CN211514464U - Continuous reaction production device for paraphthaloyl chloride - Google Patents
Continuous reaction production device for paraphthaloyl chloride Download PDFInfo
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- CN211514464U CN211514464U CN201922452243.XU CN201922452243U CN211514464U CN 211514464 U CN211514464 U CN 211514464U CN 201922452243 U CN201922452243 U CN 201922452243U CN 211514464 U CN211514464 U CN 211514464U
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Abstract
The utility model belongs to the technical field of the chemical synthesis device, concretely relates to paraphthaloyl chloride continuous reaction apparatus for producing. The continuous reaction production device for the paraphthaloyl chloride comprises a thionyl chloride tank and a solvent tank, wherein the thionyl chloride tank is connected with a thionyl chloride mixing tank, and the top of the thionyl chloride mixing tank is provided with a catalyst feeding port; the solvent tank is connected with the raw material acid mixing tank, and the top of the raw material acid mixing tank is provided with a terephthalic acid feeding port; and the thionyl chloride mixing tank and the raw acid mixing tank are connected with a feed inlet at the upper part of the reactor. The utility model has simple, stable and high-efficiency process device, can realize continuous production, can lead the solvent to dissolve the terephthalic acid, and changes the original heterogeneous reaction into the homogeneous reaction, thus leading the reaction to be more complete and leading the reaction efficiency to be higher; the catalyst can be added into thionyl chloride, and compared with the existing catalyst which is directly added into a reaction kettle, the catalyst is dispersed more uniformly.
Description
Technical Field
The utility model belongs to the technical field of the chemical synthesis device, concretely relates to paraphthaloyl chloride continuous reaction apparatus for producing.
Background
The paraphthaloyl chloride is a monomer for synthesizing special fiber, can be used as aramid fiber and chinlon reinforcing agent, can be used for preparing resin dye, pigment, medicine, pesticide and the like, and can be used for organic synthesis.
When the thionyl chloride method is used for producing the terephthaloyl chloride, the terephthalic acid is taken as a raw material, reacts with the thionyl chloride under the action of a small amount of catalyst N, N-dimethylformamide or pyridine, and the terephthaloyl chloride product is obtained by distillation, wherein the reaction process is as follows:
the thionyl chloride method has simple production process, the thionyl chloride is an acidic corrosive substance, the thionyl chloride is used for replacing highly toxic raw materials such as phosphorus pentachloride, chlorine, phosgene and the like used in the traditional process, the thionyl chloride is used as a raw material and a solvent to react with a solid raw material under normal pressure, the feeding is convenient, an effective catalyst is selected, the reaction time is short, the yield is improved to more than 98 percent, the product purity reaches more than 99.9 percent, byproducts generated in the process are all gaseous substances, the separation is easy, and the operation danger and the labor intensity of workers are greatly reduced compared with the traditional process.
However, most of the production in the prior art is intermittent reaction, so that a large amount of auxiliary production time exists, the production period is long, and the production efficiency is low. In the reaction process, the raw materials are mixed with the reaction products, the reaction speed is obviously reduced in the later stage of the reaction, the production period is long, the efficiency is low, and the possibility of incomplete reaction exists. In addition, the prior art adopts solid-liquid heterogeneous reaction, and has low reaction rate and incomplete reaction.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is: the continuous reaction production device for the paraphthaloyl chloride overcomes the defects of the prior art, has the characteristics of simple, continuous, stable and efficient process, greatly shortens the reaction period, improves the production efficiency and saves energy.
The utility model discloses an adopt following technical scheme to realize:
the continuous reaction production device for the paraphthaloyl chloride comprises a thionyl chloride tank and a solvent tank, wherein the thionyl chloride tank is connected with a thionyl chloride mixing tank, and the top of the thionyl chloride mixing tank is provided with a catalyst feeding port; the solvent tank is connected with the raw material acid mixing tank, and the top of the raw material acid mixing tank is provided with a terephthalic acid feeding port; and the thionyl chloride mixing tank and the raw acid mixing tank are connected with a feed inlet at the upper part of the reactor.
A material mixing tank stirrer is arranged in the thionyl chloride material mixing tank, and a raw material acid stirrer is arranged in the raw material acid material mixing tank.
The bottom of the thionyl chloride mixing tank is connected with the reactor through a thionyl chloride preheater, and the bottom of the raw material acid mixing tank is connected with the reactor through a raw material acid preheater.
The reactor is a packed tower type reactor, the outer wall of the reactor is provided with a reactor jacket, gas generated by reaction is easy to separate, a distributor is arranged at a feed inlet of the reactor, packing is filled in sections and correspondingly heated in sections, and the reactor repeatedly transfers mass and heat, so that energy can be saved.
The top of reactor has connected gradually one-level condenser, one-level vapour and liquid separator, secondary condenser, second grade vapour and liquid separator and tail gas buffer tank, one-level vapour and liquid separator's top and second grade condenser are connected, and second grade vapour and liquid separator's top and tail gas buffer tank are connected, tail gas buffer tank top and aftertreatment unit connection, one-level vapour and liquid separator's bottom and second grade vapour and liquid separator's bottom all are connected with reactor upper portion.
The bottom discharge hole of the reactor is connected with the refining unit through a product pump, and the product pump is also connected with the middle part of the reactor. Qualified products are extracted from the bottom of the reactor, and unqualified products can be pumped into the middle of the reactor through a product pump to carry out reflux reaction.
The working principle and the process are as follows:
the method comprises the following steps that a solvent enters a raw material acid mixing tank from a solvent tank, a terephthalic acid raw material enters the raw material acid mixing tank from a terephthalic acid feeding port at the top of the raw material acid mixing tank, and the terephthalic acid is dissolved in the solvent under the stirring of a raw material acid stirrer to obtain a terephthalic acid solution; thionyl chloride enters a thionyl chloride mixing tank from a thionyl chloride tank, a catalyst enters the thionyl chloride mixing tank from a catalyst feeding port at the top of the thionyl chloride mixing tank, the catalyst is mixed into the thionyl chloride under the stirring of a mixer of the mixing tank, terephthalic acid solution and a thionyl chloride raw material mixed with the catalyst are preheated by a raw material acid preheater and a thionyl chloride preheater respectively according to a proportion by a metering pump and then enter a reactor for reflux reaction, gas generated in the reaction process, thionyl chloride and solvent steam are discharged from the upper part of the reactor and enter a primary condenser for condensation, a gas-liquid mixture after condensation enters a primary gas-liquid separator for phase separation, a liquid phase gas phase enters a secondary condenser for condensation, a gas-liquid mixture after condensation enters a secondary gas-liquid separator for phase separation, a gas phase enters a post-treatment unit after being buffered by a tail gas buffer tank, and the secondary gas-liquid phase and the primary gas-liquid phase reflux enter the, qualified products are extracted from the bottom of the reactor to the refining unit through the product pump, and unqualified products can be pumped into the middle of the reactor through the product pump to perform reflux reaction.
Compared with the prior art, the beneficial effects of the utility model are as follows:
1. the utility model discloses can make the solvent dissolve terephthalic acid, change the homogeneous reaction into by original heterogeneous reaction for the reaction is more complete, and reaction efficiency is higher.
2. The utility model discloses can make during the catalyst joins in marriage thionyl chloride, compare in directly dropping into reation kettle with current catalyst, the catalyst dispersion is more even.
3. The utility model discloses a reactor be filler tower type reactor, the gaseous easy separation that the reaction produced, reactor feed inlet department is equipped with the distributor, and the filler segmentation is loaded and corresponding segmentation heating, and the reactor is mass transfer heat transfer repeatedly, but the energy saving.
4. The utility model discloses process units is simple, steady and high-efficient, can realize continuous production, has shortened reaction cycle greatly, can increase substantially production efficiency.
Drawings
Fig. 1 is a schematic structural view of the present invention;
in the figure: 1. a thionyl chloride tank; 2. a thionyl chloride pump; 3. a thionyl chloride mixing tank; 4. a mixer of the mixing tank; 5. a catalyst addition port; 6. a thionyl chloride feed pump; 7. a thionyl chloride preheater; 8. a solvent tank; 9. a solvent pump; 10. a raw material acid mixing tank; 11. a raw material acid stirrer; 12. a terephthalic acid feeding port; 13. a feed pump for the raw acid; 14. a raw material acid preheater; 15. a reactor; 16. a reactor jacket; 17. a product pump; 18. a first-stage condenser; 19. a first-stage gas-liquid separator; 20. a secondary condenser; 21. a secondary gas-liquid separator; 22. a tail gas buffer tank; 23. a post-processing unit; 24. and a refining unit.
Detailed Description
The present invention will be further described with reference to the accompanying drawings.
As shown in fig. 1, the continuous reaction production device for terephthaloyl chloride comprises a thionyl chloride tank 1 and a solvent tank 8, wherein the thionyl chloride tank 1 is connected with a thionyl chloride mixing tank 3, a thionyl chloride pump 2 is arranged between the thionyl chloride tank 1 and the thionyl chloride mixing tank 3, and the top of the thionyl chloride mixing tank 3 is provided with a catalyst inlet 5; the solvent tank 8 is connected with a raw material acid mixing tank 10, a solvent pump 9 is arranged between the solvent tank 8 and the raw material acid mixing tank 10, and the top of the raw material acid mixing tank 10 is provided with a terephthalic acid feeding port 12; the bottom of the thionyl chloride mixing tank 3 is connected with a thionyl chloride preheater 7 through a thionyl chloride feed pump 6, the bottom of the raw material acid mixing tank 10 is connected with a raw material acid preheater 14 through a raw material acid feed pump 13, and the top of the thionyl chloride preheater 7 and the top of the raw material acid preheater 14 are connected with a feed inlet on the upper part of the reactor 15.
And a material mixing tank stirrer 4 is arranged in the thionyl chloride material mixing tank 3, and a raw material acid stirrer 11 is arranged in the raw material acid material mixing tank 10.
The reactor 15 is a packed tower type reactor, a distributor is arranged at a feed inlet of the reactor 15, and a reactor jacket 16 is arranged on the outer wall of the reactor 15.
The top of reactor 15 has connected gradually one-level condenser 18, one-level vapour and liquid separator 19, second grade condenser 20, second grade vapour and liquid separator 21 and tail gas buffer tank 22, one-level vapour and liquid separator 19's top and second grade condenser 20 are connected, and second grade vapour and liquid separator 21's top and tail gas buffer tank 22 are connected, tail gas buffer tank 22 top and aftertreatment unit 23 are connected, one-level vapour and liquid separator 19's bottom and second grade vapour and liquid separator 21's bottom all are connected with reactor 15 upper portion.
The bottom discharge hole of the reactor 15 is connected with a refining unit 24 through a product pump 17, and the product pump 17 is also connected with the middle part of the reactor 15.
During operation, a solvent enters a raw material acid mixing tank 10 from a solvent tank 8 through a solvent pump 9, a terephthalic acid raw material enters the raw material acid mixing tank 10 from a terephthalic acid feeding port 12 at the top of the raw material acid mixing tank 10, and terephthalic acid is dissolved in the solvent under the stirring of a raw material acid stirrer 11 to obtain a terephthalic acid solution; thionyl chloride enters a thionyl chloride mixing tank 3 from a thionyl chloride tank 1 through a thionyl chloride pump 2, the catalyst enters the thionyl chloride mixing tank 3 from a catalyst inlet 5 at the top of the thionyl chloride mixing tank 3, the catalyst is mixed into thionyl chloride under the stirring of a mixing tank stirrer 4, terephthalic acid solution enters a raw material acid preheater 14 through a raw material acid feed pump 13, a thionyl chloride raw material mixed with the catalyst enters a thionyl chloride preheater 7 through a thionyl chloride feed pump 6, the raw material is preheated by the preheater and then enters a reactor 15 for reflux reaction, gas generated in the reaction process, the thionyl chloride and solvent steam are discharged from the upper part of the reactor 15 and enter a primary condenser 18 for condensation, the condensed gas-liquid mixture enters a primary gas-liquid separator 19 for phase separation, a liquid phase gas enters a secondary condenser 20 for condensation, the condensed gas-liquid mixture enters a secondary gas-liquid separator 21 for phase separation, the gas phase is buffered by the tail gas buffer tank 22 and then enters the post-processing unit 23, the liquid phase of the secondary gas-liquid separator 21 and the liquid phase of the primary gas-liquid separator 19 flow back to enter the reactor 15, qualified products are extracted from the bottom of the reactor 15 to the refining unit 24 through the product pump 17, and unqualified products can be sent to the middle of the reactor 15 through the product pump 17 to perform reflux reaction.
Of course, the above description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the embodiments of the present invention. The present invention is not limited to the above examples, and the technical field of the present invention is equivalent to the changes and improvements made in the actual range of the present invention, which should be attributed to the patent coverage of the present invention.
Claims (6)
1. The utility model provides a continuous reaction apparatus for producing of p-phthaloyl chloride, includes thionyl chloride jar (1) and solvent jar (8), its characterized in that: the thionyl chloride tank (1) is connected with a thionyl chloride mixing tank (3), and the top of the thionyl chloride mixing tank (3) is provided with a catalyst feeding port (5); the solvent tank (8) is connected with a raw material acid mixing tank (10), and the top of the raw material acid mixing tank (10) is provided with a terephthalic acid feeding port (12); and the thionyl chloride mixing tank (3) and the raw material acid mixing tank (10) are connected with a feed inlet at the upper part of the reactor (15).
2. The continuous terephthaloyl chloride reaction production apparatus of claim 1, wherein: a material mixing tank stirrer (4) is arranged in the thionyl chloride material mixing tank (3), and a raw material acid stirrer (11) is arranged in the raw material acid material mixing tank (10).
3. The continuous terephthaloyl chloride reaction production apparatus of claim 1, wherein: the bottom of the thionyl chloride mixing tank (3) is connected with the reactor (15) through a thionyl chloride preheater (7), and the bottom of the raw material acid mixing tank (10) is connected with the reactor (15) through a raw material acid preheater (14).
4. The continuous terephthaloyl chloride reaction production apparatus of claim 1, wherein: the reactor (15) is a packed tower type reactor, a distributor is arranged at a feed inlet of the reactor (15), and a reactor jacket (16) is arranged on the outer wall of the reactor (15).
5. The continuous terephthaloyl chloride reaction production apparatus of claim 1, wherein: the top of reactor (15) has connected gradually one-level condenser (18), one-level vapour and liquid separator (19), second grade condenser (20), second grade vapour and liquid separator (21) and tail gas buffer tank (22), the top and the second grade condenser (20) of one-level vapour and liquid separator (19) are connected, and the top and the tail gas buffer tank (22) of second grade vapour and liquid separator (21) are connected, tail gas buffer tank (22) top is connected with aftertreatment unit (23), the bottom of one-level vapour and liquid separator (19) and the bottom of second grade vapour and liquid separator (21) all are connected with reactor (15) upper portion.
6. The continuous terephthaloyl chloride reaction production apparatus of claim 1, wherein: the bottom discharge hole of the reactor (15) is connected with a refining unit (24) through a product pump (17), and the product pump (17) is also connected with the middle part of the reactor (15).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922452243.XU CN211514464U (en) | 2019-12-30 | 2019-12-30 | Continuous reaction production device for paraphthaloyl chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922452243.XU CN211514464U (en) | 2019-12-30 | 2019-12-30 | Continuous reaction production device for paraphthaloyl chloride |
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| Publication Number | Publication Date |
|---|---|
| CN211514464U true CN211514464U (en) | 2020-09-18 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201922452243.XU Active CN211514464U (en) | 2019-12-30 | 2019-12-30 | Continuous reaction production device for paraphthaloyl chloride |
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| CN (1) | CN211514464U (en) |
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2019
- 2019-12-30 CN CN201922452243.XU patent/CN211514464U/en active Active
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