- circulating hot water regulating valve, TV02- hydrogen chloride cooler recirculated water are adjusted Valve;CICR01- on-line checking point.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and examples.
As shown in Figure 1, the hydrogen chloride synthesis system of the raising product purity of the utility model, including by process pipe according to The micro-mixer 1 of secondary connection, microreactor 2, hydrogen chloride cooler 3, hydrogen chloride buffer tank 4;It further include hot water cyclesystem 5, Igniter 6, circulation 7, hydrogen gas tank 8 and chlorine pot 9;The hydrogen gas tank 8, chlorine pot 9 are connect with micro-mixer 1, institute State igniter 6, hot water cyclesystem 5 is connect with microreactor 2, the circulation 7 is connect with hydrogen chloride cooler 4; The microreactor 2 includes air-tight chamber 201 and the reaction zone 202 being arranged in air-tight chamber 201, the reaction zone 202 are provided with several microchannels;The hot water cyclesystem 5 includes being connected to the air-tight chamber 202 of microreactor 2 Circulating hot water upper hose 501 and circulating hot water return pipe 502;Divide equally on the inlet duct and outlet conduit of the micro-mixer 1 Temperature monitor and pressure sensor are not provided with it;On-line detector, temperature inspection are provided on 2 outlet conduit of microreactor It surveys instrument and pressure sensor, the on-line detector includes hydrogen chloride purity detecting instrument and free chlorine contents detector;The chlorine Change hydrogen surge tank 4 and is provided with pressure sensor.
Embodiment one:
The production of hydrogen chloride is used for using above-mentioned apparatus according to the following steps:
(1) by Jing Guo Gan Zaochuliing hydrogen and chlorine each lead into hydrogen gas tank 8, in chlorine pot 9;Open simultaneously hydrogen and Chlorine intake valve makes hydrogen and chlorine while entering the two entrances of micro-mixer 1, regulates and controls the molar flow ratio of hydrogen and chlorine Hydrogen: chlorine=1.01:1.0 ratio is passed through micro-mixer 1 and is uniformly mixed, and obtains mixed gas;
(2) enter microreactor 2 from the mixed gas that micro-mixer 1 comes out, pass through 6 provocative reaction of igniter, mixing Gas reacts in microchannel generates hydrogen chloride gas, while circulating hot water passes through the circulating hot water of hot water cyclesystem 5 Upper hose 501 enters in the air-tight chamber 201 of microreactor 2, occurs with the microchannel internal-response object of reaction zone 202 Indirect heat exchange, the circulating hot water shape by control loop hot water temperature and flow by reaction temperature control at 1900 DEG C, after heat exchange After recycling heat generation steam by hot water cyclesystem 5 at hot water and vapor mixture, circulating hot water passes through circulating hot water and returns Water pipe 502 returns to the heat for taking away microreactor generation, and the steam pressure is 0.5MPa;The mixed gas is being reacted In microchannel is 10s by the time;
(3) enter hydrogen chloride cooler 3 by the hydrogen chloride gas that the reaction of microreactor 2 generates to store after circulating water It is stored in hydrogen chloride buffer tank 4, measuring gained hydrogen chloride product purity is 98.7%.
Embodiment two:
The production of hydrogen chloride is used for using above-mentioned apparatus according to the following steps:
(1) by Jing Guo Gan Zaochuliing hydrogen and chlorine each lead into hydrogen gas tank 8, in chlorine pot 9;Open simultaneously hydrogen and Chlorine intake valve makes hydrogen and chlorine while entering the two entrances of micro-mixer 1, regulates and controls the molar flow ratio of hydrogen and chlorine Hydrogen: chlorine=1.03:1.0 ratio is passed through micro-mixer 1 and is uniformly mixed, and obtains mixed gas;
(2) enter microreactor 2 from the mixed gas that micro-mixer 1 comes out, pass through 6 provocative reaction of igniter, mixing Gas reacts in microchannel generates hydrogen chloride gas, while circulating hot water passes through the circulating hot water of hot water cyclesystem 5 Upper hose 501 enters in the air-tight chamber 201 of microreactor 2, occurs with the microchannel internal-response object of reaction zone 202 Indirect heat exchange, the circulating hot water shape by control loop hot water temperature and flow by reaction temperature control at 2100 DEG C, after heat exchange After recycling heat generation steam by hot water cyclesystem 5 at hot water and vapor mixture, circulating hot water passes through circulating hot water and returns Water pipe 502 returns to the heat for taking away microreactor generation, and the steam pressure is 1.1MPa;The mixed gas is being reacted In microchannel is 12s by the time;
(3) enter hydrogen chloride cooler 3 by the hydrogen chloride gas that the reaction of microreactor 2 generates to store after circulating water It is stored in hydrogen chloride buffer tank 4, measuring gained hydrogen chloride product purity is 98.5%.
Embodiment three:
The production of hydrogen chloride is used for using above-mentioned apparatus according to the following steps:
(1) by Jing Guo Gan Zaochuliing hydrogen and chlorine each lead into hydrogen gas tank 8, in chlorine pot 9;Open simultaneously hydrogen and Chlorine intake valve makes hydrogen and chlorine while entering the two entrances of micro-mixer 1, regulates and controls the molar flow ratio of hydrogen and chlorine Hydrogen: chlorine=1.05:1.0 ratio is passed through micro-mixer 1 and is uniformly mixed, and obtains mixed gas;
(2) enter microreactor 2 from the mixed gas that micro-mixer 1 comes out, pass through 6 provocative reaction of igniter, mixing Gas reacts in microchannel generates hydrogen chloride gas, while circulating hot water passes through the circulating hot water of hot water cyclesystem 5 Upper hose 501 enters in the air-tight chamber 201 of microreactor 2, occurs with the microchannel internal-response object of reaction zone 202 Indirect heat exchange, the circulating hot water shape by control loop hot water temperature and flow by reaction temperature control at 2100 DEG C, after heat exchange After recycling heat generation steam by hot water cyclesystem 5 at hot water and vapor mixture, circulating hot water passes through circulating hot water and returns Water pipe 502 returns to the heat for taking away microreactor generation, and the steam pressure is 1.9MPa;The mixed gas is being reacted In microchannel is 18s by the time;
(3) enter hydrogen chloride cooler 3 by the hydrogen chloride gas that the reaction of microreactor 2 generates to store after circulating water It is stored in hydrogen chloride buffer tank 4, measuring gained hydrogen chloride product purity is 98.1%.
The above, only the utility model enumerate preferable example, do not make in any form to the utility model With substantial limitation, it is noted that for those skilled in the art, in the premise for not departing from the utility model method Under, the numerous improvement that can also be made and supplement, these are improved and supplement should also be as being considered as the protection scope of the utility model.It is all In the case where not departing from the spirit and scope of the utility model, made when using the revealed content of the above utility model Variation, modification and differentiation equivalent variations, be the equivalent embodiment of the utility model;Meanwhile it is all according to the utility model Variation, modification and differentiation of the substantial technological to any equivalent variations made by above-described embodiment, should belong to the utility model Technical solution in the range of.

Claims (4)

1. improving the hydrogen chloride synthesis system of product purity, it is characterised in that: including microreactor (2), synthetic reaction is micro- anti- It answers in device (2) and carries out;The microreactor (2) includes air-tight chamber (201) and is arranged in air-tight chamber (201) Reaction zone (202), the reaction zone (202) are provided at least one microchannel;The hydraulic diameter of the microchannel For 0.1~5mm.
2. the hydrogen chloride synthesis system according to claim 1 for improving product purity, it is characterised in that: the raising product The hydrogen chloride synthesis system of purity includes by the sequentially connected micro-mixer of process pipe (1), microreactor (2), hydrogen chloride Cooler (3), hydrogen chloride buffer tank (4);It further include the igniter (6) for provocative reaction.
3. the hydrogen chloride synthesis system according to claim 1 for improving product purity, it is characterised in that: the raising product The hydrogen chloride synthesis system of purity further includes hot water cyclesystem (5), and the hot water cyclesystem (5) includes and microreactor (2) the circulating hot water upper hose (501) and circulating hot water return pipe (502) of air-tight chamber (201) connection.
4. the hydrogen chloride synthesis system according to claim 2 for improving product purity, it is characterised in that: the micro-mixer (1) temperature monitor and pressure sensor are respectively arranged on inlet duct and outlet conduit;The microreactor (2) goes out It is provided with on-line detector, temperature monitor and pressure sensor on mouth pipeline, the on-line detector includes chlorination hydrogen purity Detector and free chlorine contents detector;The hydrogen chloride buffer tank (4) is provided with pressure sensor.
CN201821948469.8U 2018-11-23 2018-11-23 Improve the hydrogen chloride synthesis system of product purity Active CN209721581U (en)

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Application Number Priority Date Filing Date Title
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