CN109806816A - A kind of chlorination reaction device of continuous round-robin method production - Google Patents
A kind of chlorination reaction device of continuous round-robin method production Download PDFInfo
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Abstract
A kind of chlorination reaction device of continuous round-robin method production, is related to the technical field of chlorination reaction device.Chlorated liquid in chlorine and circulating pump enters in first-stage reactor, the output end of first-stage reactor and the input terminal of separator connect, first output end of separator and the input terminal of second reactor connect, the output end of second reactor and the input terminal of first-stage condenser connect, the output end of first-stage condenser and the input terminal of secondary condenser connect, and the output end of secondary condenser and the input terminal of demister connect;The input terminal connection of the first output end and hot-water cylinder on the plate heat exchanger of cooling water inlet is set, and the second output terminal of plate heat exchanger is connect with second reactor, and the third output end of plate heat exchanger is connect with first-stage reactor;The output end of hot-water cylinder is connect by heat-exchanger pump with first-stage reactor.It is simple that the present invention realizes structure, not only shortens the reaction time, but also vacate reaction compartment, being capable of continuous production, the purpose of efficient operation.
Description
Technical field
The present invention relates to the technical fields of chlorination reaction device.
Background technique
Monoxone is a kind of important organic fine industrial chemicals, mainly for the production of carboxymethyl cellulose, glycine, 2,
4-D acid, thioacetic acid, cyanoacetic acid, ethyl chloroacetate, iodoacetic acid, nitrilotriacetic acid, chloroacetonitrile, malonic acid, phenoxy acetic acid, cyanogen
The chemical intermediates such as acetic acid, methyl α-naphthyl acetate and product.Make pesticide made from raw material, medicine, carboxymethyl cellulose etc. with monoxone to produce
Product have biggish development, to chloroacetic demand also sustainable growth therewith.
Producing chloroacetic technique at present mostly uses greatly intermittent chlorination method to produce, and catalyst is sulphur or aceticanhydride.Acetic acid by
Elevated dosing vessel enters chlorination tank, is warming up to 70 °C of logical chlorine chlorinations after catalyst is added, and it is appropriate smaller to start logical chlorine dose.Chlorine
Changing reaction is exothermic reaction, and with the progress of reaction, chlorated liquid temperature is increased, and the cold true water of adjustment collet maintains temperature in the kettle at 100 °
C or so, and suitably increase logical chlorine dose.The tail gas that chlorination process generates recycles acyl chlorides therein, acetic acid etc. through condensed in two stages device, then
After washing, it is absorbed into absorption tower water and generates hydrochloric acid sale.React chloroacetic acid, two in a period of time post analysis chlorated liquid
Monoxone and acetic acid content, acetic acid content fewer reaction later period reduce logical chlorine dose, wait acetic acid contents less than 1~2% after stop
Logical chlorine.Chlorated liquid is put into crystallization kettle, and a certain amount of mother liquor, slow cooling is added.It, can be with after a large amount of chloroacetic acids are precipitated
Accelerate the rate of cooling.Crystal solution is down to close to after cooling water temperature, and crystal solution is put into centrifuge and isolates monoxone.
Either using sulphur or aceticanhydride as catalyst, equipment and technique only control temperature in chlorination without big difference
Slight difference on degree.The hydrogen chloride gas that chlorination reaction generates carries out multistage cold through main reaction kettle, condenser, secondary reacting kettle etc.
It is solidifying, first go rinsing bowl to wash, then 2 grade hydrochloric acid film-falling absorption towers is gone to absorb, wherein the acyl chlorides carried secretly, two sulphur of dichloro, acetic acid etc. are miscellaneous
Matter is washed thoroughly absorption.Increase water-washing process and sufficiently wash tail gas, do not allow impurity to take in byproduct hydrochloric acid, cleaning solution returns
Chlorination tank makees raw material, to reduce the consumption of raw material, improves the quality of byproduct hydrochloric acid.
Have the following problems in production processes of chloroacetic acid at present: acetic acid consumption is high.There is no chlorated liquid catalytic hydrogenation, causes vinegar
The consumption of acid is too high.It is unable to continuous production.
Summary of the invention
It is an object of the present invention to provide a kind of structure is simple, the reaction time is not only shortened, but also vacate reaction compartment, it can be continuous
The chlorination reaction device of production, the continuous round-robin method production of efficient operation.
A kind of chlorination reaction device of continuous round-robin method production, including circulating pump, chlorated liquid in chlorine and circulating pump into
Enter in first-stage reactor, the output end of first-stage reactor and the input terminal of separator connect, the first output end of separator and two
The input terminal of stage reactor connects, and the output end of second reactor and the input terminal of first-stage condenser connect, first-stage condenser
The connection of the input terminal of output end and secondary condenser, the output end of secondary condenser and the input terminal of demister connect;It is arranged cold
But the input terminal of the first output end on the plate heat exchanger of water inlet and hot-water cylinder connects, the second output terminal of plate heat exchanger
It is connect with second reactor, the third output end of plate heat exchanger is connect with first-stage reactor;The output end of hot-water cylinder passes through heat
Water pump is connect with first-stage reactor.
The present invention carries out chlorination reaction using continuous round-robin method, comes into full contact with gas-liquid, increases its residence time, using big
Flow chlorated liquid circulation, first order reaction and second order reaction system, while controlling the temperature of reaction process and enhancing gas-liquid contact
Disperse and mixes, the generation of the generation of controlling depth chlorination reaction, i.e. dichloride and terchoride.
The present invention carries out chlorination using continuous round-robin method, i.e., reaction chlorated liquid and chlorine flow into chlorination reaction according to a certain ratio
Device, stability contorting conversion zone temperature make reaction heat quantify releasing, and the product that simultaneous reactions generate also quantitatively is flowed out, both shortened
Reaction time, and reaction compartment is vacateed, production can continuous, efficient operation.The tail chlorine after chlorine gas liquefaction can be used in the present invention
As raw material chlorine without influencing product quality.
The utility model has the advantages that
1, from chlorination reaction mechanism it is found that reaction temperature, the mixability of reaction mass, depth of chlorination, catalyst amount and
Co-catalyst etc. is the principal element for influencing production process dichloride and generating.For the generation for reducing dichloride, improve simultaneously
Product quality, the present invention use second order reaction, and fully reacting makes the active principles such as catalyst that can not escape, is fully used,
Reduce consumption, save the cost.
2, the present invention uses big flow chlorated liquid circular response, chlorated liquid and chlorine 6 ~ 12:1 of molar ratio, can be very good
Reaction speed is controlled, chlorine energy 100% reacts, and tail gas is free of free chlorine, removes Alkali absorption free chlorine process, reduces cost.
3, the present invention uses chlorated liquid systemic circulation, and reaction chlorine can use the tail gas chlorine after liquefaction, solve at enterprise's tail gas
Manage difficult problem.
4, the present invention uses chlorated liquid systemic circulation, can effectively control chlorination reaction depth, guarantees that dichloride content exists
0.3% hereinafter, can remove high-pressure hydrogenation process in rear road product handling system technique, shortening process flow is kept the safety in production secure,
Equipment investment greatly reduces.
5, of the invention that reactor uses tower high efficiency reactor, first is that the specific surface area of filler is very big, gas-liquid contact is non-
Often sufficiently, fully reacting.Second is that the structure of tower eliminates wall flow phenomenon, effecting reaction is increased, improves reaction rate.Collet is used
Hot water circuit can effectively control reaction rate and depth of chlorination with stability contorting reaction temperature, contain the generation of dichloro trichlorine.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the invention.
Fig. 2 is the result schematic diagram of reactor of the present invention.
Specific embodiment
Technical solution of the present invention is described in detail with reference to the accompanying drawing:
As shown in Figure 1, a kind of chlorination reaction device of continuous production, including circulating pump 1, chlorine and the chlorination in circulating pump 1
Liquid enters in first-stage reactor 2, and the output end of first-stage reactor 2 is connect with the input terminal of separator 3, and the first of separator 3 is defeated
Outlet 31 is connect with the input terminal of second reactor 4, and the output end of second reactor 4 is connect with the input terminal of first-stage condenser 5,
The output end of first-stage condenser 5 is connect with the input terminal of secondary condenser 6, output end and the demister 10 of secondary condenser 6
Input terminal connection;The first output end being arranged on the plate heat exchanger 9 of cooling water inlet 91 is connect with the input terminal of hot-water cylinder 7,
The second output terminal of plate heat exchanger 9 is connect with second reactor 4, the third output end and first-stage reactor 2 of plate heat exchanger 9
Connection;The output end of hot-water cylinder 7 is connect by heat-exchanger pump 8 with first-stage reactor 2.
As shown in Fig. 2, first-stage reactor 2 of the invention, second reactor 4 include multiple groups packed tower, on every group of packed tower
Gas feed 221, exhaust outlet 228 is respectively set, also sets up the material inlet 223 for being passed through chlorated liquid, mixture export 222 is located at
Temperature-measuring port 224 is arranged in the upper end of the upper end of reactor, reactor;Cooling water inlet 225, hot water outlet 226 are arranged in instead
It answers on the side wall of device;Discharging hole 227 is set in the sidewall of reactor near material inlet 223.
As shown in Figure 1, the steam inlet 71 for being passed through steam is arranged on hot-water cylinder 7 of the invention.
As shown in Figure 1, the cooling water inlet for being passed through cooling water is arranged on hot-water cylinder 7 of the invention.
As shown in Figure 1, the material liquid import 41 for being passed through material liquid is arranged on second reactor 4 of the invention.
As shown in Figure 1, the second order reaction cooling water outlet for cooling water to be discharged is arranged on second reactor 4 of the invention
42。
As shown in Figure 1, the catalyst inlet 43 for being passed through catalyst is arranged on second reactor 4 of the invention.
As shown in Figure 1, being arranged in first-stage condenser 5 of the invention for being passed through water inlet in the freezing that 0 degree freezes upper water
51;Level-one water return outlet 52 of the setting for level-one freezing return water in first-stage condenser 5.
As shown in Figure 1, the chilled water import 61 for being passed through -15 degree chilled waters is arranged on secondary condenser 6 of the invention;
Second level water return outlet 62 of the setting for second level freezing return water on secondary condenser 6.
A large amount of chlorated liquids of chlorine and circulating pump 1 of the invention enter right after progress chlorination reaction in first-stage reactor 2
Enter separator 3 afterwards, the mixed liquor in separator 3 is heated at driving initial stage by steam, after reaching reaction temperature, certainly by automatic valve
The dosage of adjusting steam is moved to control the temperature in separator, guarantees the reaction temperature needed in first-stage reactor 2.First order reaction
The heat that generation is reacted in device 2 is removed by the hot water that heat-exchanger pump 8 is sent from collet, and controls reaction temperature by hot water, in chlorination
Liquid hold-up reaches 80% or so, and when two chlorinities 0.3%, reaction reaches balance, beginning continuous production.Hydrogen chloride in separator 3
And the active constituent of entrainment enters in second reactor 4, with the raw material and second reactor middle part come from 4 tower top of second reactor
Next catalyst (if needing catalyst) counter current contacting is simultaneously reacted, and the chlorine for the traces of unreacted carried secretly in mixed gas then may be used
With the reaction was continued and cooling, the intermediate active product of entrainment and light group unreacted through first-stage condenser 5, secondary condenser 6
Divide and be trapped, tail gas hydrogen chloride is gone down after demister 10 further recycling intermediate active product and the purification of unreacted light component
Process.The active material that the light component of recycling and reaction generate is added to 2 lower part of first-stage reactor through circulating pump 1, continues to participate in anti-
It answers, cuts down the consumption of raw materials.Fresh feed and catalyst are added to after metering in second reactor 4.Chlorated liquid in separator 3 is used
Pumping, which goes out to be sent to rectifying, sets, the active material of recycling raw material and reaction generation, then finished product packing.
1, reaction temperature is reduced, the selectivity of reaction is improved:
Since reaction temperature directly affects the selectivity that chlorine atom replaces in chlorination reaction, the high side reaction Probability of reaction temperature
Increase.By consulting the activation energy of chlorination main side effect it is found that chlorination reaction generates the activation energy of dichloride higher than chlorination life
At the activation energy of monochloride, at the same temperature, monochloride generating rate is greater than the generating rate of dichloride, if instead
Temperature is answered to increase, then the reaction rate for generating dichloride is accelerated, and reaction selectivity reduces.But the too low chlorination process reaction of temperature
Speed is very slow.Reaction temperature can be strictly controlled in continuous round-robin method chlorination process, no more than ± 1 DEG C of set temperature.
2, reaction process is strengthened, and accelerates reaction speed:
For the reaction of most of gas-liquid two-phase, reaction speed generally depends on the control of entire mass transfer to reaction process.Even
Gas-liquid can generate phase interface that is huge and quickly updating in new and effective main reactor in continuous round-robin method chlorination process, make alternate
Mass transfer rate is than improving 1~3 order of magnitude in traditional tower, and even hundred times than high ten times in stirred tank.Its reaction solution mixing and
Mass transport process is greatly strengthened.That is good dispersion between gas-liquid can accelerate reaction speed.
3, it controls depth of chlorination, reduce side reaction:
Depth of chlorination is high, and the utilization rate of raw material is high, but easily causes the generation of polychloride.The selectivity of monochloride reduces,
The quality and yield for making product are affected.Therefore, select suitable depth of chlorination extremely important.The ratio of raw material and chlorine with
Depth of chlorination is associated, exactly participate in reaction raw material and chlorine weight ratio, under the conditions of gas-liquid two-phase is evenly dispersed, ratio compared with
When big, i.e., material liquid is significantly excessive, and the selectivity of monochloro improves, and the production quantity of dichloride is lower.Conversely, the choosing of monochloro compound
Selecting property reduces, and the dichloride of generation is more.Due to being circular response, that is, internal circulating load is especially big in the chlorated liquid recycled, chlorination
The absolute weight of raw material is also big in liquid, can reduce side reaction in this way.Chlorated liquid is adjusted in continuous round-robin method chlorination process
With chlorine 6~12:1 of molar ratio, i.e., reacted using a large amount of circulation chlorated liquid with chlorine.We can be effectively controlled chlorated liquid
For middle monochloride content at 80% or so, dichloride content is less than 0.3%, and no terchoride generates, due to a large amount of chlorated liquids
Circulation, material quantity is significantly excessive, can chlorine be reacted completely, and free chlorine is not present in chlorated liquid.
4, catalyst loss amount is reduced, production cost is reduced:
The present invention uses two-stage reactor, and chlorated liquid after first-stage reactor is reacted carries out gas-liquid separation, hydrogen chloride and not anti-
The intermediate active substance etc. for answering complete chlorine entrainment material liquid, reaction to generate enters second reactor bottom, comes with top
The catalyst that material liquid and middle part are come counter current contacting reaction in second reactor generates intermediate active substance, cold through subcooler
But temperature drops to 35 degree hereinafter, being far below the boiling point of these materials and being trapped, and increase precision again after cooler and catch after
The droplet retention that storage will likely be carried secretly, accurate filter can recycle most originals with the droplet of 100% trapping 1u or more
Material and catalyst and useful intermediate active substance, greatly reduce cost.
5, using new and effective reactor:
First-stage reactor of the invention, second reactor use gas-liquid two-phase reactor.The characteristics of gas-liquid two-phase reactor, is: chlorine
Change reaction tower to be made of the packed tower that multiple trourelles pass through, using the filler of bigger serface, eliminates the wall of common fillers tower
Flow phenomenon, uniform gas-liquid distribution considerably increase gas-liquid two-phase collision probability, while increasing the residence time of gas phase, improve
Reaction efficiency.Reaction tower increase it is jacket structured, reaction temperature can by the hot water of reactor jacket come automatic and accurate control,
The progress that can inhibit side reaction avoids cooling water with hot water circuit and the chlorated liquid temperature difference is too big, directly anti-using cooling water
The drawbacks of answering temperature to be difficult control.Because dichloride content is very low in entire production technology, hydrogenation process is eliminated without making
Adding hydrogen tower with high temperature and pressure, eliminates the investment of precious metals palladium catalyst, process flow is shortened, and equipment investment substantially reduces,
Device operating cost, process operability and safety greatly improve.
Claims (9)
1. a kind of chlorination reaction device of continuous round-robin method production, it is characterised in that including circulating pump (1), chlorine and circulating pump
(1) chlorated liquid in enters in first-stage reactor (2), and the output end of first-stage reactor (2) and the input terminal of separator (3) connect
It connects, the first output end (31) of separator (3) is connect with the input terminal of second reactor (4), the output end of second reactor (4)
It being connect with the input terminal of first-stage condenser (5), the output end of first-stage condenser (5) is connect with the input terminal of secondary condenser (6),
The output end of secondary condenser (6) is connect with the input terminal of demister (10);The plate heat exchanger of cooling water inlet (91) is set
(9) the first output end on is connect with the input terminal of hot-water cylinder (7), the second output terminal and second order reaction of plate heat exchanger (9)
Device (4) connection, the third output end of plate heat exchanger (9) are connect with first-stage reactor (2);The output end of hot-water cylinder (7) passes through
Heat-exchanger pump (8) is connect with first-stage reactor (2).
2. the chlorination reaction device of continuous round-robin method production according to claim 1, it is characterised in that above-mentioned first order reaction
Device (2), second reactor (4) include multiple groups packed tower, and gas feed (221), exhaust outlet are respectively set on every group of packed tower
(228), the material inlet (223) for being passed through chlorated liquid is also set up, mixture export (222) is located at the upper end of reactor, reactor
Upper end be arranged temperature-measuring port (224);Cooling water inlet (225), hot water outlet (226) are arranged on the side wall of reactor;
Discharging hole (227) are set in the sidewall of reactor of material inlet (223) nearby.
3. the chlorination reaction device of continuous round-robin method production according to claim 1, it is characterised in that above-mentioned hot-water cylinder (7)
The upper steam inlet (71) being arranged for being passed through steam.
4. the chlorination reaction device of continuous round-robin method production according to claim 1, it is characterised in that above-mentioned hot-water cylinder (7)
The upper cooling water inlet being arranged for being passed through cooling water.
5. the chlorination reaction device of continuous round-robin method production according to claim 1, it is characterised in that above-mentioned second order reaction
Material liquid import (41) for being passed through material liquid is set on device (4).
6. the chlorination reaction device of continuous round-robin method production according to claim 1, it is characterised in that above-mentioned second order reaction
Second order reaction cooling water outlet (42) for cooling water to be discharged is set on device (4).
7. the chlorination reaction device of continuous round-robin method production according to claim 1, it is characterised in that above-mentioned second order reaction
Catalyst inlet (43) for being passed through catalyst is set on device (4).
8. the chlorination reaction device of continuous round-robin method production according to claim 1, it is characterised in that above-mentioned level-one condensation
It is arranged on device (5) for being passed through water inlet (51) in the freezing that 0 degree freezes upper water;Setting is used for level-one in first-stage condenser (5)
Freeze the level-one water return outlet (52) of return water.
9. the chlorination reaction device of continuous round-robin method production according to claim 1, it is characterised in that above-mentioned B-grade condensation
Chilled water import (61) for being passed through -15 degree chilled waters is set on device (6);Setting is cold for second level on secondary condenser (6)
Freeze the second level water return outlet (62) of return water.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111320544A (en) * | 2020-04-13 | 2020-06-23 | 湖北可赛化工有限公司 | Process and equipment for three-stage semi-continuous synthesis of bis (trichloromethyl) carbonate |
CN113477208A (en) * | 2021-06-16 | 2021-10-08 | 湖北泰盛化工有限公司 | Chloroacetic acid production device and process |
CN117776855A (en) * | 2024-02-27 | 2024-03-29 | 山东新龙科技股份有限公司 | Continuous production method and device for refining tetrachloroethane by reaction |
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CN106242961A (en) * | 2016-07-29 | 2016-12-21 | 河北科技大学 | Production of chloroacetic acid equipment |
CN109134231A (en) * | 2018-10-30 | 2019-01-04 | 杭州众立化工科技有限公司 | A kind of chloroacetic device and process of differential circulation continuous production |
CN209791506U (en) * | 2019-03-28 | 2019-12-17 | 南京嘉源润新环保科技有限公司 | chlorination reaction device for continuous circulation production |
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CN205443146U (en) * | 2016-03-14 | 2016-08-10 | 中昊晨光化工研究院有限公司 | A device for adjusting polytetrafluoroethylene reaction temperature |
CN106242961A (en) * | 2016-07-29 | 2016-12-21 | 河北科技大学 | Production of chloroacetic acid equipment |
CN109134231A (en) * | 2018-10-30 | 2019-01-04 | 杭州众立化工科技有限公司 | A kind of chloroacetic device and process of differential circulation continuous production |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111320544A (en) * | 2020-04-13 | 2020-06-23 | 湖北可赛化工有限公司 | Process and equipment for three-stage semi-continuous synthesis of bis (trichloromethyl) carbonate |
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CN113477208B (en) * | 2021-06-16 | 2022-10-04 | 湖北泰盛化工有限公司 | Chloroacetic acid production device and process |
CN117776855A (en) * | 2024-02-27 | 2024-03-29 | 山东新龙科技股份有限公司 | Continuous production method and device for refining tetrachloroethane by reaction |
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