CN114681944B - Forced condensing system and method for reducing consumption of chloroacetic acid in production of methyl chloroacetate - Google Patents
Forced condensing system and method for reducing consumption of chloroacetic acid in production of methyl chloroacetate Download PDFInfo
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- CN114681944B CN114681944B CN202210063232.6A CN202210063232A CN114681944B CN 114681944 B CN114681944 B CN 114681944B CN 202210063232 A CN202210063232 A CN 202210063232A CN 114681944 B CN114681944 B CN 114681944B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D5/0033—Other features
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- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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Abstract
The invention relates to the technical field of forced condensation of fine organic chemistry, in particular to a forced condensation system and a method for reducing chloroacetic acid consumption in the production of methyl chloroacetate, comprising a first-stage diversion condenser arranged at the outlet end of a distillation gas-phase pipe, wherein the inlet end of the distillation gas-phase pipe is connected with a reaction kettle in the methyl chloroacetate production system, azeotrope formed by materials such as ester, water, alcohol and acid is arranged in the reaction kettle, a second-stage diversion condenser is connected at the downstream of the first-stage diversion condenser, a third-stage diversion condenser is connected at the downstream of the second-stage diversion condenser, and monochloroacetic acid reflux mechanisms are arranged at the bottoms of the first-stage diversion condenser, the second-stage diversion condenser and the third-stage diversion condenser. The whole system can be effectively matched with various existing methyl chloroacetate production systems, can be directly matched for use without greatly improving the methyl chloroacetate production system, and has strong overall universality and high installation flexibility.
Description
Technical Field
The invention relates to the technical field of forced condensation of fine organic chemistry, in particular to a forced condensation system and a method which can be applied to a traditional methyl chloroacetate production workshop with low cost and smoothness for improving the production quality of methyl chloroacetate, and particularly can reduce the consumption of chloroacetic acid in the production of methyl chloroacetate.
Background
When methyl chloroacetate is produced in a traditional workshop and esterified, raw materials such as methanol, chloroacetic acid and the like are added, and materials such as ester, water, alcohol, acid and the like in a reaction kettle can form an azeotropic phenomenon in the distillation process.
For example, in patent application No.: CN201410342356.3, patent name: the method for preparing methyl chloroacetate comprises the following specific contents: the method is characterized by taking chloroacetic acid and methanol as raw materials and acid resin as a catalyst for gas, liquid and solid three-phase reaction, and is characterized in that: the modified acid resin is used as a catalyst, and can be completed by adopting a one-stage fixed bed reactor, and the process does not need to add a water carrying agent, and comprises the following steps: (1) uniformly mixing chloroacetic acid and methanol according to a certain proportion; (2) A fixed bed reactor, the amount of packed catalyst is 2/3 of the volume of the reactor; (3) Controlling the reaction temperature to be 80-120 ℃ and the space velocity to be 0.5-2g of raw material/catalyst; (4) continuously feeding by adopting a feeding pump; (5) The gas phase reaction product exits … … at the top of the reactor and the product is collected.
The above patent discloses a method for producing methyl chloroacetate by gas, liquid and solid three-phase reaction using chloroacetic acid and methanol as raw materials and acidic resin as catalyst.
In addition, by combining the description in the prior art and long-term experience accumulation of production workers in a processing workshop of our company, the fact that 1 ton of methyl chloroacetate is produced by using the traditional process approximately needs to consume 1.05 tons of chloroacetic acid and 0.1 ton of sodium carbonate when in production is found, and the time for producing single batch materials is reduced by approximately 42-45 hours; in addition, the traditional processing technology and system have the problem of excessive consumption of chloroacetic acid when methyl chloroacetate is produced, which not only results in huge consumption of chloroacetic acid, but also influences the product yield of the whole production process and the time consumption of product production.
Excessive consumption of chloroacetic acid in the traditional production process also causes excessive acidity of the product, influences the quality of the product, and excessive consumption of the chloroacetic acid affects the cost of the product, so that excessive waste of raw materials in the traditional process and equipment for producing methyl chloroacetate is caused, and the defect of market competitiveness is overcome.
Although the conventional workshops have the problems, because the production process and the production equipment of methyl chloroacetate in the original workshops are mature technologies, excessive changes not only can cause the workshops to run abnormally, but also can cause the construction cost to be too high.
Therefore, it is of great importance to the prior art how to achieve a lower cost for methyl chloroacetate production, lower chloroacetic acid consumption, and improved product quality and yield.
Therefore, the invention creatively designs a forced condensing system which can be applied to a traditional methyl chloroacetate production workshop with low cost and smoothness and can improve the production quality of the methyl chloroacetate, so as to better solve the problems in the prior art.
Disclosure of Invention
The invention aims to solve one of the technical problems, and adopts the following technical scheme: the forced condensing system for reducing chloroacetic acid consumption in the production of methyl chloroacetate is installed in the production system of methyl chloroacetate and used, and comprises a first-stage diversion condenser installed at the outlet end of a distillation gas-phase pipe, wherein the inlet end of the distillation gas-phase pipe is connected with a reaction kettle in the production system of methyl chloroacetate, an azeotrope formed by materials such as ester, water, alcohol and acid is installed in the reaction kettle, the downstream of the first-stage diversion condenser is connected with a second-stage diversion condenser, the downstream of the second-stage diversion condenser is connected with a third-stage diversion condenser, a main heat insulation structure is installed between the first-stage diversion condenser and the second-stage diversion condenser and between the second-stage diversion condenser and the third-stage diversion condenser, the first-stage diversion condenser, the second-stage diversion condenser and the third-stage diversion condenser are all only used for forcibly condensing chloroacetic acid in the azeotrope, and the bottoms of the first-stage diversion condensers, the second-stage diversion condenser and the third-stage diversion condenser are all installed with an acid reflux mechanism, and the chloroacetic acid reflux mechanisms are respectively used for carrying back flow to the upper part of the chloroacetic acid kettle for recycling after being pressed.
In any of the above schemes, preferably, the main heat insulation structure comprises a heat insulation pipe support, a heat insulation cavity is arranged in the center of the heat insulation pipe support in a penetrating manner, an annular clamping cavity is respectively arranged at the top and the bottom of the heat insulation pipe support at the periphery of the heat insulation cavity, a heat insulation layer is arranged between the two annular clamping cavities, and the two annular clamping cavities on the same heat insulation pipe support are used for sealing and sleeving the flow guide condensers at the corresponding end parts.
In any of the above aspects, preferably, a seal ring is disposed in each of the annular clamping cavities.
In any of the above schemes, preferably, the first-stage diversion condenser comprises a forced cooling pipe, the forced cooling pipe comprises a U-shaped pipe section in the middle, two end tops of the U-shaped pipe section are respectively connected with an elbow reversing section in an integrated manner, the upstream elbow reversing section is connected with the outlet end of the distillation gas-phase pipe, the downstream elbow reversing section is connected with the inlet end of the second-stage diversion condenser, the forced cooling pipe comprises a diversion inner pipe and a condensation outer pipe, the diversion inner pipe and the condensation outer pipe are relatively fixedly connected through a plurality of heat conducting rings, a plurality of diversion holes are formed on the surface of each heat conducting ring, an annular condensation channel through which condensate flows is formed between the diversion inner pipe and the condensation outer pipe, circulating power is provided for the coolant by an external circulating conveying pump, and the temperature of the coolant is lower than the boiling point temperature of chloroacetic acid and higher than the temperature of other azeotropes.
In any of the above schemes, it is preferable that a heat-insulating electric heating sleeve is sleeved on the periphery of the condensation outer tube, and the heat-insulating electric heating sleeve is connected with an external power supply through a wire.
In any of the above schemes, preferably, the heat-preserving electric heating sleeve is further provided with a heat-preserving controller, a plurality of waterproof temperature sensors are installed on the side wall of the annular condensing channel along the flowing direction of the cooling liquid, and each waterproof temperature sensor is in signal connection with the heat-preserving controller.
In any of the above schemes, preferably, the structures of the secondary diversion condenser and the tertiary diversion condenser are the same as those of the primary diversion condenser.
In any of the above schemes, it is preferable that a circulating liquid inlet control pipe communicated with an annular condensing channel inside the primary diversion condenser is connected to a water inlet end of a condensing outer pipe of the primary diversion condenser, a circulating liquid outlet control pipe communicated with the annular condensing channel inside the tertiary diversion condenser is connected to a water outlet end of the condensing outer pipe of the tertiary diversion condenser, the circulating liquid inlet control pipe and the circulating liquid outlet control pipe are respectively connected with a circulating heating container through circulating pipelines, and circulating conveying pumps are installed on the circulating pipelines.
In any of the above solutions, preferably, a spiral internal thread diversion trench is disposed on a side wall of an inner cavity of the U-shaped pipe section of each diversion inner pipe.
In any of the above schemes, preferably, the chloroacetic acid reflux mechanism comprises a reflux pipe installed at the bottom of the U-shaped pipe section of the condensing outer pipe, the tail end of the reflux pipe is connected back to the feed inlet of the reaction kettle, and the upper end and the tail end of the reflux pipe are both provided with a liquid inlet one-way control valve and a liquid outlet one-way control valve.
In any of the above schemes, preferably, a side-through pressurizing pipe is communicated with one side of the upper part of the return pipe, a plunger pressurizing pump is installed at the outer end of the upper part of the side-through pressurizing pipe, a piston end of the plunger pressurizing pump movably seals and stretches into an inner cavity of the side-through pressurizing pipe, and the plunger pressurizing pump controls chloroacetic acid condensed in the return pipe to realize pressurized liquid outlet through expansion and contraction.
The invention also provides a forced condensing method for reducing chloroacetic acid consumption in the production of methyl chloroacetate by using the forced condensing system for reducing chloroacetic acid consumption, which comprises the following steps:
s1: installing the forced condensing system for reducing chloroacetic acid consumption into a methyl chloroacetate production system;
the inlet end of the forced condensing system for reducing the consumption of the chloroacetic acid is connected with the outlet end of a distillation gas phase pipe of the methyl chloroacetate production system, and the outlet ends of all chloroacetic acid reflux mechanisms of the forced condensing system for reducing the consumption of the chloroacetic acid are respectively connected with the feed inlet of a reaction kettle of the methyl chloroacetate production system;
s2: preheating the discharging pipelines of the methyl chloroacetate production system and the forced condensing system for reducing the consumption of the chloroacetic acid, adding the reaction raw materials in proportion after the preheating reaches the requirement, and simultaneously starting equipment such as a reaction kettle of the methyl chloroacetate production system and the forced condensing system for reducing the consumption of the chloroacetic acid;
s3: controlling each reaction raw material to heat in the reaction kettle and form azeotrope formed by materials such as ester, water, alcohol, acid and the like, and fully reacting, wherein the azeotrope moves upwards in the reaction process and enters the first-stage diversion condenser of the forced condensation system for reducing chloroacetic acid consumption from the outlet end of the distillation gas phase pipe;
s4: the azeotrope is controlled to pass through the primary diversion condenser in sequence to realize primary condensation, the circulating heating container is controlled to continuously convey cooling liquid with the temperature lower than the boiling point temperature of chloroacetic acid and higher than the boiling point temperature of the rest azeotrope into the annular condensation channel, preferably the temperature of the cooling liquid is 95-100 ℃, and the cooling liquid realizes primary forced condensation liquefaction of chloroacetic acid in the primary diversion condenser;
in the process of introducing cooling liquid, a waterproof temperature sensor is used for monitoring the temperature of the cooling liquid in real time and keeping the temperature within a set temperature range, an electric heating sleeve is used for realizing electric heating and temperature rising of the cooling liquid with lower temperature, and meanwhile, a heat preservation controller is used for controlling the heating degree;
s5: the azeotrope is cooled by the first-stage diversion condenser and then continuously flows downwards, and the chloroacetic acid is subjected to second-stage forced condensation liquefaction and third-stage forced condensation liquefaction by the second-stage diversion condenser and the third-stage diversion condenser, so that the chloroacetic acid content in the azeotrope is reduced;
s6: the chloroacetic acid condensate condensed and liquefied in each level of diversion condenser is accumulated in the chloroacetic acid reflux mechanisms, the liquid inlet one-way control valve of each chloroacetic acid reflux mechanism is controlled to be opened, so that the chloroacetic acid condensate enters the reflux pipe, then the plunger pressurizing pump is controlled to work to pressurize the chloroacetic acid condensate in the reflux pipe, and the liquid outlet one-way control valve is opened, so that the chloroacetic acid condensate is refluxed into the reaction kettle;
s7: after the reflux is finished, the chloroacetic acid condensate flows back into the reaction kettle to continue the reaction;
s8: thus, the multistage repeated condensation reflux and the repeated utilization of the chloroacetic acid in the reaction process are realized reciprocally, and the full utilization of the chloroacetic acid is ensured.
Compared with the prior art, the invention has the following beneficial effects:
1. the whole system can be effectively matched with various existing methyl chloroacetate production systems, can be directly matched for use without greatly improving the methyl chloroacetate production system, and has strong overall universality and high installation flexibility.
2. The system utilizes the first-stage diversion condenser, the second-stage diversion condenser and the third-stage diversion condenser to realize multistage condensation of chloroacetic acid on the reacted azeotrope gas, ensures that only chloroacetic acid is liquefied and other azeotropes are not liquefied, and can effectively ensure full recycling of chloroacetic acid.
3. Only liquefy chloroacetic acid and not liquefy other azeotrope when the system condenses, can guarantee the abundant recycle of chloroacetic acid effectively, and each chloroacetic acid reflux mechanism of direct utilization can realize effectively retrieving chloroacetic acid condensate to the reation kettle in the time of retrieving and collect, guarantees reuse, the abundant reaction of chloroacetic acid, reduces the waste of chloroacetic acid in the whole reaction effectively, has reduced product cost, has improved market competition.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. Like elements or features are generally identified by like reference numerals throughout the drawings. In the drawings, the elements or components are not necessarily drawn to scale.
Fig. 1 is a schematic view of the installation state structure of the present invention.
Fig. 2 is a schematic view of the internal cross-sectional structure of the present invention.
In the figure, 1, a distillation gas phase pipe; 2. a primary flow directing condenser; 3. a reaction kettle; 4. a primary insulation structure; 401. a heat insulation pipe support; 402. a heat insulating chamber; 403. an annular clamping cavity; 404. a seal ring; 5. chloroacetic acid reflux mechanism; 501. a return pipe; 502. a liquid inlet one-way control valve; 503. a liquid outlet one-way control valve; 504. a pressurizing pipe is laterally communicated; 505. a plunger pressurizing pump; 6. a forced cooling pipe; 601. a diversion inner tube; 602. condensing the outer tube; 603. a heat conducting ring; 604 a deflector hole; 605. an annular condensing passage; 607. a thermal insulation controller; 608. a waterproof temperature sensor; 7. a U-shaped pipe section; 8. a bent pipe reversing section; 9. a circulating liquid inlet control pipe; 10. a circulating liquid outlet control pipe; 11. a circulation line; 12. a cyclic heating container; 13. a circulating delivery pump; 14. a secondary flow-guiding condenser; 15. three-stage flow guiding condenser.
Detailed Description
Embodiments of the technical scheme of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for more clearly illustrating the technical aspects of the present invention, and thus are merely examples, and are not intended to limit the scope of the present invention. The specific structure of the invention is shown in figures 1-2.
Example 1:
the forced condensing system for reducing chloroacetic acid consumption in the production of methyl chloroacetate is installed in the production system of methyl chloroacetate and used, and comprises a first-stage diversion condenser 2 installed at the outlet end of a distillation gas phase pipe 1, the inlet end of the distillation gas phase pipe is connected with a reaction kettle 3 in the production system of methyl chloroacetate, azeotrope formed by materials such as ester, water, alcohol and acid is installed in the reaction kettle 3, a second-stage diversion condenser 14 is connected to the downstream of the first-stage diversion condenser 2, a third-stage diversion condenser 15 is connected to the downstream of the second-stage diversion condenser 14, a main heat insulation structure 4 is installed between the first-stage diversion condenser 2 and the second-stage diversion condenser 14 and between the second-stage diversion condenser 14 and the third-stage diversion condenser 15, the first-stage diversion condenser 2, the second-stage diversion condenser 14 and the third-stage diversion condenser 15 are all only used for forcibly condensing chloroacetic acid in the azeotrope, and a reflux mechanism 5 is installed at the bottom of each first-stage diversion condenser 2, the second-stage diversion condenser 14 and the third-stage diversion condenser 15 and a reflux mechanism 5 is installed at the bottom of each first-stage diversion condenser 15 for conveying chloroacetic acid to the first-stage reflux mechanism for the reflux of the chloroacetic acid to the reaction kettle.
The whole system can be effectively matched with various existing methyl chloroacetate production systems, can be directly matched for use without greatly improving the methyl chloroacetate production system, and has strong overall universality and high installation flexibility.
After the installation is finished, the system can be well matched with the prior chloroacetic acid methyl ester production system to be used, the chloroacetic acid methyl ester production system is started, the first-stage diversion condenser 2, the second-stage diversion condenser 14 and the third-stage diversion condenser 15 can be directly utilized to realize multistage condensation chloroacetic acid on the reacted azeotrope gas, so that the chloroacetic acid is only liquefied and other azeotropes are not liquefied, the full recycling of the chloroacetic acid can be effectively ensured, the chloroacetic acid condensate can be effectively recycled into the reaction kettle 3 to be collected by directly utilizing each chloroacetic acid reflux mechanism 5 during recycling, the repeated utilization and full reaction of the chloroacetic acid are ensured, and the waste of the chloroacetic acid in the whole reaction is effectively reduced.
In any of the above schemes, preferably, the main heat insulation structure 4 includes a heat insulation pipe support 401, a heat insulation cavity 402 is provided in the center of the heat insulation pipe support 401, an annular clamping cavity 403 is provided at the top and bottom of the heat insulation pipe support 401 at the periphery of the heat insulation cavity 402, a separation layer is provided between the two annular clamping cavities 403, and two annular clamping cavities 403 on the same heat insulation pipe support 401 are used for sealing and clamping and sleeving on the diversion condenser at the corresponding end.
The main roles of the insulating tube rest 401 are 2: one is to connect the strong cooling pipe 6 of the adjacent diversion condenser and ensure the communication of the inner cavity of the adjacent diversion inner pipe 601 and the communication of the adjacent annular condensing channel 605; and secondly, the heat insulation and sealing functions are achieved.
In any of the above embodiments, it is preferable that a seal 404 is provided in each of the annular locking cavities 403.
The sealing ring 404 is additionally arranged to better ensure the tightness after connection and prevent the problem of leakage of air and liquid.
In any of the above schemes, preferably, the primary diversion condenser 2 includes a strong cooling pipe 6, the strong cooling pipe 6 includes a U-shaped pipe section 7 in the middle, two end tops of the U-shaped pipe section 7 are respectively connected with an elbow reversing section 8 in an integrated manner, the upstream elbow reversing section 8 is connected with an outlet end of the distillation gas phase pipe 1, the downstream elbow reversing section 8 is connected with an inlet end of the secondary diversion condenser 14, the strong cooling pipe 6 includes a diversion inner pipe 601 and a condensation outer pipe 602, the diversion inner pipe 601 and the condensation outer pipe 602 are relatively fixedly connected through a plurality of heat conducting rings 603, a plurality of diversion holes 604 are formed on surfaces of the heat conducting rings 603, an annular condensation channel 605 through which condensate flows is formed between the diversion inner pipe 601 and the condensation outer pipe 602, a cooling liquid capable of circulating is introduced into the annular condensation channel 605, the cooling liquid is provided with circulating power by an external circulating conveying pump 13, and the temperature of the cooling liquid is lower than the boiling point temperature of chloroacetic acid and higher than the boiling point temperature of the rest azeotropy.
In any of the above embodiments, the structures of the secondary diversion condenser 14 and the tertiary diversion condenser 15 are preferably the same as the structure of the primary diversion condenser 2.
The first-stage diversion condenser 2, the second-stage diversion condenser 14 and the third-stage diversion condenser 15 have the same structure and function and mainly play a role in multi-stage condensation; when the azeotrope enters the strong cooling pipe 6 and flows through the central diversion inner pipe 601, and cooling liquid with the temperature of 95-100 ℃ is introduced into the annular condensation channel 605 at the periphery of the diversion inner pipe 601, the azeotrope can be relatively cooled, and after cooling, only chloroacetic acid is in a liquefied state because the boiling point of ester, water, alcohol and the like in the azeotrope is lower than the temperature, and of course, a very small amount of other azeotropes can be allowed to be liquefied, and the condensate of the general monochloroacetic acid is mainly.
The condensed chloroacetic acid enters the corresponding chloroacetic acid reflux mechanism 5 for temporary storage, unreacted azeotrope is continuously conveyed downstream to finish re-condensation, and the chloroacetic acid in the azeotrope can be effectively removed basically through multistage condensation.
In any of the above solutions, it is preferable that a circulating inlet control pipe 9 connected to an annular condensing channel 605 inside the condensation outer pipe 602 of the primary diversion condenser 2 is connected to an inlet end of the condensation outer pipe 602 of the tertiary diversion condenser 15, a circulating outlet control pipe 10 connected to an annular condensing channel 605 inside the condensation outer pipe 602 is connected to an outlet end of the condensation outer pipe 602 of the tertiary diversion condenser 15, and the circulating inlet control pipe 9 and the circulating outlet control pipe 10 are respectively connected to a circulating heating container 12 through circulating pipes 11, and circulating conveying pumps 13 are installed on the circulating pipes 11.
The circulation heating container 12 can provide continuous cooling liquid for the annular condensing channel 605, so as to ensure the rapid and effective condensation and recovery of the chloroacetic acid in the annular condensing channel, and the circulation conveying pump 13 can improve the conveying efficiency.
In any of the above embodiments, it is preferable that a spiral internal thread diversion trench is provided on the inner cavity side wall of the U-shaped pipe section 7 of each diversion inner pipe 601.
The spiral internal thread guiding gutter's effect has 2, and one is: the contact area between the azeotrope and the inner side wall of the diversion inner pipe 601 can be properly increased; and the second is: the length of the travelling path of the azeotrope in the diversion inner pipe 601 can be effectively prolonged, and the condensation effect is increased.
Example 2:
the forced condensing system for reducing chloroacetic acid consumption in the production of methyl chloroacetate is installed in the production system of methyl chloroacetate and used, and comprises a first-stage diversion condenser 2 installed at the outlet end of a distillation gas phase pipe 1, the inlet end of the distillation gas phase pipe is connected with a reaction kettle 3 in the production system of methyl chloroacetate, azeotrope formed by materials such as ester, water, alcohol and acid is installed in the reaction kettle 3, a second-stage diversion condenser 14 is connected to the downstream of the first-stage diversion condenser 2, a third-stage diversion condenser 15 is connected to the downstream of the second-stage diversion condenser 14, a main heat insulation structure 4 is installed between the first-stage diversion condenser 2 and the second-stage diversion condenser 14 and between the second-stage diversion condenser 14 and the third-stage diversion condenser 15, the first-stage diversion condenser 2, the second-stage diversion condenser 14 and the third-stage diversion condenser 15 are all only used for forcibly condensing chloroacetic acid in the azeotrope, and a reflux mechanism 5 is installed at the bottom of each first-stage diversion condenser 2, the second-stage diversion condenser 14 and the third-stage diversion condenser 15 and a reflux mechanism 5 is installed at the bottom of each first-stage diversion condenser 15 for conveying chloroacetic acid to the first-stage reflux mechanism for the reflux of the chloroacetic acid to the reaction kettle.
The whole system can be effectively matched with various existing methyl chloroacetate production systems, can be directly matched for use without greatly improving the methyl chloroacetate production system, and has strong overall universality and high installation flexibility.
After the installation is finished, the system can be well matched with the prior chloroacetic acid methyl ester production system to be used, the chloroacetic acid methyl ester production system is started, the first-stage diversion condenser 2, the second-stage diversion condenser 14 and the third-stage diversion condenser 15 can be directly utilized to realize multistage condensation chloroacetic acid on the reacted azeotrope gas, so that the chloroacetic acid is only liquefied and other azeotropes are not liquefied, the full recycling of the chloroacetic acid can be effectively ensured, the chloroacetic acid condensate can be effectively recycled into the reaction kettle 3 to be collected by directly utilizing each chloroacetic acid reflux mechanism 5 during recycling, the repeated utilization and full reaction of the chloroacetic acid are ensured, and the waste of the chloroacetic acid in the whole reaction is effectively reduced.
In any of the above schemes, preferably, the main heat insulation structure 4 includes a heat insulation pipe support 401, a heat insulation cavity 402 is provided in the center of the heat insulation pipe support 401, an annular clamping cavity 403 is provided at the top and bottom of the heat insulation pipe support 401 at the periphery of the heat insulation cavity 402, a separation layer is provided between the two annular clamping cavities 403, and two annular clamping cavities 403 on the same heat insulation pipe support 401 are used for sealing and clamping and sleeving on the diversion condenser at the corresponding end.
The main roles of the insulating tube rest 401 are 2: one is to connect the strong cooling pipe 6 of the adjacent diversion condenser and ensure the communication of the inner cavity of the adjacent diversion inner pipe 601 and the communication of the adjacent annular condensing channel 605; and secondly, the heat insulation and sealing functions are achieved.
In any of the above embodiments, it is preferable that a seal 404 is provided in each of the annular locking cavities 403.
The sealing ring 404 is additionally arranged to better ensure the tightness after connection and prevent the problem of leakage of air and liquid.
In any of the above schemes, preferably, the primary diversion condenser 2 includes a strong cooling pipe 6, the strong cooling pipe 6 includes a U-shaped pipe section 7 in the middle, two end tops of the U-shaped pipe section 7 are respectively connected with an elbow reversing section 8 in an integrated manner, the upstream elbow reversing section 8 is connected with an outlet end of the distillation gas phase pipe 1, the downstream elbow reversing section 8 is connected with an inlet end of the secondary diversion condenser 14, the strong cooling pipe 6 includes a diversion inner pipe 601 and a condensation outer pipe 602, the diversion inner pipe 601 and the condensation outer pipe 602 are relatively fixedly connected through a plurality of heat conducting rings 603, a plurality of diversion holes 604 are formed on surfaces of the heat conducting rings 603, an annular condensation channel 605 through which condensate flows is formed between the diversion inner pipe 601 and the condensation outer pipe 602, a cooling liquid capable of circulating is introduced into the annular condensation channel 605, the cooling liquid is provided with circulating power by an external circulating conveying pump 13, and the temperature of the cooling liquid is lower than the boiling point temperature of chloroacetic acid and higher than the boiling point temperature of the rest azeotropy.
In any of the above embodiments, the structures of the secondary diversion condenser 14 and the tertiary diversion condenser 15 are preferably the same as the structure of the primary diversion condenser 2.
The first-stage diversion condenser 2, the second-stage diversion condenser 14 and the third-stage diversion condenser 15 have the same structure and function and mainly play a role in multi-stage condensation; when the azeotrope enters the strong cooling pipe 6 and flows through the central diversion inner pipe 601, and cooling liquid with the temperature of 95-100 ℃ is introduced into the annular condensation channel 605 at the periphery of the diversion inner pipe 601, the azeotrope can be relatively cooled, and after cooling, only chloroacetic acid is in a liquefied state because the boiling point of ester, water, alcohol and the like in the azeotrope is lower than the temperature, and of course, a very small amount of other azeotropes can be allowed to be liquefied, and the condensate of the general monochloroacetic acid is mainly.
The condensed chloroacetic acid enters the corresponding chloroacetic acid reflux mechanism 5 for temporary storage, unreacted azeotrope is continuously conveyed downstream to finish re-condensation, and the chloroacetic acid in the azeotrope can be effectively removed basically through multistage condensation.
In any of the above schemes, it is preferable that a thermal insulation electric heating sleeve is sleeved on the periphery of the condensation outer tube 602, and the thermal insulation electric heating sleeve is connected with an external power supply through a wire.
The main function of the insulating electric heating jacket is to heat the condensing outer tube 602, so as to ensure that the cooling liquid in the condensing outer tube 602 is kept within a required temperature range.
In any of the above solutions, preferably, the insulating electric heating jacket is further provided with an insulating controller 607, and a plurality of waterproof temperature sensors 608 are installed on the side wall of the annular condensing channel 605 along the flowing direction of the cooling liquid, and each waterproof temperature sensor 608 is in signal connection with the insulating controller 607.
The waterproof temperature sensor 608 can detect the temperature of the cooling liquid at the current position in real time and feed back the temperature according to actual conditions, so that the purposes of receiving signals by the heat preservation controller 607 and controlling the heat preservation electric heating sleeve to heat are achieved.
In any of the above solutions, it is preferable that a circulating inlet control pipe 9 connected to an annular condensing channel 605 inside the condensation outer pipe 602 of the primary diversion condenser 2 is connected to an inlet end of the condensation outer pipe 602 of the tertiary diversion condenser 15, a circulating outlet control pipe 10 connected to an annular condensing channel 605 inside the condensation outer pipe 602 is connected to an outlet end of the condensation outer pipe 602 of the tertiary diversion condenser 15, and the circulating inlet control pipe 9 and the circulating outlet control pipe 10 are respectively connected to a circulating heating container 12 through circulating pipes 11, and circulating conveying pumps 13 are installed on the circulating pipes 11.
The circulation heating container 12 can provide continuous cooling liquid for the annular condensing channel 605, so as to ensure the rapid and effective condensation and recovery of the chloroacetic acid in the annular condensing channel, and the circulation conveying pump 13 can improve the conveying efficiency.
In any of the above embodiments, it is preferable that a spiral internal thread diversion trench is provided on the inner cavity side wall of the U-shaped pipe section 7 of each diversion inner pipe 601.
The spiral internal thread guiding gutter's effect has 2, and one is: the contact area between the azeotrope and the inner side wall of the diversion inner pipe 601 can be properly increased; and the second is: the length of the travelling path of the azeotrope in the diversion inner pipe 601 can be effectively prolonged, and the condensation effect is increased.
In any of the above schemes, it is preferable that the chloroacetic acid reflux mechanism 5 includes a reflux pipe 501 installed at the bottom of the U-shaped pipe section 7 of the condensation outer pipe 602, the end of the reflux pipe 501 is connected back to the feed inlet of the reaction kettle 3, and a liquid inlet unidirectional control valve 502 and a liquid outlet unidirectional control valve 503 are installed at the upper end and the end of the reflux pipe 501.
The mutual coordination of the liquid inlet one-way control valve 502 and the liquid outlet one-way control valve 503 can effectively control the one-way mobility of chloroacetic acid.
In any of the above aspects, it is preferable that a side-through pressurizing pipe 504 is connected to one side of the upper portion of the return pipe 501, a plunger pressurizing pump 505 is mounted at an outer end of the upper portion of the side-through pressurizing pipe 504, a piston end of the plunger pressurizing pump 505 is movably sealed and extends into an inner cavity of the side-through pressurizing pipe 504, and the plunger pressurizing pump 505 is configured to control chloroacetic acid condensed in the return pipe 501 to realize pressurized liquid by telescoping.
The plunger pressurizing pump 505 is arranged on the side-through pressurizing pipe 504, so that the chloroacetic acid can be effectively discharged at high pressure during discharging chloroacetic acid, and the chloroacetic acid condensate can be effectively and rapidly fed into the reaction kettle 3.
Working principle:
the invention also provides a forced condensing method for reducing chloroacetic acid consumption in the production of methyl chloroacetate by using the forced condensing system for reducing chloroacetic acid consumption, which comprises the following steps:
s1: installing the forced condensing system for reducing chloroacetic acid consumption into a methyl chloroacetate production system;
the inlet end of the forced condensing system for reducing the consumption of the chloroacetic acid is connected with the outlet end of the distillation gas phase pipe 1 of the methyl chloroacetate production system, and the outlet ends of the chloroacetic acid reflux mechanisms 5 of the forced condensing system for reducing the consumption of the chloroacetic acid are respectively connected with the feed inlet of the reaction kettle 3 of the methyl chloroacetate production system;
s2: preheating the discharging pipelines of the methyl chloroacetate production system and the forced condensing system for reducing the consumption of the chloroacetic acid, adding the reaction raw materials in proportion after the preheating reaches the requirement, and simultaneously starting equipment such as a reaction kettle 3 and the like of the methyl chloroacetate production system and starting the forced condensing system for reducing the consumption of the chloroacetic acid;
s3: controlling each reaction raw material to heat in the reaction kettle 3 and form azeotrope formed by materials such as ester, water, alcohol, acid and the like, and fully reacting, wherein the azeotrope moves upwards in the reaction process and enters the first-stage diversion condenser 2 of the forced condensation system for reducing chloroacetic acid consumption from the outlet end of the distillation gas phase pipe 1;
s4: the azeotrope is controlled to pass through the primary diversion condenser 2 in sequence to realize primary condensation, the circulating heating container 12 is controlled to continuously convey cooling liquid with the temperature lower than the boiling point temperature of chloroacetic acid and higher than the boiling point temperature of the rest azeotrope into the annular condensation channel 605, the temperature of the cooling liquid is preferably 95-100 ℃, and the cooling liquid realizes primary forced condensation liquefaction of the chloroacetic acid in the primary diversion condenser 2;
in the process of introducing the cooling liquid, the temperature of the cooling liquid is monitored in real time by utilizing a waterproof temperature sensor 608 and kept in a set temperature range, and the cooling liquid with lower temperature is electrically heated by utilizing a heat preservation electric heating sleeve, so that the heating degree is controlled by a heat preservation controller 607;
s5: the azeotrope is cooled by the first-stage diversion condenser 2 and then continuously flows downwards, and the chloroacetic acid is subjected to second-stage forced condensation liquefaction and third-stage forced condensation liquefaction by the second-stage diversion condenser 14 and the third-stage diversion condenser 15, so that the chloroacetic acid content in the azeotrope is reduced;
s6: the chloroacetic acid condensate condensed and liquefied in each level of diversion condenser is accumulated in the chloroacetic acid reflux mechanisms 5, the liquid inlet one-way control valve 502 of each chloroacetic acid reflux mechanism 5 is controlled to be opened, so that the chloroacetic acid condensate enters the reflux pipe 501, then the plunger pressurizing pump 505 is controlled to work to pressurize the chloroacetic acid condensate in the reflux pipe 501, and the liquid outlet one-way control valve 503 is opened, so that the chloroacetic acid condensate is refluxed into the reaction kettle 3;
s7: after the reflux is finished, the chloroacetic acid condensate flows back into the reaction kettle 3 for continuous reaction;
s8: thus, the multistage repeated condensation reflux and the repeated utilization of the chloroacetic acid in the reaction process are realized reciprocally, and the full utilization of the chloroacetic acid is ensured.
The whole system can be effectively matched with various existing methyl chloroacetate production systems, can be directly matched for use without greatly improving the methyl chloroacetate production system, and has strong overall universality and high installation flexibility. The system utilizes the first-stage diversion condenser 2, the second-stage diversion condenser 14 and the third-stage diversion condenser 15 to realize multistage condensation of chloroacetic acid on the reacted azeotrope gas, ensures that only chloroacetic acid is liquefied and other azeotropes are not liquefied, and can effectively ensure full recycling of chloroacetic acid. Only liquefy chloroacetic acid and not liquefy other azeotrope when the system condenses, can guarantee the abundant recycle of chloroacetic acid effectively, and each chloroacetic acid reflux mechanism 5 is directly utilized in the time of retrieving can realize effectively retrieving chloroacetic acid condensate to the reation kettle 3 in collect, guarantees reuse, the abundant reaction of chloroacetic acid, reduces the waste of chloroacetic acid in the whole reaction effectively, has reduced product cost, has improved market competition.
The above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention and are intended to be within the scope of the appended claims and description; any alternative modifications or variations to the embodiments of the present invention will fall within the scope of the present invention for those skilled in the art.
The present invention is not described in detail in the present application, and is well known to those skilled in the art.
Claims (7)
1. The forced condensation method for reducing chloroacetic acid consumption in the production of methyl chloroacetate, which is used in a methyl chloroacetate production system, is characterized in that: the method comprises a first-stage diversion condenser arranged at the outlet end of a distillation gas phase pipe, wherein the inlet end of the distillation gas phase pipe is connected with a reaction kettle in a methyl chloroacetate production system, azeotrope formed by ester, water, alcohol and acid materials is arranged in the reaction kettle, a second-stage diversion condenser is connected to the downstream of the first-stage diversion condenser, a third-stage diversion condenser is connected to the downstream of the second-stage diversion condenser, a main heat insulation structure is arranged between the first-stage diversion condenser and the second-stage diversion condenser and between the second-stage diversion condenser and the third-stage diversion condenser, the first-stage diversion condenser, the second-stage diversion condenser and the third-stage diversion condenser are all used for forcedly condensing chloroacetic acid in azeotrope, a monochloroacetic acid reflux mechanism is arranged at the bottoms of the first-stage diversion condenser, the second-stage diversion condenser and the third-stage diversion condenser, and the chloroacetic acid reflux mechanisms are respectively used for carrying out reflux and reutilization in the upstream reaction kettle after pressurizing the chloroacetic acid, and the temperature of cooling liquid of each diversion condenser is lower than the boiling point temperature of the chloroacetic acid and higher than the boiling point temperature of the rest azeotrope.
2. The forced condensing method for reducing chloroacetic acid consumption in the production of methyl chloroacetate of claim 1, wherein: the main heat insulation structure comprises a heat insulation pipe support, a heat insulation cavity which is arranged in a penetrating mode is arranged in the center of the heat insulation pipe support, an annular clamping cavity is arranged at the top and the bottom of the heat insulation pipe support on the periphery of the heat insulation cavity respectively, a heat insulation layer exists between the annular clamping cavities, and two annular clamping cavities on the same heat insulation pipe support are used for being in sealing clamping connection with a diversion condenser sleeved on the corresponding end portion.
3. The forced condensing method for reducing chloroacetic acid consumption in the production of methyl chloroacetate according to claim 2, wherein: and sealing rings are respectively arranged in the annular clamping cavities.
4. A forced condensing process for reducing chloroacetic acid consumption in the production of methyl chloroacetate of claim 3, wherein: the first-stage water conservancy diversion condenser includes strong cold pipe, strong cold pipe includes the U type pipeline section in middle part the both ends top of U type pipeline section is integrated into one piece respectively and is connected with a return bend switching-over section, and the upper reaches return bend switching-over section is connected distillation gas phase pipe exit end, the low reaches return bend switching-over section is connected the entrance point of second grade water conservancy diversion condenser, strong cold pipe includes water conservancy diversion inner tube, condensation outer tube, water conservancy diversion inner tube with realize linking firmly relatively through a plurality of heat conduction ring between the condensation outer tube, a plurality of water conservancy diversion hole has all been seted up on the surface of each heat conduction ring, water conservancy diversion inner tube with form the annular space condensation passageway that supplies the condensate flow to flow through between the condensation outer tube annular space condensation passageway is inside to be led with circulated flow's coolant liquid, and the coolant liquid is provided circulating power by outside circulating conveying pump.
5. The forced condensing method for reducing chloroacetic acid consumption in methyl chloroacetate production of claim 4, wherein: the structures of the secondary diversion condenser and the tertiary diversion condenser are the same as those of the primary diversion condenser.
6. The forced condensing method for reducing chloroacetic acid consumption in methyl chloroacetate production of claim 5, wherein: the water inlet end of the condensation outer pipe of the primary diversion condenser is connected with a circulating liquid inlet control pipe communicated with an annular condensation channel inside the primary diversion condenser, the water outlet end of the condensation outer pipe of the tertiary diversion condenser is connected with a circulating liquid outlet control pipe communicated with the annular condensation channel inside the tertiary diversion condenser, and the circulating liquid inlet control pipe and the circulating liquid outlet control pipe are respectively connected with a circulating heating container through circulating pipelines, and a circulating conveying pump is arranged on the circulating pipeline.
7. The forced condensing method for reducing chloroacetic acid consumption in methyl chloroacetate production of claim 6, wherein: the inner cavity side wall of the U-shaped pipe section of each diversion inner pipe is provided with a spiral internal thread diversion trench.
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| CN114681944A (en) | 2022-07-01 |
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