CN112358385A - Continuous production equipment and production method for methoxyacetophenone - Google Patents
Continuous production equipment and production method for methoxyacetophenone Download PDFInfo
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- CN112358385A CN112358385A CN202011243218.1A CN202011243218A CN112358385A CN 112358385 A CN112358385 A CN 112358385A CN 202011243218 A CN202011243218 A CN 202011243218A CN 112358385 A CN112358385 A CN 112358385A
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- C07C45/45—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by condensation
- C07C45/46—Friedel-Crafts reactions
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- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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Abstract
The invention relates to continuous production equipment and a continuous production method of methoxyacetophenone, wherein the equipment at least comprises a reaction unit, and the reaction unit comprises a first reaction kettle and a second reaction kettle; the batching unit comprises a first batching tank and a second batching tank which are connected in parallel; the separation unit comprises a first distillation tower, a second distillation tower, a third distillation tower and a crystallizer which are sequentially connected in series. The production method comprises the steps of sequentially introducing an anisole hot solution and an acylation reagent hot solution prepared in a dosing unit into a first reaction kettle, a second reaction kettle, a first distillation tower, a second distillation tower, a third distillation tower and a crystallizer, and finally separating pure white p-methoxyacetophenone crystals. The continuous production equipment and the production method of the methoxyacetophenone provided by the invention can effectively solve the problems of catalyst activity loss and carbon deposition, and the repeated utilization rate of the catalyst is improved.
Description
Technical Field
The invention relates to the field of chemical mechanical equipment, in particular to continuous production equipment and a continuous production method for methoxyacetophenone.
Background
The p-methoxyacetophenone is a white crystal, has the fragrance of hawthorn flowers and similar anisaldehyde, is mainly used for synthesizing medicines and spices, is a key intermediate of puerarin and raloxifene, is commonly used in high-grade cosmetics and soap essence, has high stability in the soap, can also be used as fruit food essence, and has wide market and development prospects.
Friedel-Crafts acylation reaction is an important way for synthesizing p-methoxyacetophenone, and a typical preparation method of the p-methoxyacetophenone is to use anisole as a raw material, acetyl chloride or acetic anhydride as an acylation reagent and use a solid acid catalyst for carrying out Friedel-Crafts acylation reaction.
In the traditional process, Lewis acid (such as ZnCl2 and AlCl3) is usually adopted as a catalyst, the required catalyst amount is large, the reaction temperature is high, the yield is low, and a large amount of waste metal and acid sludge are easily generated due to difficult homogeneous catalytic separation and high energy consumption, so that the equipment corrosion in the production process is serious, and the environmental pollution is caused.
Xumei, etc. of the petrochemical institute of Liaoning petrochemical university use pure heteropoly acid as catalyst, and the acylation reaction of anisole and acetic anhydride is used to synthesize p-methoxyacetophenone, and the yield of the product can reach 52.9% by using modified phosphotungstic acid as catalyst. However, in the process, phosphotungstic acid is completely dissolved in the reaction liquid and is difficult to recover, and moreover, the phosphotungstic acid is easy to coke and deposit carbon in the reaction process, so that the activity of the catalyst is influenced.
Chenping et al at northeast university have studied that H beta zeolite is used as a catalyst to catalyze Friedel-Crafts acylation reaction of anisole and acetic anhydride to selectively generate p-methoxyacetophenone under the condition of no solvent.
In the above process, various problems occur in the batch reaction: (1) the carbon deposition phenomenon is serious, and the activity of the catalyst is rapidly reduced; (2) the loss of active components is serious, and the reuse rate is reduced; (3) the intermittent reaction is difficult to reach the completeness, and the reaction rate is influenced in the later period of the reaction; (4) small scale, low yield, and the simultaneous problem of catalyst removal compared with other processes, thus also resulting in poor yield and purity.
Disclosure of Invention
The invention aims to provide continuous production equipment and a continuous production method for methoxyacetophenone, and solves the problems that the activity of a catalyst is rapidly reduced, the loss of active components is serious, the reuse rate is reduced and the like due to carbon deposition generated in the conventional intermittent production process.
In order to achieve the above object, the present invention provides a continuous production apparatus for methoxyacetophenone, which at least comprises:
the reaction unit comprises a first reaction kettle and a second reaction kettle connected in series with the first reaction kettle;
the batching unit is connected with an input pipeline of the reaction unit and comprises a first batching tank and a second batching tank which is connected with the first batching tank in parallel;
and the separation unit is connected with the output pipeline of the reaction unit and comprises a first distillation tower, a second distillation tower, a third distillation tower and a crystallizer which are sequentially connected in series.
Preferably, first batching jar and second batching jar with be provided with first control valve and second control valve on the connecting pipeline between the first reation kettle respectively, first batching jar and second batching jar respectively through the heat preservation pipeline with first reation kettle links to each other.
Preferably, the bottom of first reation kettle and second reation kettle is provided with the filter, be provided with third control valve and first charge pump on the connecting line between first reation kettle and the second reation kettle, the second reation kettle with be provided with fourth control valve and second charge pump on the connecting line between the first distillation column.
Preferably, the first distillation tower is an atmospheric distillation tower, the second distillation tower is a vacuum distillation tower, the third distillation tower is a rectification tower, a fifth control valve and a third feed pump are arranged on a connecting pipeline between the first distillation tower and the second distillation tower, a sixth control valve and a fourth feed pump are arranged on a connecting pipeline between the second distillation tower and the third distillation tower, and a heat exchanger is further arranged between the fourth feed pump and the third distillation tower.
Preferably, the top of first distillation column is established ties in proper order and is had first condenser and ordinary pressure liquid storage pot, the top of second distillation column is established ties in proper order and is had second condenser and decompression liquid storage pot, third distillation column top is established ties in proper order and is had third condenser and reflux drum, reflux drum bottom end is connected through seventh valve, eighth valve respectively the third distillation column with the crystallizer, the third distillation column bottom is connected with cauldron formula reboiler through fifth charge pump.
Preferably, temperature detectors are respectively arranged at the bottoms of the first batching tank, the second batching tank, the first reaction kettle, the second reaction kettle, the first distillation tower, the second distillation tower, the third distillation tower and the crystallizer, and the temperature detectors feed temperature detection signals back to the DCS system.
Preferably, concentration detectors are respectively arranged at the bottom ends of the first reaction kettle, the second reaction kettle, the first distillation tower and the second distillation tower and at the top end of the third distillation tower, and the concentration detectors feed concentration detection signals back to the DCS system.
The invention also provides a continuous production method of the methoxyacetophenone, which is applied to the continuous production equipment of the methoxyacetophenone and mainly comprises the following steps:
(1) preparing an anisole hot solution at the temperature of 60-80 ℃ in a first preparation tank, and preparing an acylation reagent hot solution at the temperature of 40-50 ℃ in a second preparation tank;
(2) introducing the prepared anisole hot solution and the prepared acylation reagent hot solution into a first reaction kettle, and obtaining a first-stage output liquid with the yield of the p-methoxyacetophenone not less than 60 percent after first-stage reaction;
(3) introducing the primary output liquid into a second reaction kettle, and obtaining a secondary output liquid with the yield of the p-methoxyacetophenone not less than 85% after secondary reaction;
(4) introducing the secondary output liquid into a first distillation tower, and obtaining a primary tower bottom output liquid with the mass fraction of the p-methoxyacetophenone not less than 90% after primary distillation;
(5) introducing the primary tower bottom product liquid into a second distillation tower, and obtaining a secondary tower bottom product liquid with the mass fraction of p-methoxyacetophenone not less than 95% after secondary distillation;
(6) introducing the secondary tower bottom product into a third distillation tower, and performing three-stage distillation to obtain tower top distillate with the mass fraction of p-methoxyacetophenone not less than 99.5%;
(7) and (3) introducing the distillate at the tower top into a crystallizer, cooling and crystallizing, and separating the p-methoxyacetophenone to obtain pure white crystals.
Preferably, the temperature in the first reaction kettle is controlled between 40 ℃ and 80 ℃, and the temperature in the second reaction kettle is controlled between 80 ℃ and 120 ℃.
Preferably, the temperature in the first distillation column is controlled between 90 ℃ and 150 ℃, the temperature in the second distillation column is controlled between 60 ℃ and 100 ℃, the temperature in the third distillation column is controlled between 120 ℃ and 220 ℃, and the temperature in the crystallizer is controlled between-10 ℃ and 10 ℃.
The continuous production equipment and the continuous production method for the methoxyacetophenone, provided by the invention, have the advantages that the raw materials adopted by the process only comprise anisole, an acylation reagent and a solid acid catalyst, the reaction is carried out at normal pressure, and the operation is simple and convenient; the method effectively solves the problems of the loss of the activity of the catalyst and the carbon deposition phenomenon, has short reaction time, and improves the repeated utilization rate of the catalyst; the continuous production method of the methoxyacetophenone has simple process, is easy to realize continuous and automatic production, and improves the industrial production efficiency of the methoxyacetophenone; the grain size distribution of the produced p-methoxyacetophenone is uniform, and the product quality is greatly improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings according to the drawings.
FIG. 1 is a schematic structural diagram of a continuous production apparatus for p-methoxyacetophenone of the present invention;
illustration of the drawings: 1. 2, 6, 12 and 35 are motors; 3 is an anisole batching tank; 4 is an acylation reagent dosing tank; 8 is a first reaction kettle; 13 is a second reaction kettle; 17 is an atmospheric distillation tower; 23 is a reduced pressure distillation tower; 28 is a rectifying tower; 36 is a crystallizer; 5. 7, 10, 15, 18, 22, 32 and 33 are valves; 9. 14 is a filter; 11. 16, 19, 25 and 29 are feed pumps; 20. 24, 30 are condensers; 21 is a normal pressure liquid storage tank; 26 is a tubular heat exchanger; 27 is a pressure reduction liquid storage tank; 31 is a reflux tank; and 34 is a kettle reboiler.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
FIG. 1 is a schematic structural diagram of a continuous production apparatus for p-methoxyacetophenone provided by the present invention.
Continuous production equipment for p-methoxyacetophenone at least comprises a batching unit, a reaction unit and a separation unit, wherein the batching unit comprises an anisole batching tank 3 and an acylation reagent batching tank 4 which are connected in parallel and are respectively used for preparing anisole solution and acylation reagent solution; the reaction unit comprises a first reaction kettle 8 and a second reaction kettle 13 connected in series with the first reaction kettle 8, wherein the first reaction kettle 8 is respectively connected with an anisole batching tank 3 and an acylation reagent batching tank 4 through a valve 5 and a valve 7; the separation unit is connected with an output pipeline of the second reaction kettle 13, and comprises four parts, namely an atmospheric distillation tower 17, a reduced pressure distillation tower 23, a rectifying tower 28 and a crystallizer 36.
8 tops of first reation kettle are connected with batching unit through the heat preservation pipeline, and the bottom exit is provided with filter 9 and valve 10, valve 10 passes through the heat preservation pipeline and is connected with charge pump 11, second reation kettle 13's upper end in proper order, 13 bottom exits of second reation kettle are provided with filter 14 and valve 15, valve 15 passes through the heat preservation pipeline and links to each other with charge pump 16, atmospheric distillation tower 17 in proper order.
A valve 18 and a feeding pump 19 are arranged at an outlet at the bottom end of the atmospheric distillation tower 17, and the feeding pump 19 is connected with a reduced pressure distillation tower 23 through a heat-insulating pipeline; the top end of the atmospheric distillation tower 17 is connected with a condenser 20, and the condenser 20 is connected with an atmospheric liquid storage tank 21. A valve 22 and a feed pump 25 are arranged at an outlet at the bottom end of the reduced pressure distillation tower 23, the feed pump 25 is connected with a tubular heat exchanger 26 through a heat insulation pipeline, and the tubular heat exchanger 26 is connected with a rectification tower 28 through a heat insulation pipeline; the top end of the reduced pressure distillation tower 23 is connected with a condenser 24, and the condenser 24 is connected with a reduced pressure liquid storage tank 27 connected with a vacuum connecting pipe. A feed pump 29 is arranged at the outlet of the bottom end of the rectifying tower 28, the feed pump 29 is connected with a kettle-type reboiler 34 through a heat-insulating pipeline, the reboiled liquid flowing out of the kettle-type reboiler 34 enters the rectifying tower 28 through the heat-insulating pipeline, the top end of the rectifying tower 28 is connected with a condenser 30, the condenser 30 is connected with a reflux tank 31, a valve 32 and a valve 33 are arranged at the outlet of the bottom end of the reflux tank 31, the valve 32 is connected with the rectifying tower 28, and the valve 33 is connected with a crystallizer 36.
Anisole batching jar 3, acylation reagent batching jar 4, first reation kettle 8, second reation kettle 13, the top of crystallizer correspond respectively to be connected with motor 1, motor 2, motor 6, motor 12 and motor 35.
Valves, motors, feeding pumps and heating medium devices arranged in connecting pipelines of the batching unit, the reaction unit and the separation unit are all controlled by a Distributed Control System (DCS for short).
Preferably, temperature detectors are arranged at the bottom of the anisole batching tank 3, the bottom of the acylation reagent batching tank 4, the bottom of the first reaction kettle 8, the bottom of the second reaction kettle 13, the bottom of the atmospheric distillation tower 17, the bottom of the reduced pressure distillation tower 23, the bottom of the rectification tower 28 and the bottom of the crystallizer 36, and are used for detecting the temperature of the internal liquid and feeding back temperature detection signals to the DCS system to realize the control of the reaction temperature.
Preferably, the bottom of the first reaction kettle 8, the bottom of the second reaction kettle 13, the bottom of the atmospheric distillation tower 17, the bottom of the vacuum distillation tower 23, the top of the rectification tower 28 and the tail of the condenser 30 are all connected with a concentration detector, and the concentration detector is used for detecting the concentration of the p-methoxyacetophenone and feeding back a concentration detection signal to the DCS system.
The invention also provides a continuous production method of the methoxyacetophenone, which is applied to the production of the continuous production equipment of the methoxyacetophenone provided by any one of the embodiments and mainly comprises the following steps:
(1) preparing an anisole hot solution with the temperature of 60-80 ℃ in an anisole preparing tank 3, preparing an acylation reagent hot solution with the temperature of 40-50 ℃ in an acylation reagent preparing tank 4, wherein the molar ratio of the anisole hot solution to the acylation reagent hot solution is 1.5: 1.
(2) the DCS controls to open the valve 5 and the valve 7, the prepared anisole hot solution and the prepared acylation reagent hot solution are introduced into the first reaction kettle 8, the reaction temperature in the first reaction kettle 8 is controlled to be 80 ℃, preferably 40-80 ℃, and a first-stage output liquid of the p-methoxyacetophenone is obtained after first-stage reaction.
(3) In the first reaction kettle 8, when the concentration detector detects that the yield of the p-methoxyacetophenone is not lower than 60%, sending feedback information to a DCS (distributed control system), after receiving a feedback signal, starting a filter 9, a valve 10 and a feed pump 11, introducing a primary product liquid into a second reaction kettle 13, and then closing the filter 9, the valve 10 and the feed pump 11; the DCS system controls the reaction temperature in the second reaction kettle 13 to be 100 ℃, preferably between 80 ℃ and 120 ℃, and secondary output liquid of the yield of the p-methoxyacetophenone is obtained.
(4) In the second reaction kettle 13, when the concentration detector detects that the yield of the p-methoxyacetophenone is not lower than 85%, sending feedback information to the DCS, starting the filter 14, the valve 15 and the feed pump 16 by the DCS, introducing a secondary product liquid into the atmospheric distillation tower 17, and then closing the filter 14, the valve 15 and the feed pump 16; the DCS system controls the system temperature of the atmospheric distillation tower 17 to be 130 ℃, preferably between 90 ℃ and 150 ℃, after the atmospheric distillation is finished, the condenser 20 is started to remove unreacted acylation reagent and generated micromolecules in the atmospheric distillation tower 17, and a primary tower bottom output liquid of the p-methoxyacetophenone is obtained.
(5) In the atmospheric distillation process, when the concentration detector detects that the mass fraction of the p-methoxyacetophenone is not less than 90%, sending feedback information to a DCS (distributed control system), starting a valve 18 and a feed pump 19 by the DCS, introducing a first-stage tower bottom output liquid of an atmospheric distillation tower 17 into a vacuum distillation tower 23, and then closing the valve 18 and the feed pump 19; the DCS system controls the system temperature in the reduced pressure distillation tower 23 to be 80 ℃, preferably between 60 ℃ and 100 ℃, after the reduced pressure distillation is finished, the condenser 24 is started, a vacuum connecting pipe is connected to the reduced pressure liquid storage tank 27, and unreacted anisole in the reduced pressure distillation tower 23 is removed to obtain a secondary tower bottom output liquid of the p-methoxyacetophenone.
(6) In the process of reduced pressure distillation, when a concentration detector detects that the mass fraction of the p-methoxyacetophenone is not less than 95%, sending feedback information to a DCS (distributed control system), starting a valve 22 and a feed pump 25 by the DCS, introducing a secondary tower bottom product liquid into a tubular heat exchanger 26, controlling the temperature of the product liquid at an outlet of the tubular heat exchanger 26 to be 200 ℃, preferably between 120 ℃ and 220 ℃ by the DCS, heating the secondary tower bottom product liquid to 200 ℃ by the tubular heat exchanger 26, introducing the secondary tower bottom product liquid into a rectifying tower 28, and closing the valve 22 and the feed pump 25 by the DCS; and starting a feed pump 29 and a kettle-type reboiler 34, reboiling the produced liquid in the rectifying tower 28, and controlling the system temperature of the kettle-type reboiler 34 to 190 ℃ by a DCS (distributed control System), preferably between 120 and 220 ℃ to obtain the top distillate of the p-methoxyacetophenone.
In the rectification process, when the tower top distillate is introduced into the reflux tank 31, the concentration of the p-methoxyacetophenone is detected by a concentration detector, when the mass fraction is detected to be less than 99.5%, the DCS system opens the valve 32, and the tower top distillate enters the rectification tower 28 for rectification again; when the mass fraction of the p-methoxyacetophenone is detected to be more than or equal to 99.5 percent, the DCS system closes the valve 32, opens the valve 33, and the distillate at the tower top enters the crystallizer 36.
(7) And (3) introducing the distillate at the tower top into a crystallizer, cooling and crystallizing, and separating the p-methoxyacetophenone to obtain pure white crystals.
The overhead distillate in the rectifying tower 28 enters a crystallizer 36, the crystallizer 36 starts cooling circulation to cool and crystallize the overhead distillate, the temperature of the crystallizer is controlled by a DCS system to be 3 ℃, preferably between-10 ℃ and 10 ℃, and finally, the p-methoxyacetophenone is crystallized and separated to obtain pure white crystals.
Example 1:
the temperature of an anisole batching tank 3 is preheated to 60 ℃, the temperature of an acylation reagent batching tank 4 is preheated to 50 ℃, the temperature of a first reaction kettle 8 is preheated to 80 ℃, and the temperature of a second reaction kettle 13 is preheated to 100 ℃ under the control of a DCS system; the temperature in the atmospheric distillation tower 17 was preheated to 130 deg.C, the temperature in the vacuum distillation tower 23 was preheated to 80 deg.C, and the temperature in the rectifying tower 28 was preheated to 200 deg.C.
162g of anisole, 78g of acetyl chloride and ZnAl in the first reaction kettle 82O415.6g of catalyst charge and ZnAl in the second reaction kettle 132O47.8g of catalyst is fed; the yield of the first-stage product liquid of the methoxy acetophenone is 65.86 percent, the yield of the second-stage product liquid of the methoxy acetophenone is 85.31 percent, the yield of the methoxy acetophenone is 93.18 percent after atmospheric distillation, the yield of the methoxy acetophenone is 96.80 percent after vacuum distillation, and the yield of the methoxy acetophenone is 99.76 percent after rectification.
Example 2:
unlike example 1, the temperature in the second reaction vessel 13 was controlled to 120 ℃ and other reaction conditions were kept constant. The yield of the first-stage product liquid p-methoxyacetophenone is 66.89%, the yield of the second-stage product liquid p-methoxyacetophenone is 89.15%, the yield of the p-methoxyacetophenone after atmospheric distillation is 94.20%, the yield of the p-methoxyacetophenone after vacuum distillation is 97.38%, and the yield of the p-methoxyacetophenone after rectification is 99.81%.
Example 3:
in contrast to example 1, the acylating agent was acetic anhydride, the charge of acetic anhydride was 102g, and the catalyst used in the first and second reaction vessels 8 and 13 was HPW/Fe2O3The amount of the feed was 20.4g and 10.2g, respectively, and the other reaction conditions were unchanged. To obtain a first-grade output liquid pairThe yield of methoxyacetophenone is 72.16%, the yield of p-methoxyacetophenone of secondary product is 86.05%, the yield of p-methoxyacetophenone after atmospheric distillation is 91.58%, the yield of p-methoxyacetophenone after vacuum distillation is 96.62%, and the yield of p-methoxyacetophenone after rectification is 99.80%.
Example 4:
unlike example 3, the temperature in the second reaction vessel 13 was 120 ℃ and other reaction conditions were unchanged. The yield of the first-stage product liquid p-methoxyacetophenone is 72.53%, the yield of the second-stage product liquid p-methoxyacetophenone is 89.86%, the yield of the p-methoxyacetophenone after atmospheric distillation is 92.50%, the yield of the p-methoxyacetophenone after vacuum distillation is 97.08%, and the yield of the p-methoxyacetophenone after rectification is 99.89%.
The continuous production equipment and the continuous production method for the methoxyacetophenone, provided by the invention, have the advantages that the raw materials adopted by the process only comprise anisole, an acylation reagent and a solid acid catalyst, the reaction is carried out at normal pressure, and the operation is simple and convenient; the method effectively solves the problems of the loss of the activity of the catalyst and the carbon deposition phenomenon, has short reaction time, and improves the repeated utilization rate of the catalyst; the continuous production method of the methoxyacetophenone has simple process, is easy to realize continuous and automatic production, and improves the industrial production efficiency of the methoxyacetophenone; the grain size distribution of the produced p-methoxyacetophenone is uniform, and the product quality is greatly improved.
It should be understood that the detailed description of the present invention is only for illustrating the present invention and is not limited by the technical solutions described in the embodiments of the present invention, and those skilled in the art should understand that the present invention can be modified or substituted equally to achieve the same technical effects; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (10)
1. A continuous production equipment for methoxyacetophenone is characterized by at least comprising:
the reaction unit comprises a first reaction kettle and a second reaction kettle connected in series with the first reaction kettle;
the batching unit is connected with an input pipeline of the reaction unit and comprises a first batching tank and a second batching tank which is connected with the first batching tank in parallel;
and the separation unit is connected with the output pipeline of the reaction unit and comprises a first distillation tower, a second distillation tower, a third distillation tower and a crystallizer which are sequentially connected in series.
2. The continuous production apparatus of p-methoxyacetophenone as set forth in claim 1,
first batching jar and second batching jar with be provided with first control valve and second control valve on the connecting pipeline between the first reation kettle respectively, first batching jar and second batching jar respectively through the insulating tube with first reation kettle links to each other.
3. The continuous production apparatus of p-methoxyacetophenone as set forth in claim 2,
the bottom of first reation kettle and second reation kettle is provided with the filter, be provided with third control valve and first charge pump on the connecting pipeline between first reation kettle and the second reation kettle, the second reation kettle with be provided with fourth control valve and second charge pump on the connecting pipeline between the first distillation column.
4. The continuous production apparatus of p-methoxyacetophenone as set forth in claim 3,
the first distillation tower is an atmospheric distillation tower, the second distillation tower is a vacuum distillation tower, the third distillation tower is a rectifying tower, a fifth control valve and a third feed pump are arranged on a connecting pipeline between the first distillation tower and the second distillation tower, a sixth control valve and a fourth feed pump are arranged on a connecting pipeline between the second distillation tower and the third distillation tower, and a heat exchanger is further arranged between the fourth feed pump and the third distillation tower.
5. The continuous production apparatus of p-methoxyacetophenone as set forth in claim 1,
the top of first distillation column is established ties in proper order and is had first condenser and ordinary pressure liquid storage pot, the top of second distillation column is established ties in proper order and is had second condenser and decompression liquid storage pot, third distillation column top is established ties in proper order and is had third condenser and reflux drum, reflux drum bottom end is connected through seventh valve, eighth valve respectively the third distillation column with the crystallizer, the third distillation column bottom is connected with cauldron formula reboiler through fifth charge pump.
6. The continuous production apparatus of p-methoxyacetophenone as set forth in claim 1,
the bottom of first batching jar, second batching jar, first reation kettle, second reation kettle, first distillation column, second distillation column, third distillation column and crystallizer sets up thermodetector respectively, thermodetector feeds back the temperature detection signal to the DCS system.
7. The continuous production apparatus of p-methoxyacetophenone as set forth in claim 1,
and concentration detectors are respectively arranged at the bottom ends of the first reaction kettle, the second reaction kettle, the first distillation tower and the second distillation tower and at the top end of the third distillation tower, and the concentration detectors feed concentration detection signals back to the DCS.
8. A continuous production method of methoxyacetophenone, which is applied to the continuous production equipment of methoxyacetophenone as claimed in any one of claims 1 to 7, and is characterized by comprising the following steps:
(1) preparing an anisole hot solution at the temperature of 60-80 ℃ in a first preparation tank, and preparing an acylation reagent hot solution at the temperature of 40-50 ℃ in a second preparation tank;
(2) introducing the prepared anisole hot solution and the prepared acylation reagent hot solution into a first reaction kettle, and obtaining a first-stage output liquid with the yield of the p-methoxyacetophenone not less than 60 percent after first-stage reaction;
(3) introducing the primary output liquid into a second reaction kettle, and obtaining a secondary output liquid with the yield of the p-methoxyacetophenone not less than 85% after secondary reaction;
(4) introducing the secondary output liquid into a first distillation tower, and obtaining a primary tower bottom output liquid with the mass fraction of the p-methoxyacetophenone not less than 90% after primary distillation;
(5) introducing the primary tower bottom product liquid into a second distillation tower, and obtaining a secondary tower bottom product liquid with the mass fraction of p-methoxyacetophenone not less than 95% after secondary distillation;
(6) introducing the secondary tower bottom product into a third distillation tower, and performing three-stage distillation to obtain tower top distillate with the mass fraction of p-methoxyacetophenone not less than 99.5%;
(7) and (3) introducing the distillate at the tower top into a crystallizer, cooling and crystallizing, and separating the p-methoxyacetophenone to obtain pure white crystals.
9. The continuous production method of methoxyacetophenone according to claim 8, wherein the temperature in the first reaction vessel is controlled to 40 ℃ to 80 ℃ and the temperature in the second reaction vessel is controlled to 80 ℃ to 120 ℃.
10. The continuous production method of p-methoxyacetophenone according to claim 8, wherein the temperature in the first distillation column is controlled to be between 90 ℃ and 150 ℃, the temperature in the second distillation column is controlled to be between 60 ℃ and 100 ℃, the temperature in the third distillation column is controlled to be between 120 ℃ and 220 ℃, and the temperature in the crystallizer is controlled to be between-10 ℃ and 10 ℃.
Priority Applications (1)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2018056864A1 (en) * | 2016-09-22 | 2018-03-29 | Общество с ограниченной ответственностью "СИНТОН" | Catalyst, method for using same, and installation for hydrogen-free dewaxing of a hydrocarbon feedstock |
| CN108727172A (en) * | 2018-06-25 | 2018-11-02 | 南京师范大学 | A kind of process for catalytic synthesis of acetanisole |
| CN110655461A (en) * | 2019-10-24 | 2020-01-07 | 江苏沐阳智骅能源科技有限公司 | DMS esterification feed serialization system |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018056864A1 (en) * | 2016-09-22 | 2018-03-29 | Общество с ограниченной ответственностью "СИНТОН" | Catalyst, method for using same, and installation for hydrogen-free dewaxing of a hydrocarbon feedstock |
| CN108727172A (en) * | 2018-06-25 | 2018-11-02 | 南京师范大学 | A kind of process for catalytic synthesis of acetanisole |
| CN110655461A (en) * | 2019-10-24 | 2020-01-07 | 江苏沐阳智骅能源科技有限公司 | DMS esterification feed serialization system |
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