CN114681944A - Forced condensation system and method for reducing chloroacetic acid consumption in methyl chloroacetate production - Google Patents
Forced condensation system and method for reducing chloroacetic acid consumption in methyl chloroacetate production Download PDFInfo
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- CN114681944A CN114681944A CN202210063232.6A CN202210063232A CN114681944A CN 114681944 A CN114681944 A CN 114681944A CN 202210063232 A CN202210063232 A CN 202210063232A CN 114681944 A CN114681944 A CN 114681944A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0036—Multiple-effect condensation; Fractional condensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Abstract
The invention relates to the technical field of fine organic chemical forced condensation, in particular to a forced condensation system and a method for reducing chloroacetic acid consumption in methyl chloroacetate production. 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 fine organic chemical forced condensation, in particular to a condensation system which can be applied to a traditional methyl chloroacetate production workshop to improve the production quality of methyl chloroacetate with low cost and fluency, and particularly relates to a forced condensation system and a method for reducing chloroacetic acid consumption in the production of methyl chloroacetate.
Background
During esterification in the traditional workshop for producing methyl chloroacetate, raw materials such as methanol, chloroacetic acid and the like can be 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 nos.: CN201410342356.3, patent name: a method for preparing methyl chloroacetate comprises the following specific contents: the method is characterized in that the method comprises the following steps of (1) carrying out gas-liquid-solid three-phase reaction by taking chloroacetic acid and methanol as raw materials and acid resin as a catalyst, wherein the method comprises the following steps: the modified acidic resin is used as a catalyst, and can be completed by adopting a section of fixed bed reactor, and a water-carrying agent is not required to be added in the process, and the method comprises the following steps: (1) uniformly mixing chloroacetic acid and methanol according to a certain proportion; (2) a fixed bed reactor packed with 2/3 parts by volume of catalyst; (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 using a feeding pump; (5) the gas phase reaction product is collected at the top end of the reactor … ….
The above patent discloses a method for producing methyl chloroacetate by gas-liquid-solid three-phase reaction using chloroacetic acid and methanol as raw materials and acidic resin as a catalyst.
In addition, by combining the introduction in the prior art and the long-term experience accumulation of production workers in a processing workshop of the company, the general situation that 1.05 tons of chloroacetic acid and 0.1 ton of soda ash are consumed for producing 1 ton of methyl chloroacetate by using the traditional process during production is found, and the time consumption for producing a single batch of materials is reduced to 42-45 hours; in addition, the traditional processing technology and system have the problem of excessive consumption of chloroacetic acid during methyl chloroacetate production, which not only causes huge dosage of chloroacetic acid, but also influences product yield of the whole production process and product production time consumption.
The excessive consumption of chloroacetic acid in the traditional production process also causes the over-high acidity of the product, affects the product quality, and the excessive consumption of chloroacetic acid affects the product cost, thereby causing the excessive waste of raw materials in the traditional process and equipment for producing methyl chloroacetate and having no market competitiveness.
Although the traditional workshop has the problems, the production process and the production equipment of methyl chloroacetate in the original workshop are mature technologies, and the too large change not only can cause the abnormal operation of the workshop, but also can cause the overhigh construction cost.
Therefore, how to realize the production of methyl chloroacetate with lower cost, reduce the consumption of chloroacetic acid and improve the quality and yield of products is of great significance to the prior art.
Therefore, the forced condensation system which can be applied to the traditional methyl chloroacetate production workshop to improve the production quality of methyl chloroacetate is innovatively designed at low cost and fluently, so that the problems in the prior art are better solved.
Disclosure of Invention
In order to solve one of the technical problems, the invention adopts the technical scheme that: reduce the compulsory condensing system of chloroacetic acid consumption in methyl chloroacetate production, reduce the compulsory condensing system of chloroacetic acid consumption and use in methyl chloroacetate production system in methyl chloroacetate production, including installing the one-level water conservancy diversion condenser at distillation gas phase pipe exit end, the reation kettle in the methyl chloroacetate production system is connected to the entrance point of distillation gas phase pipe, is equipped with the azeotrope that materials such as ester, water, alcohol, acid formed in the reation kettle, be connected with second grade water conservancy diversion condenser in the low reaches of one-level water conservancy diversion condenser, be connected with tertiary water conservancy diversion condenser in the low reaches of second grade water conservancy diversion condenser, all install main heat-insulating structure between one-level water conservancy diversion condenser and second grade water conservancy diversion condenser, between second grade water conservancy diversion condenser and the tertiary water conservancy diversion condenser, first-level water conservancy diversion condenser, second grade water conservancy diversion condenser, tertiary water conservancy diversion condenser all are only used for carrying out the compulsory condensation to the chloroacetic acid in the azeotrope, and chloroacetic acid reflux mechanisms are respectively arranged at the bottoms of the first-stage diversion condenser, the second-stage diversion condenser and the third-stage diversion condenser and are used for pressurizing chloroacetic acid and then refluxing the chloroacetic acid and conveying the chloroacetic acid to an upstream reaction kettle for reuse.
It is preferred in any of the above-mentioned schemes that main thermal-insulated structure includes a thermal-insulated conduit saddle, thermal-insulated conduit saddle center is provided with the thermal-insulated chamber that link up the setting thermal-insulated chamber the outlying thermal-insulated conduit saddle top and the bottom in thermal-insulated chamber are provided with an annular joint chamber respectively, two there is the partition layer between the annular joint chamber, and two annular joint chambers on the same thermal-insulated conduit saddle are used for sealing the joint cover to establish on the water conservancy diversion condenser that corresponds the tip.
In any of the above schemes, it is preferable that a sealing ring is respectively provided in each annular clamping cavity.
Preferably, in any of the above schemes, the first-stage diversion condenser includes a forced cooling pipe, the forced cooling pipe includes a U-shaped pipe section at the middle part, the top of the two ends of the U-shaped pipe section is respectively connected with a bend reversing section in an integrated forming manner, the upper part of the bend reversing section is connected with the outlet end of the distillation gas phase pipe, the lower part of the bend reversing section is connected with the inlet end of the second-stage diversion condenser, the forced cooling pipe includes 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 conduction rings, a plurality of diversion holes are respectively formed on the surface of each heat conduction ring, an annulus condensation channel for the flowing of the condensate liquid is formed between the diversion inner pipe and the condensation outer pipe, the cooling liquid capable of circularly flowing is communicated inside the annulus condensation channel, the cooling liquid has an external circulating delivery pump to provide circulating power, and the temperature of the cooling liquid is lower than the boiling temperature of chloroacetic acid, Above the boiling temperature of the remaining azeotrope.
In any of the above schemes, preferably, a heat-insulating electric heating jacket is sleeved on the periphery of the condensation outer pipe, and the heat-insulating electric heating jacket is connected with an external power supply through a lead.
In any of the above schemes, preferably, the heat-insulating electric heating jacket is further provided with a heat-insulating controller, a plurality of waterproof temperature sensors are installed on the side wall of the annular condensation channel along the flowing direction of the cooling liquid, and each waterproof temperature sensor is in signal connection with the heat-insulating controller.
In any of the above schemes, preferably, the structures of the second-stage diversion condenser and the third-stage diversion condenser are the same as the structure of the first-stage diversion condenser.
It is preferred in any preceding scheme the end of intaking of the condensation outer tube of one-level water conservancy diversion condenser is connected with a circulation feed liquor control pipe rather than the annular space condensation passageway of inside and is linked together the play water end of the condensation outer tube of tertiary water conservancy diversion condenser is connected with a circulation play liquid control pipe rather than the annular space condensation passageway of inside and is linked together, circulation feed liquor control pipe the circulation play liquid control pipe is connected with a circulation heating container through circulation pipeline respectively circulation pipeline all install the circulation delivery pump on the circulation pipeline.
In any of the above schemes, preferably, a spiral internal thread diversion trench is provided on the inner cavity side wall of the U-shaped pipe section of each diversion inner pipe.
In any of the above schemes, preferably, the chloroacetic acid reflux mechanism includes a reflux pipe installed at the bottom of the U-shaped pipe section of the condensation outer pipe, the reflux pipe is communicated with the interior of the annular condensation channel at the corresponding position, 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, one side of the upper part of the return pipe is communicated with a side-through pressurizing pipe, the outer end of the upper part of the side-through pressurizing pipe is provided with a plunger pressurizing pump, the piston end of the plunger pressurizing pump movably and hermetically extends into the 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 discharge through expansion and contraction.
The invention also provides a forced condensation method for reducing chloroacetic acid consumption in methyl chloroacetate production by using the forced condensation system for reducing chloroacetic acid consumption, which comprises the following steps:
s1: installing the forced condensation system for reducing the consumption of the chloroacetic acid into a methyl chloroacetate production system;
connecting the inlet end of the forced condensation system for reducing chloroacetic acid consumption to the outlet end of a distillation gas phase pipe of a methyl chloroacetate production system, and simultaneously connecting the outlet ends of all chloroacetic acid reflux mechanisms of the forced condensation system for reducing chloroacetic acid consumption to the feed inlet of a reaction kettle of the methyl chloroacetate production system respectively;
s2: preheating discharge pipelines of a methyl chloroacetate production system and the forced condensation system for reducing chloroacetic acid consumption, adding reaction raw materials in proportion after preheating meets the requirement, simultaneously starting equipment such as a reaction kettle of the methyl chloroacetate production system and the like, and starting the forced condensation system for reducing chloroacetic acid consumption;
s3: controlling each reaction raw material to be heated in the reaction kettle and form an 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: controlling the azeotrope to sequentially pass through a first-stage diversion condenser to realize first-stage condensation, controlling a circulating heating container 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 an annular condensation channel, preferably controlling the temperature of the cooling liquid to be 95-100 ℃, and realizing first-stage forced condensation and liquefaction of chloroacetic acid in the first-stage diversion condenser by the cooling liquid;
in the process of introducing the cooling liquid, a waterproof temperature sensor is utilized to monitor the temperature of the cooling liquid in real time and keep the temperature within a set temperature range, a heat-preservation electric heating sleeve is utilized to realize electric heating on the cooling liquid with lower temperature, and a heat-preservation controller is utilized to control the heating degree;
s5: the azeotrope continuously flows downstream after passing through the first-stage diversion condenser and cooling, and the chloroacetic acid is subjected to second-stage forced condensation liquefaction and third-stage forced condensation liquefaction through the second-stage diversion condenser and the third-stage diversion condenser, so that the chloroacetic acid content in the azeotrope is reduced;
s6: chloroacetic acid condensate condensed and liquefied in each stage of diversion condenser can be accumulated in a chloroacetic acid reflux mechanism, the opening of a liquid inlet one-way control valve of each chloroacetic acid reflux mechanism is controlled, so that the chloroacetic acid condensate enters a reflux pipe, then a plunger pressure pump is controlled to work to pressurize the chloroacetic acid condensate in the reflux pipe, and then a liquid outlet one-way control valve is opened, so that the chloroacetic acid condensate is refluxed into a reaction kettle;
s7: after the reflux is finished, refluxing chloroacetic acid condensate into the reaction kettle for continuous reaction;
s8: multistage repeated condensation reflux and reutilization of chloroacetic acid in the reaction process are repeatedly realized, so that the chloroacetic acid is fully utilized.
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, thereby effectively ensuring the full recycling of chloroacetic acid.
3. Only liquefy chloroacetic acid and do not liquefy other azeotropes during the system condensation, can guarantee the abundant recycle of chloroacetic acid effectively, each chloroacetic acid backward flow mechanism of direct utilization can realize effectively retrieving the chloroacetic acid condensate and collect in the reation kettle during the recovery, 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 detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or components are generally identified by like reference numerals. In the drawings, elements or components are not necessarily drawn to scale.
Fig. 1 is a schematic structural view of the installation state 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 first stage diversion condenser; 3. a reaction kettle; 4. a primary insulating structure; 401. a heat-insulating pipe bracket; 402. a thermally insulating cavity; 403. an annular clamping cavity; 404. a seal ring; 5. a 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 communicated laterally; 505. a plunger pressure pump; 6. a forced cooling pipe; 601. a flow guiding inner pipe; 602. condensing the outer tube; 603. a heat conducting ring; 604 flow guiding holes; 605. an annular condensing channel; 607. a heat preservation controller; 608. a waterproof type 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. circularly heating the container; 13. a circulating delivery pump; 14. a secondary diversion condenser; 15. and a third-stage diversion condenser.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby. The specific structure of the invention is shown in fig. 1-2.
Example 1:
reduce the compulsory condensing system of chloroacetic acid consumption in methyl chloroacetate production, reduce the compulsory condensing system of chloroacetic acid consumption and use in methyl chloroacetate production system in methyl chloroacetate production, including installing the one-level water conservancy diversion condenser 2 at distillation gas phase pipe 1 exit end in the methyl chloroacetate production, reation kettle 3 in the entrance connection methyl chloroacetate production system of distillation gas phase pipe is equipped with the azeotrope that materials such as ester, water, alcohol, acid formed in reation kettle 3, the low reaches of one-level water conservancy diversion condenser 2 are connected with second grade water conservancy diversion condenser 14, third grade water conservancy diversion condenser 15 is connected to the low reaches of second grade water conservancy diversion condenser 14, all install main heat-proof structure 4 between one-level water conservancy diversion condenser 2 and second grade water conservancy diversion condenser 14, between second grade water conservancy diversion condenser 14 and third grade water conservancy diversion condenser 15, one-level water conservancy diversion condenser 2, second grade water conservancy diversion condenser 14, The three-stage diversion condensers 15 are only used for forcibly condensing chloroacetic acid in the azeotrope, chloroacetic acid reflux mechanisms 5 are mounted at the bottoms of the first-stage diversion condensers 2, the second-stage diversion condensers 14 and the third-stage diversion condensers 15, and the chloroacetic acid reflux mechanisms 5 are respectively used for pressurizing chloroacetic acid and then refluxing and conveying the chloroacetic acid to the upstream reaction kettle 3 for reuse.
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.
This system can be better after the installation is accomplished the current methyl chloroacetate production system of matching use, open methyl chloroacetate production system and can directly utilize one-level water conservancy diversion condenser 2, second grade water conservancy diversion condenser 14, tertiary water conservancy diversion condenser 15 realizes realizing multistage condensation chloroacetic acid to the azeotrope gas that reacts out, guarantee only to liquefy chloroacetic acid and do not liquefy other azeotrope, thereby can guarantee the abundant recycle of chloroacetic acid effectively, directly utilize each chloroacetic acid backward flow mechanism 5 can realize effectively retrieving the chloroacetic acid condensate and collect in reation kettle 3 during the recovery, guarantee the reuse of chloroacetic acid, the abundant reaction, reduce the waste of chloroacetic acid in the whole reaction effectively.
It is preferred in any of the above schemes that main heat-proof structure 4 includes a thermal-insulated conduit saddle 401, thermal-insulated conduit saddle 401 center is provided with the thermal-insulated chamber 402 that link up the setting thermal-insulated chamber 402 that the peripheral thermal-insulated conduit saddle 401 top and bottom of thermal-insulated chamber 402 are provided with an annular joint chamber 403 respectively, two there is the partition layer between the annular joint chamber 403, and two annular joint chambers 403 on the same thermal-insulated conduit saddle 401 are used for the sealing joint cover to establish on the water conservancy diversion condenser that corresponds the tip.
The main functions of the heat insulation pipe bracket 401 are 2: one is to connect the strong cooling pipes 6 of the adjacent diversion condensers and ensure the communication of the inner cavities of the adjacent diversion inner pipes 601 and the communication of the adjacent annular condensation channels 605; and the other one plays roles of heat insulation and sealing.
In any of the above embodiments, it is preferable that a sealing ring 404 is provided in each of the annular clamping cavities 403.
The sealing ring 404 is added to better ensure the sealing performance after connection, so that the problems of air leakage and liquid leakage are prevented.
In any of the above schemes, preferably, the first-stage flow guide condenser 2 includes a forced cooling pipe 6, the forced cooling pipe 6 includes a U-shaped pipe section 7 in the middle, the top of the two ends of the U-shaped pipe section 7 is respectively and integrally connected with a bent pipe reversing section 8, the bent pipe reversing section 8 at the upstream is connected with the outlet end of the distillation gas phase pipe 1, the bent pipe reversing section 8 at the downstream is connected with the inlet end of the second-stage flow guide condenser 14, the forced cooling pipe 6 includes a flow guide inner pipe 601 and a condensation outer pipe 602, the flow guide inner pipe 601 and the condensation outer pipe 602 are relatively and fixedly connected through a plurality of heat conduction rings 603, the surface of each heat conduction ring 603 is provided with a plurality of flow guide holes 604, an annular condensation channel 605 for flowing the condensation liquid is formed between the flow guide inner pipe 601 and the condensation outer pipe 602, and the cooling liquid capable of circulating flows through the annular condensation channel 605, the cooling liquid is provided with an external circulating delivery pump 13 for providing circulating power, and the temperature of the cooling liquid is lower than the boiling temperature of chloroacetic acid and higher than the boiling temperature of the rest azeotrope.
In any of the above solutions, it is preferable that the structures of the secondary diversion condenser 14 and the tertiary diversion condenser 15 are 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, the azeotrope flows through the central diversion inner pipe 601, and the 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, so that the azeotrope can be relatively cooled, and after cooling, ester, water, alcohol and the like in the azeotrope are in a liquefied state because the boiling point is lower than the temperature, only chloroacetic acid can be liquefied, and certainly, a very small amount of other azeotropes can be allowed to be liquefied, and the condensate of monochloroacetic acid is mainly used.
The condensed chloroacetic acid can enter the corresponding chloroacetic acid reflux mechanism 5 for temporary storage, the unreacted azeotrope is continuously conveyed downstream to further complete secondary condensation, and the chloroacetic acid in the azeotrope can be effectively removed through multi-stage condensation.
In any of the above schemes, preferably, the water inlet end of the condensation outer tube 602 of the first-stage diversion condenser 2 is connected with a circulation liquid inlet control tube 9 communicated with the annular condensation channel 605 inside the condensation outer tube, the water outlet end of the condensation outer tube 602 of the third-stage diversion condenser 15 is connected with a circulation liquid outlet control tube 10 communicated with the annular condensation channel 605 inside the condensation outer tube, the circulation liquid inlet control tube 9 and the circulation liquid outlet control tube 10 are respectively connected with a circulation heating container 12 through a circulation pipeline 11, and the circulation pipeline 11 is provided with a circulation delivery pump 13.
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 inside, and the circulation delivery pump 13 can improve the delivery efficiency.
In any of the above schemes, 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 effect of spiral helicine internal thread guiding gutter has 2, and one is: the contact area of the azeotrope and the inner side wall of the diversion inner pipe 601 can be properly increased; the second is that: the length of the walking path of the azeotrope in the inner diversion pipe 601 can be effectively prolonged, and the condensation effect is increased.
Example 2:
reduce the compulsory condensing system of chloroacetic acid consumption in methyl chloroacetate production, reduce the compulsory condensing system of chloroacetic acid consumption and use in methyl chloroacetate production system in methyl chloroacetate production, including installing the one-level water conservancy diversion condenser 2 at distillation gas phase pipe 1 exit end in the methyl chloroacetate production, reation kettle 3 in the entrance connection methyl chloroacetate production system of distillation gas phase pipe is equipped with the azeotrope that materials such as ester, water, alcohol, acid formed in reation kettle 3, the low reaches of one-level water conservancy diversion condenser 2 are connected with second grade water conservancy diversion condenser 14, third grade water conservancy diversion condenser 15 is connected to the low reaches of second grade water conservancy diversion condenser 14, all install main heat-proof structure 4 between one-level water conservancy diversion condenser 2 and second grade water conservancy diversion condenser 14, between second grade water conservancy diversion condenser 14 and third grade water conservancy diversion condenser 15, one-level water conservancy diversion condenser 2, second grade water conservancy diversion condenser 14, The three-stage diversion condensers 15 are only used for forcibly condensing chloroacetic acid in the azeotrope, chloroacetic acid reflux mechanisms 5 are mounted at the bottoms of the first-stage diversion condensers 2, the second-stage diversion condensers 14 and the third-stage diversion condensers 15, and the chloroacetic acid reflux mechanisms 5 are respectively used for pressurizing chloroacetic acid and then refluxing and conveying the chloroacetic acid to the upstream reaction kettle 3 for reuse.
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.
This system can be better after the installation is accomplished the current methyl chloroacetate production system of matching use, open methyl chloroacetate production system and can directly utilize one-level water conservancy diversion condenser 2, second grade water conservancy diversion condenser 14, tertiary water conservancy diversion condenser 15 realizes realizing multistage condensation chloroacetic acid to the azeotrope gas that reacts out, guarantee only to liquefy chloroacetic acid and do not liquefy other azeotrope, thereby can guarantee the abundant recycle of chloroacetic acid effectively, directly utilize each chloroacetic acid backward flow mechanism 5 can realize effectively retrieving the chloroacetic acid condensate and collect in reation kettle 3 during the recovery, guarantee the reuse of chloroacetic acid, the abundant reaction, reduce the waste of chloroacetic acid in the whole reaction effectively.
It is preferred in any of the above schemes that main heat-proof structure 4 includes a thermal-insulated conduit saddle 401, thermal-insulated conduit saddle 401 center is provided with the thermal-insulated chamber 402 that link up the setting thermal-insulated chamber 402 that the peripheral thermal-insulated conduit saddle 401 top and bottom of thermal-insulated chamber 402 are provided with an annular joint chamber 403 respectively, two there is the partition layer between the annular joint chamber 403, and two annular joint chambers 403 on the same thermal-insulated conduit saddle 401 are used for the sealing joint cover to establish on the water conservancy diversion condenser that corresponds the tip.
The main functions of the heat insulation pipe bracket 401 are 2: one is to connect the strong cooling pipes 6 of the adjacent diversion condensers and ensure the communication of the inner cavities of the adjacent diversion inner pipes 601 and the communication of the adjacent annular condensation channels 605; and the other one plays roles of heat insulation and sealing.
In any of the above embodiments, it is preferable that a sealing ring 404 is provided in each of the annular clamping cavities 403.
The sealing ring 404 is added to better ensure the sealing performance after connection and prevent the problems of air leakage and liquid leakage.
In any of the above schemes, preferably, the first-stage flow guide condenser 2 includes a forced cooling pipe 6, the forced cooling pipe 6 includes a U-shaped pipe section 7 in the middle, the top of the two ends of the U-shaped pipe section 7 is respectively and integrally connected with a bent pipe reversing section 8, the bent pipe reversing section 8 at the upstream is connected with the outlet end of the distillation gas phase pipe 1, the bent pipe reversing section 8 at the downstream is connected with the inlet end of the second-stage flow guide condenser 14, the forced cooling pipe 6 includes a flow guide inner pipe 601 and a condensation outer pipe 602, the flow guide inner pipe 601 and the condensation outer pipe 602 are relatively and fixedly connected through a plurality of heat conduction rings 603, the surface of each heat conduction ring 603 is provided with a plurality of flow guide holes 604, an annular condensation channel 605 for flowing the condensation liquid is formed between the flow guide inner pipe 601 and the condensation outer pipe 602, and the cooling liquid capable of circulating flows through the annular condensation channel 605, the cooling liquid is provided with an external circulating delivery pump 13 for providing circulating power, and the temperature of the cooling liquid is lower than the boiling temperature of chloroacetic acid and higher than the boiling temperature of the rest azeotrope.
In any of the above solutions, it is preferable that the structures of the secondary diversion condenser 14 and the tertiary diversion condenser 15 are 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, the azeotrope flows through the central diversion inner pipe 601, and the 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, so that the azeotrope can be relatively cooled, and after cooling, ester, water, alcohol and the like in the azeotrope are in a liquefied state because the boiling point is lower than the temperature, only chloroacetic acid can be liquefied, and certainly, a very small amount of other azeotropes can be allowed to be liquefied, and the condensate of monochloroacetic acid is mainly used.
The condensed chloroacetic acid can enter the corresponding chloroacetic acid reflux mechanism 5 for temporary storage, the unreacted azeotrope is continuously conveyed downstream to further complete secondary condensation, and the chloroacetic acid in the azeotrope can be effectively removed through multi-stage condensation.
In any of the above schemes, preferably, a heat-insulating electric heating jacket is sleeved on the periphery of the condensation outer tube 602, and the heat-insulating electric heating jacket 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 inside the condensing outer tube 602 is kept within a required temperature range.
In any of the above embodiments, it is preferable that the heat-insulating electric heating jacket further includes a heat-insulating controller 607, a plurality of waterproof temperature sensors 608 are mounted on a side wall of the annular condensation passage 605 along a flow direction of the cooling liquid, and each of the waterproof temperature sensors 608 is in signal connection with the heat-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 purpose of receiving signals and controlling the heating of the heat-preservation electric heating jacket by the heat-preservation controller 607 is achieved.
In any of the above schemes, preferably, the water inlet end of the condensation outer tube 602 of the first-stage diversion condenser 2 is connected with a circulation liquid inlet control tube 9 communicated with the annular condensation channel 605 inside the condensation outer tube, the water outlet end of the condensation outer tube 602 of the third-stage diversion condenser 15 is connected with a circulation liquid outlet control tube 10 communicated with the annular condensation channel 605 inside the condensation outer tube, the circulation liquid inlet control tube 9 and the circulation liquid outlet control tube 10 are respectively connected with a circulation heating container 12 through a circulation pipeline 11, and the circulation pipeline 11 is provided with a circulation delivery pump 13.
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 inside, and the circulation delivery pump 13 can improve the delivery efficiency.
In any of the above schemes, 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 effect of spiral helicine internal thread guiding gutter has 2, and one is: the contact area of the azeotrope and the inner side wall of the diversion inner pipe 601 can be properly increased; the second is that: the length of the walking path of the azeotrope in the inner diversion pipe 601 can be effectively prolonged, and the condensation effect is increased.
In any of the above schemes, preferably, 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 reflux pipe 501 is communicated with the interior of the annular condensation channel 605 at a corresponding position, the tail end of the reflux pipe 501 is connected back to the feed port of the reaction kettle 3, and the upper end and the tail end of the reflux pipe 501 are both provided with a liquid inlet one-way control valve 502 and a liquid outlet one-way control valve 503.
The mutual matching of the liquid inlet one-way control valve 502 and the liquid outlet one-way control valve 503 can effectively control the one-way fluidity of chloroacetic acid.
In any of the above embodiments, a side-through pressurizing pipe 504 is preferably communicated with one side of the upper portion of the return pipe 501, a plunger pressurizing pump 505 is mounted at the outer end of the upper portion of the side-through pressurizing pipe 504, the piston end of the plunger pressurizing pump 505 movably and hermetically extends into the inner cavity of the side-through pressurizing pipe 504, and the plunger pressurizing pump 505 extends and retracts to control chloroacetic acid condensed in the return pipe 501 to realize pressurized liquid discharge.
The plunger pressure pump 505 arranged on the side-through pressure pipe 504 can effectively ensure that the chloroacetic acid is effectively discharged at high pressure when the chloroacetic acid is discharged, and the chloroacetic acid condensate is effectively fed into the reaction kettle 3 quickly.
The working principle is as follows:
the invention also provides a forced condensation method for reducing chloroacetic acid consumption in methyl chloroacetate production by using the forced condensation 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;
connecting the inlet end of the forced condensation system for reducing chloroacetic acid consumption to the outlet end of a distillation gas phase pipe 1 of a methyl chloroacetate production system, and respectively connecting the outlet ends of chloroacetic acid reflux mechanisms 5 of the forced condensation system for reducing chloroacetic acid consumption to the feed inlet of a reaction kettle 3 of the methyl chloroacetate production system;
s2: preheating discharge pipelines of a methyl chloroacetate production system and the forced condensation system for reducing chloroacetic acid consumption, adding reaction raw materials in proportion after the preheating meets the requirement, simultaneously starting equipment such as a reaction kettle 3 of the methyl chloroacetate production system and the like, and starting the forced condensation system for reducing chloroacetic acid consumption;
s3: controlling each reaction raw material to be heated in the reaction kettle 3 and form an 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: controlling the azeotrope to sequentially pass through the first-stage diversion condenser 2 to realize first-stage condensation, controlling the circulating heating container 12 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, preferably controlling the temperature of the cooling liquid to be 95-100 ℃, and realizing first-stage forced condensation and liquefaction of chloroacetic acid in the first-stage diversion condenser 2 by the cooling liquid;
in the process of introducing the cooling liquid, the temperature of the cooling liquid is monitored by the waterproof temperature sensor 608 in real time to be kept within a set temperature range, the cooling liquid with lower temperature is electrically heated by the heat-insulating electric heating jacket, and the heating degree is controlled by the heat-insulating controller 607;
s5: the azeotrope continuously flows downstream after passing through the first-stage diversion condenser 2 and after being cooled, and the chloroacetic acid is subjected to second-stage forced condensation liquefaction and third-stage forced condensation liquefaction through 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: chloroacetic acid condensate condensed and liquefied in each stage of diversion condenser can be accumulated in a chloroacetic acid reflux mechanism 5, a 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 a reflux pipe 501, then a plunger pressure pump 505 is controlled to work to pressurize the chloroacetic acid condensate in the reflux pipe 501, and a liquid outlet one-way control valve 503 is opened, so that the chloroacetic acid condensate is refluxed into a reaction kettle 3;
s7: after the reflux is finished, refluxing chloroacetic acid condensate into the reaction kettle 3 for continuous reaction;
s8: multistage repeated condensation reflux and reutilization of chloroacetic acid in the reaction process are repeatedly realized, so that the chloroacetic acid is fully utilized.
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. This system utilizes one-level water conservancy diversion condenser 2, second grade water conservancy diversion condenser 14, tertiary water conservancy diversion condenser 15 to realize realizing multistage condensation chloroacetic acid to the azeotrope gas that reacts, guarantees only to liquefy chloroacetic acid and not liquefy other azeotropes to can guarantee the abundant recycle of chloroacetic acid effectively. Only liquefy chloroacetic acid and do not liquefy other azeotropes during the system condensation, can guarantee the abundant recycle of chloroacetic acid effectively, each chloroacetic acid backward flow mechanism 5 of direct utilization can realize effectively retrieving the chloroacetic acid condensate and collect in reation kettle 3 during the recovery, guarantee reuse, the abundant reaction of chloroacetic acid, reduce the waste of chloroacetic acid in the whole reaction effectively, reduced product cost, improved market competition.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; the modifications or the substitutions do not cause the essence of the corresponding technical solutions to depart from the scope of the technical solutions of the embodiments of the present invention, and the technical solutions are all covered in the scope of the claims and the specification of the present invention; it will be apparent to those skilled in the art that any alternative modifications or variations to the embodiments of the present invention may be made within the scope of the present invention.
The present invention is not described in detail, but is known to those skilled in the art.
Claims (7)
1. Reduce the compulsory condensing system of chloroacetic acid consumption in methyl chloroacetate production, the compulsory condensing system that reduces chloroacetic acid consumption in methyl chloroacetate production installs and uses in methyl chloroacetate production system, its characterized in that: 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, an azeotrope formed by materials such as ester, water, alcohol, acid and the like is filled 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, main heat insulation structures are respectively 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 only used for forcibly condensing chloroacetic acid in the azeotrope, and chloroacetic acid reflux mechanisms are respectively arranged at the bottoms of the first-stage diversion condenser, the second-stage diversion condenser and the third-stage diversion condenser and are used for pressurizing chloroacetic acid and then refluxing and conveying the chloroacetic acid to an upstream reaction kettle for reuse.
2. The forced condensation system for reducing chloroacetic acid consumption in methyl chloroacetate production according to claim 1, wherein: the main heat insulation structure comprises a heat insulation pipe support, a heat insulation cavity which is communicated with the heat insulation pipe support is arranged at the center of the heat insulation pipe support, an annular clamping cavity is respectively arranged at the top and the bottom of the heat insulation cavity, a partition layer is arranged between the annular clamping cavities, and two annular clamping cavities on the same heat insulation pipe support are used for being sleeved on the diversion condenser corresponding to the end part in a sealing clamping mode.
3. The forced condensation system for reducing chloroacetic acid consumption in methyl chloroacetate production according to claim 2, wherein: and a sealing ring is arranged in each annular clamping cavity.
4. A forced condensation system for reducing chloroacetic acid consumption in methyl chloroacetate production according to claim 3, wherein: the one-level water conservancy diversion condenser includes the forced cooling pipe, the forced cooling pipe includes the U type pipeline section at middle part U type pipeline section's both ends top difference integrated into one piece is connected with a return bend switching-over section, the upper reaches the return bend switching-over section is connected distillation gas phase pipe exit end, low reaches the entrance point of second grade water conservancy diversion condenser is connected to return bend switching-over section, the forced cooling pipe includes water conservancy diversion inner tube, condensation outer tube, the 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 liquid to flow through between the condensation outer tube the annular space condensation passageway is inside to lead to has the coolant liquid that can circulate, and the coolant liquid has outside circulating pump to provide circulation power, and the temperature of coolant liquid is less than the boiling temperature of chloroacetic acid, Above the boiling temperature of the remaining azeotrope.
5. The forced condensation system for reducing chloroacetic acid consumption in methyl chloroacetate production according to claim 4, wherein: the structures of the second-stage diversion condenser and the third-stage diversion condenser are the same as the structure of the first-stage diversion condenser.
6. The forced condensation system for reducing chloroacetic acid consumption in methyl chloroacetate production according to claim 5, wherein: the water inlet end of the condensation outer pipe of the first-level diversion condenser is connected with a circulation liquid inlet control pipe communicated with an annular condensation channel inside the condensation outer pipe, the water outlet end of the condensation outer pipe of the third-level diversion condenser is connected with a circulation liquid outlet control pipe communicated with the annular condensation channel inside the condensation outer pipe, the circulation liquid inlet control pipe is connected with a circulation heating container through a circulation pipeline, and a circulation conveying pump is installed on the circulation pipeline.
7. The forced condensation system for reducing chloroacetic acid consumption in methyl chloroacetate production according to claim 6, wherein: spiral internal thread diversion grooves are arranged on the side wall of the inner cavity of the U-shaped pipe section of each diversion inner pipe.
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