CN209791506U - chlorination reaction device for continuous circulation production - Google Patents
chlorination reaction device for continuous circulation production Download PDFInfo
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- CN209791506U CN209791506U CN201920405600.4U CN201920405600U CN209791506U CN 209791506 U CN209791506 U CN 209791506U CN 201920405600 U CN201920405600 U CN 201920405600U CN 209791506 U CN209791506 U CN 209791506U
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Abstract
A chlorination reaction device for continuous circulation production relates to the technical field of chlorination reaction devices. Chlorine and a chlorination solution in a circulating pump enter a primary reactor, the output end of the primary reactor is connected with the input end of a separator, the first output end of the separator is connected with the input end of a secondary reactor, the output end of the secondary reactor is connected with the input end of a primary condenser, the output end of the primary condenser is connected with the input end of a secondary condenser, and the output end of the secondary condenser is connected with the input end of a demister; a first output end of the plate heat exchanger provided with a cooling water inlet is connected with an input end of the hot water tank, a second output end of the plate heat exchanger is connected with the secondary reactor, and a third output end of the plate heat exchanger is connected with the primary reactor; the output end of the hot water tank is connected with the first-stage reactor through a hot water pump. The utility model discloses realized simple structure, both shortened reaction time, vacated the reaction space again, purpose that can continuous production, high-efficient operation.
Description
Technical Field
The utility model relates to a technical field of chlorination reaction unit.
Background
Chloroacetic acid is an important organic fine chemical raw material, and is mainly used for producing chemical intermediates and products such as carboxymethyl cellulose, glycine, 2, 4-D acid, thioglycollic acid, cyanoacetic acid, ethyl chloroacetate, iodoacetic acid, nitrilotriacetic acid, chloroacetonitrile, malonic acid, phenoxyacetic acid, cyanoacetic acid, naphthylacetic acid and the like. The pesticide, medicine, carboxymethyl cellulose and other products prepared by using chloroacetic acid as raw material have been developed greatly, and the demand for chloroacetic acid is continuously increased.
Most of the prior processes for producing chloroacetic acid adopt an intermittent chlorination method, and a catalyst is sulfur or acetic anhydride. Acetic acid enters the chlorination kettle from the high-level metering tank, the temperature is raised to 70 ℃ after the catalyst is added, chlorine is introduced for chlorination, and the chlorine introduction amount is appropriately smaller. The chlorination reaction is an exothermic reaction, the temperature of the chlorination liquid rises along with the reaction, the temperature in the kettle is maintained at about 100 ℃ by adjusting the cold water of the jacket, and the chlorine passing amount is increased properly. The tail gas generated in the chlorination process is subjected to two-stage condenser to recover acyl chloride, acetic acid and the like, and then is washed by water and enters an absorption tower to be absorbed by water to generate hydrochloric acid for sale. And after the reaction is carried out for a period of time, analyzing the contents of monochloroacetic acid, dichloroacetic acid and acetic acid in the chlorination solution, reducing the chlorine introduction amount in the later reaction period with less acetic acid content, and stopping chlorine introduction when the acetic acid content is less than 1-2%. And (3) putting the chlorination solution into a crystallization kettle, adding a certain amount of mother solution, and slowly cooling. When a large amount of monochloroacetic acid is separated out, the cooling rate can be increased. And (4) after the temperature of the crystallization liquid is reduced to be close to the temperature of cooling water, putting the crystallization liquid into a centrifugal machine to separate chloroacetic acid.
No matter sulfur or acetic anhydride is adopted as a catalyst, the equipment and the process have no big difference, and only have slight difference on the chlorination control temperature. The hydrogen chloride gas generated by chlorination reaction is subject to multistage condensation by a main reaction kettle, a condenser, an auxiliary reaction kettle and the like, and is firstly washed by a washing tank and then absorbed by a 2-stage hydrochloric acid falling film absorption tower, wherein impurities such as carried acyl chloride, dichlorodithio, acetic acid and the like are fully washed and absorbed. The tail gas is fully washed in the water washing process, impurities are not brought into the hydrochloric acid of the byproduct, and the washing liquid returns to the chlorination kettle to serve as the raw material, so that the consumption of the raw material is reduced, and the quality of the hydrochloric acid of the byproduct is improved.
The prior chloroacetic acid production process has the following problems: the consumption of acetic acid is high. No chlorination liquid is used for catalytic hydrogenation, so that the consumption of acetic acid is too high. Continuous production is not possible.
Disclosure of Invention
The utility model aims at providing a simple structure had both shortened reaction time, vacated reaction space again, chlorination reaction unit of continuous cycle method production that can continuous production, high-efficient operation.
A chlorination reaction device produced by a continuous circulation method comprises a circulating pump, wherein chlorine and chlorination liquid in the circulating pump enter a primary reactor, the output end of the primary reactor is connected with the input end of a separator, the first output end of the separator is connected with the input end of a secondary reactor, the output end of the secondary reactor is connected with the input end of a primary condenser, the output end of the primary condenser is connected with the input end of a secondary condenser, and the output end of the secondary condenser is connected with the input end of a demister; a first output end of the plate heat exchanger provided with a cooling water inlet is connected with an input end of the hot water tank, a second output end of the plate heat exchanger is connected with the secondary reactor, and a third output end of the plate heat exchanger is connected with the primary reactor; the output end of the hot water tank is connected with the first-stage reactor through a hot water pump.
The utility model discloses a continuous circulation method carries out chlorination, makes the gas-liquid fully contact, increases its dwell time, adopts large-traffic chlorination liquid circulation, one-level reaction and second grade reaction system, and the temperature of simultaneous control reaction process and the dispersion and the mixture of reinforcing gas-liquid contact control degree of depth chlorination's emergence, the formation of dichloride and trichloride promptly.
The utility model discloses a continuous circulation method chloridizes, reacts chlorination liquid and chlorine and flows into chlorination reactor according to certain ratio promptly, and the stable control reaction section temperature makes the reaction heat ration emit, and the product that the reaction generated simultaneously also ration flows, has both shortened reaction time, vacates reaction space again, and production can be in succession, high-efficient operation. The utility model discloses can use the tail chlorine after the chlorine liquefaction to not influence product quality as raw materials chlorine.
Has the advantages that:
1. As can be seen from the mechanism of chlorination reaction, the reaction temperature, the degree of mixing of the reaction materials, the depth of chlorination, the amount of catalyst and the promoter are the main factors affecting the formation of dichloride in the production process. For the formation that reduces the dichloride, improve product quality simultaneously, the utility model discloses a second grade reaction, the reaction is complete, makes effective substance such as catalyst can't escape, obtains make full use of, reduces the consumption, practices thrift the cost.
2. The utility model discloses a large-traffic chlorination liquid circulation reaction, chlorination liquid and chlorine mol ratio 6 ~ 12: 1, control reaction rate that can be fine, chlorine can 100% reaction, and tail gas does not contain free chlorine, gets rid of alkali and absorbs free chlorine process, reduce cost.
3. the utility model discloses a chlorination liquid macrocycle, the tail gas chlorine after the available liquefaction of reaction chlorine solves the tail gas treatment difficulty problem of enterprise.
4. The utility model discloses a chlorination liquid macrocycle can the effective control chlorination reaction degree of depth, guarantees dichloride content below 0.3%, can get rid of high pressure hydrogenation process on the later process finished product processing technology, shortens process flow, and safety in production is secure, and equipment investment significantly reduces.
5. The reactor of the utility model adopts a tower-type high-efficiency reactor, firstly, the specific surface area of the filler is very large, the gas-liquid contact is very sufficient, and the reaction is complete. Secondly, the structure of the tower eliminates the wall flow phenomenon, increases the effective reaction and improves the reaction rate. The jacket is circulated by hot water, so that the reaction temperature can be stably controlled, the reaction rate and the chlorination depth can be effectively controlled, and the generation of dichlorotrichloro can be restrained.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Figure 2 is a schematic diagram of the results of the reactor of the present invention.
Detailed Description
The technical scheme of the utility model is explained in detail with the attached drawings as follows:
As shown in fig. 1, a chlorination reaction device for continuous production comprises a circulating pump 1, wherein chlorine and a chlorination solution in the circulating pump 1 enter a primary reactor 2, an output end of the primary reactor 2 is connected with an input end of a separator 3, a first output end 31 of the separator 3 is connected with an input end of a secondary reactor 4, an output end of the secondary reactor 4 is connected with an input end of a primary condenser 5, an output end of the primary condenser 5 is connected with an input end of a secondary condenser 6, and an output end of the secondary condenser 6 is connected with an input end of a demister 10; a first output end of the plate type heat exchanger 9 provided with the cooling water inlet 91 is connected with an input end of the hot water tank 7, a second output end of the plate type heat exchanger 9 is connected with the secondary reactor 4, and a third output end of the plate type heat exchanger 9 is connected with the primary reactor 2; the output end of the hot water tank 7 is connected with the primary reactor 2 through a hot water pump 8.
As shown in fig. 2, the first-stage reactor 2 and the second-stage reactor 4 of the present invention comprise a plurality of groups of packed towers, each group of packed towers is provided with a gas inlet 221, an exhaust port 228, and a material inlet 223 for introducing a chlorinated liquid, the mixed liquid outlet 222 is located at the upper end of the reactor, and the upper end of the reactor is provided with a temperature measuring port 224; a cold water inlet 225 and a hot water outlet 226 are respectively arranged on the side wall of the reactor; a drain 227 is provided in the side wall of the reactor adjacent the feed inlet 223.
As shown in fig. 1, the hot water tank 7 of the present invention is provided with a steam inlet 71 for introducing steam.
as shown in fig. 1, the hot water tank 7 of the present invention is provided with a cooling water inlet for introducing cooling water.
As shown in fig. 1, the second-stage reactor 4 of the present invention is provided with a raw material liquid inlet 41 for introducing a raw material liquid.
as shown in fig. 1, the second-stage reactor 4 of the present invention is provided with a second-stage reaction cooling water outlet 42 for discharging cooling water.
as shown in FIG. 1, a catalyst inlet 43 for introducing a catalyst is provided in the secondary reactor 4 of the present invention.
As shown in fig. 1, a freezing water inlet 51 for introducing 0 degree freezing water is arranged on the primary condenser 5; the primary condenser 5 is provided with a primary water return port 52 for primary refrigeration return water.
As shown in fig. 1, the second-stage condenser 6 of the present invention is provided with a chilled water inlet 61 for introducing chilled water of-15 degrees; the secondary condenser 6 is provided with a secondary water return port 62 for secondary refrigeration return water.
The utility model discloses a chlorine and a large amount of chlorination liquid that circulating pump 1 comes then get into separator 3 after carrying out chlorination reaction in getting into primary reactor 2, and the mixed liquid in separator 3 is by steam heating at the initial stage of driving, reaches reaction temperature after, and the temperature in the separator is controlled by the quantity of automatic valve automatically regulated steam, guarantees the reaction temperature that needs in the primary reactor 2. The heat generated by the reaction in the first-stage reactor 2 is removed from the jacket by hot water sent by a hot water pump 8, the reaction temperature is controlled by the hot water, when the content of the chlorination liquid reaches about 80 percent and the content of dichloro is 0.3 percent, the reaction reaches the equilibrium, and the continuous production is started. The hydrogen chloride and the entrained active components in the separator 3 enter the secondary reactor 4, and are in countercurrent contact with the raw materials from the top of the secondary reactor 4 and the catalyst (if the catalyst is needed) from the middle of the secondary reactor and react, trace unreacted chlorine gas entrained in the mixed gas can continue to react and is cooled by the primary condenser 5 and the secondary condenser 6, the entrained intermediate active products and the unreacted light components are intercepted, and the tail gas hydrogen chloride is further recycled by the demister 10, the intermediate active products and the unreacted light components are purified and then goes to the next process. The recovered light components and active substances generated by the reaction are added to the lower part of the primary reactor 2 through the circulating pump 1 to continuously participate in the reaction, so that the consumption of raw materials is reduced. Fresh feed and catalyst are metered into the secondary reactor 4. Pumping the chlorination liquid in the separator 3 to a rectifying device, recovering the raw materials and active substances generated by reaction, and packaging the finished product.
1. The reaction temperature is reduced, and the selectivity of the reaction is improved:
Because the reaction temperature directly influences the selectivity of chlorine atom substitution in the chlorination reaction, the reaction temperature is high, and the occurrence probability of side reactions is increased. By examining the activation energy of main and side chlorination reactions, the activation energy of the chlorination reaction to generate dichloride is higher than that of chlorination to generate monochloride, the generation rate of monochloride is higher than that of dichloride at the same temperature, and if the reaction temperature is increased, the reaction rate of generating dichloride is increased, and the reaction selectivity is reduced. But the reaction speed is very slow in the chlorination process due to low temperature. The reaction temperature can be strictly controlled in the continuous circulation chlorination process and does not exceed +/-1 ℃ of the set temperature.
2. The reaction process is strengthened, and the reaction speed is accelerated:
For most gas-liquid two-phase reactions, the reaction rate is generally dependent on the overall mass transfer to the process control. In the continuous circulation method chlorination process, gas and liquid in the novel efficient main reactor can generate a huge and fast-updated phase interface, so that the mass transfer rate between phases is increased by 1-3 orders of magnitude compared with that in the traditional tower, and is ten times or even hundreds times higher than that in a stirring kettle. The mixing and mass transfer processes of the reaction liquid are greatly enhanced. Namely, the dispersibility between gas and liquid is good, and the reaction speed can be accelerated.
3. The chlorination depth is controlled, and the side reaction is reduced:
the chlorination depth is high, the utilization rate of raw materials is high, but polychloride is easy to generate. The selectivity of the monochloride decreases, which affects the quality and yield of the product. Therefore, it is very important to select an appropriate chlorination depth. The proportion of the raw material and the chlorine is related to the chlorination depth, namely the weight ratio of the raw material and the chlorine participating in the reaction is larger under the condition of uniform dispersion of gas phase and liquid phase, namely the raw material liquid is greatly excessive, the selectivity of monochloro is improved, and the generation amount of dichloride is lower. Conversely, the selectivity of the monochloride decreases and more dichloride is produced. Because the method is a circulating reaction, namely the circulating amount of the circulating chlorination liquid is particularly large, the absolute weight of the raw materials in the chlorination liquid is also large, and the side reaction can be reduced. Adjusting the mol ratio of chlorination liquid to chlorine gas to be 6-12 in the continuous circulation chlorination process: 1, reacting the chlorine gas by using a large amount of circulating chlorination liquid. The method can effectively control the content of the dichloride to be less than 0.3 percent when the content of the monochloride in the chlorination solution is about 80 percent, no trichloride is generated, and because a large amount of chlorination solution circulates, the raw material amount is greatly excessive, so that the chlorine can be completely reacted, and free chlorine does not exist in the chlorination solution.
4. The loss of the catalyst is reduced, and the production cost is reduced:
The utility model discloses a two-stage reactor, carry out gas-liquid separation with the chlorination liquid after the first-stage reactor reaction, raw material liquid is smugglied secretly to hydrogen chloride and the complete chlorine of unreacted, the middle active material that the reaction produced gets into second-stage reactor bottom, the catalyst that comes with the top and middle part contacts the reaction in the second-stage reactor against the current and produces middle active material, the temperature drops to below 35 degrees after the cooler cooling, be far below the boiling point of these materials and held back, and increased the droplet that precision catcher will probably smuggle behind the cooler again and held back, the droplet more than the precision filter can 100% entrapment 1u, most raw materials and catalyst and useful middle active material have been retrieved, greatly reduced the cost.
5. Adopts a novel high-efficiency reactor:
The first-stage reactor and the second-stage reactor of the utility model adopt a gas-liquid two-phase reactor. The gas-liquid two-phase reactor is characterized in that: the chlorination reaction tower is composed of a plurality of small tower-passing packed towers, the packing with large specific surface area is adopted, the wall flow phenomenon of the common packed tower is eliminated, the gas-liquid distribution is uniform, the collision probability of the gas-liquid two phases is greatly increased, the retention time of the gas phase is increased, and the reaction efficiency is improved. The reaction tower is additionally provided with a jacket structure, the reaction temperature can be automatically and accurately controlled by hot water in the jacket of the reactor, the side reaction can be inhibited, and the defects that the temperature difference between cooling water and chlorination liquid is too large and the reaction temperature is difficult to control by directly using the cooling water are avoided by hot water circulation. In the whole production process, because the content of dichloride is very low, a hydrogenation process is removed without using a high-temperature high-pressure hydrogenation tower, the investment of a noble metal palladium catalyst is saved, the process flow is shortened, the equipment investment is greatly reduced, and the operation cost, the process operability and the safety of a device are greatly improved.
Claims (9)
1. A chlorination reaction device produced by a continuous circulation method is characterized by comprising a circulating pump (1), chlorine and chlorination liquid in the circulating pump (1) enter a primary reactor (2), the output end of the primary reactor (2) is connected with the input end of a separator (3), a first output end (31) of the separator (3) is connected with the input end of a secondary reactor (4), the output end of the secondary reactor (4) is connected with the input end of a primary condenser (5), the output end of the primary condenser (5) is connected with the input end of a secondary condenser (6), and the output end of the secondary condenser (6) is connected with the input end of a demister (10); a first output end of a plate type heat exchanger (9) provided with a cooling water inlet (91) is connected with an input end of a hot water tank (7), a second output end of the plate type heat exchanger (9) is connected with a secondary reactor (4), and a third output end of the plate type heat exchanger (9) is connected with a primary reactor (2); the output end of the hot water tank (7) is connected with the primary reactor (2) through a hot water pump (8).
2. The chlorination reaction device produced by the continuous circulation method according to claim 1, wherein the first-stage reactor (2) and the second-stage reactor (4) comprise a plurality of groups of packed towers, each group of packed towers is respectively provided with a gas inlet (221) and an exhaust port (228), a material inlet (223) for introducing chlorination liquid is also arranged, a mixed liquid outlet (222) is positioned at the upper end of the reactor, and the upper end of the reactor is provided with a temperature measuring port (224); a cold water inlet (225) and a hot water outlet (226) are respectively arranged on the side wall of the reactor; a drain hole (227) is arranged on the side wall of the reactor near the material inlet (223).
3. The chlorination reactor apparatus according to claim 1, wherein the hot water tank (7) is provided with a steam inlet (71) for introducing steam.
4. The chlorination reactor apparatus according to claim 1, wherein the hot water tank (7) is provided with a cooling water inlet for introducing cooling water.
5. The chlorination reactor apparatus according to claim 1, wherein the secondary reactor (4) is provided with a raw material liquid inlet (41) for introducing a raw material liquid.
6. The chlorination reactor apparatus according to claim 1, wherein the secondary reactor (4) is provided with a secondary reaction cooling water outlet (42) for discharging cooling water.
7. The continuous circulation chlorination reactor according to claim 1, wherein the secondary reactor (4) is provided with a catalyst inlet (43) for introducing a catalyst.
8. the chlorination reactor apparatus according to claim 1, wherein the first condenser (5) is provided with a freezing and watering inlet (51) for introducing freezing and watering at 0 degree; the primary condenser (5) is provided with a primary water return port (52) for primary refrigeration backwater.
9. The chlorination reactor apparatus produced by the continuous circulation method according to claim 1, wherein the secondary condenser (6) is provided with a chilled water inlet (61) for introducing chilled water of-15 degrees; a secondary water return port (62) for secondary refrigeration return water is arranged on the secondary condenser (6).
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| CN201920405600.4U CN209791506U (en) | 2019-03-28 | 2019-03-28 | chlorination reaction device for continuous circulation production |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109806816A (en) * | 2019-03-28 | 2019-05-28 | 南京嘉源润新环保科技有限公司 | A kind of chlorination reaction device of continuous round-robin method production |
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2019
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109806816A (en) * | 2019-03-28 | 2019-05-28 | 南京嘉源润新环保科技有限公司 | A kind of chlorination reaction device of continuous round-robin method production |
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