CN112358385B - Continuous production equipment and production method for p-methoxy acetophenone - Google Patents
Continuous production equipment and production method for p-methoxy acetophenone Download PDFInfo
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- CN112358385B CN112358385B CN202011243218.1A CN202011243218A CN112358385B CN 112358385 B CN112358385 B CN 112358385B CN 202011243218 A CN202011243218 A CN 202011243218A CN 112358385 B CN112358385 B CN 112358385B
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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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- C07C45/81—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 production method of p-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 anisole hot solution and acylation reagent hot solution prepared in a batching 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 crystals of the p-methoxyacetophenone. The continuous production equipment and the production method of the p-methoxy acetophenone can effectively solve the problems of catalyst activity loss and carbon deposition, and the recycling 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 production method of p-methoxy acetophenone.
Background
The p-methoxyacetophenone is a white crystal, has the fragrance of haw flower and similar anisaldehyde, is mainly used for synthesizing medicines and spices, for example, is a key intermediate of puerarin and raloxifene, is commonly used in advanced cosmetics and soap essence, has high stability in soap, can also be used as fruit food essence, and has wide market and development prospect.
Friedel-Crafts acylation reaction is an important way for synthesizing p-methoxyacetophenone, and the typical preparation method is to take anisole as a raw material, acetyl chloride or acetic anhydride as an acylating agent, and prepare the p-methoxyacetophenone through Friedel-Crafts acylation reaction by adopting a solid acid catalyst.
In the traditional process, lewis acid (such as ZnCl2 and AlCl 3) is often adopted as a catalyst, the required catalyst amount is large, the reaction temperature is high, the yield is low, and the homogeneous catalytic separation is difficult, the energy consumption is high, a large amount of waste metal and acid sludge are easy to generate, so that equipment corrosion is serious in the production process, and environmental pollution is caused.
The pure heteropolyacid is used as a catalyst by the university of petrochemical industry, namely Xu Mei, and the p-methoxy acetophenone is synthesized by acylation reaction of anisole and acetic anhydride, and the modified phosphotungstic acid is used as a catalyst, so that the yield of the product can reach 52.9 percent. However, in the process, the phosphotungstic acid is completely dissolved in the reaction liquid and is difficult to recycle, and carbon deposition is very easy to coke in the reaction process, so that the activity of the catalyst is influenced.
Chen Pingdeng of university of northeast studied that p-methoxyacetophenone is selectively produced by catalyzing Friedel-Crafts acylation reaction of anisole and acetic anhydride under the condition of no solvent by using H beta zeolite as a catalyst, carbon deposition is easy to occur in the reaction process of the H beta zeolite molecular sieve used by the method, and competing adsorption of products and substrates occurs on the surface of the catalyst, so that the activity of the catalyst is reduced, the application of the catalyst is restricted, and the adsorption balance is difficult to control.
In the above method, various problems are intermittently reflected: (1) The carbon deposition phenomenon is serious, so that the activity of the catalyst is rapidly reduced; (2) the loss of active components is serious, and the repeated use rate is reduced; (3) The batch reaction is difficult to reach completion, and the reaction rate is influenced in the later stage of the reaction; (4) The scale is small, the yield is low, and the catalyst removal problem exists simultaneously compared with other processes, so that the yield and the purity are also poor.
Disclosure of Invention
The invention aims to provide continuous production equipment and a production method of p-methoxyacetophenone, which solve the problems of rapid reduction of catalyst activity, serious loss of active components, reduction of reuse rate and the like caused by carbon deposition generated by the conventional intermittent production process.
In order to achieve the above purpose, the invention provides a continuous production device of p-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 the input pipeline of the reaction unit and comprises a first batching tank and a second batching tank connected with the first batching tank in parallel;
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, the first batching jar and the second batching jar with be provided with first control valve and second control valve respectively on the connecting line between the first reation kettle, first batching jar and second batching jar pass through the heat preservation pipeline respectively with first reation kettle links to each other.
Preferably, the bottom ends of the first reaction kettle and the second reaction kettle are provided with filters, a connecting pipeline between the first reaction kettle and the second reaction kettle is provided with a third control valve and a first feed pump, and a connecting pipeline between the second reaction kettle and the first distillation tower is provided with a fourth control valve and a second feed pump.
Preferably, the first distillation tower is an atmospheric distillation tower, the second distillation tower is a reduced pressure 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.
Preferably, the top end of the first distillation tower is sequentially connected with a first condenser and a normal pressure liquid storage tank in series, the top end of the second distillation tower is sequentially connected with a second condenser and a decompression liquid storage tank in series, the top end of the third distillation tower is sequentially connected with a third condenser and a reflux tank in series, the bottom end of the reflux tank is respectively connected with the third distillation tower and the crystallizer through a seventh valve and an eighth valve, and the bottom end of the third distillation tower is connected with a kettle type reboiler through a fifth feed 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 back concentration detection signals to the DCS system.
The invention also provides a p-methoxyacetophenone continuous production method which is applied to the p-methoxyacetophenone continuous production equipment and mainly comprises the following steps:
(1) Preparing anisole hot solution with the temperature of 60-80 ℃ in a first material mixing tank, and preparing acylating reagent hot solution with the temperature of 40-50 ℃ in a second material mixing tank;
(2) Introducing the prepared anisole hot solution and the acylation reagent hot solution into a first reaction kettle, and obtaining a first-stage output liquid with the yield of the p-methoxyacetophenone not lower than 60% after a first-stage reaction;
(3) Introducing the first-stage output liquid into a second reaction kettle, and obtaining a second-stage output liquid with the yield of the p-methoxyacetophenone not lower than 85% after a second-stage reaction;
(4) Introducing the second-stage effluent into a first distillation tower, and obtaining a first-stage tower bottom effluent with the mass fraction of p-methoxyacetophenone not less than 90% after first-stage distillation;
(5) Introducing the first-stage tower bottom effluent into a second distillation tower, and obtaining a second-stage tower bottom effluent with the mass fraction of p-methoxyacetophenone not less than 95% after second-stage distillation;
(6) Introducing the second-stage tower bottom product liquid into a third distillation tower, and obtaining tower top distillate with the mass fraction of the p-methoxyacetophenone not less than 99.5% after three-stage distillation;
(7) Introducing the tower top distillate into a crystallizer, cooling and crystallizing, and separating out 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 p-methoxyacetophenone continuous production equipment and method provided by the invention have the advantages that the raw materials adopted in the process are 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 problems of catalyst activity loss and carbon deposition are effectively solved, the reaction time is short, and the recycling rate of the catalyst is improved; the continuous production method of the p-methoxyacetophenone has simple process, is easy to realize continuous and automatic production, and improves the industrial production efficiency of the p-methoxyacetophenone; the produced p-methoxy acetophenone has uniform grain size distribution, 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 that are needed 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 other drawings may be obtained according to these drawings for a person skilled in the art.
FIG. 1 is a schematic structural diagram of a p-methoxyacetophenone continuous production device;
legend description: 1. 2, 6, 12 and 35 are motors; 3 is anisole batching tank; 4 is an acylating agent formulation 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 column; 28 is a rectifying tower; 36 is a crystallizer; 5. 7, 10, 15, 18, 22, 32, 33 are valves; 9. 14 is a filter; 11. 16, 19, 25, 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-reducing liquid storage tank; 31 is a reflux drum; 34 is a kettle reboiler.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments.
Fig. 1 is a schematic structural diagram of p-methoxyacetophenone continuous production equipment.
The continuous production equipment of the 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 acylating agent batching tank 4 which are connected in parallel and are respectively used for preparing anisole solution and acylating agent 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 connected with an anisole preparation tank 3 and an acylating agent preparation tank 4 through a valve 5 and a valve 7 respectively; the separation unit is connected with an output pipeline of the second reaction kettle 13, and comprises an atmospheric distillation tower 17, a vacuum distillation tower 23, a rectifying tower 28 and a crystallizer 36.
The top of the first reaction kettle 8 is connected with the batching unit through a heat-preserving pipeline, a filter 9 and a valve 10 are arranged at the outlet of the bottom of the first reaction kettle, the valve 10 is sequentially connected with the upper ends of a feed pump 11 and a second reaction kettle 13 through heat-preserving pipelines, a filter 14 and a valve 15 are arranged at the outlet of the bottom of the second reaction kettle 13, and the valve 15 is sequentially connected with the feed pump 16 and an atmospheric distillation tower 17 through heat-preserving pipelines.
A valve 18 and a feed pump 19 are arranged at the outlet of the bottom end of the atmospheric distillation tower 17, and the feed pump 19 is connected with a vacuum 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 a constant-pressure liquid storage tank 21. The outlet of the bottom end of the vacuum distillation tower 23 is provided with a valve 22 and a feed pump 25, the feed pump 25 is connected with a tubular heat exchanger 26 through a heat-preserving pipeline, and the tubular heat exchanger 26 is connected with a rectifying tower 28 through a heat-preserving pipeline; the top end of the vacuum distillation tower 23 is connected with a condenser 24, and the condenser 24 is connected with a vacuum liquid storage tank 27 connected with a vacuum connecting pipe. The bottom outlet of rectifying tower 28 is provided with charge pump 29, and charge pump 29 links to each other with kettle type reboiler 34 through the heat preservation pipeline, and the reboiling feed liquid that kettle type reboiler 34 flowed gets into rectifying tower 28 again through the heat preservation pipeline, and rectifying tower 28 top links to each other has condenser 30, and condenser 30 links to each other with reflux drum 31, and reflux drum 31 bottom outlet is provided with valve 32 and valve 33, and valve 32 is connected with rectifying tower 28, and valve 33 is connected with crystallizer 36.
The anisole batching jar 3, the acylating agent batching jar 4, the first reation kettle 8, the second reation kettle 13, the top of crystallizer respectively correspond to be connected with motor 1, motor 2, motor 6, motor 12 and motor 35.
Valves, motors, feed pumps and heating medium devices in the connection pipelines of the batching unit, the reaction unit and the separation unit are controlled by a distributed control system (Distributed Control System, DCS for short).
Preferably, temperature detectors are arranged at the bottom of the anisole preparation tank 3, the bottom of the acylating agent preparation 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 vacuum distillation tower 23, the bottom of the rectifying tower 28 and the bottom of the crystallizer 36, and are used for detecting the temperature of the internal liquid and feeding back a temperature detection signal 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 end of the rectifying tower 28 and the tail of the condenser 30 are all connected with concentration detectors, and the concentration detectors are used for detecting the concentration of the p-methoxy acetophenone and feeding back a concentration detection signal to the DCS system.
The invention also provides a continuous production method of the p-methoxyacetophenone, which is applied to the continuous production equipment production of the p-methoxyacetophenone provided by any embodiment, and mainly comprises the following steps:
(1) Preparing an anisole hot solution with the temperature of 60-80 ℃ in an anisole preparation tank 3, preparing an acylating agent hot solution with the temperature of 40-50 ℃ in an acylating agent preparation tank 4, wherein the molar ratio of the anisole hot solution to the acylating agent hot solution is 1.5:1.
(2) The DCS system controls to open the valve 5 and the valve 7, the prepared anisole hot solution and the acylation reagent hot solution are introduced into the first reaction kettle 8, the DCS system controls the reaction temperature in the first reaction kettle 8 to be 80 ℃, preferably between 40 ℃ and 80 ℃, and the first-stage product liquid of the p-methoxyacetophenone is obtained after the first-stage reaction.
(3) In a first reaction kettle 8, when the concentration detector detects that the yield of the p-methoxyacetophenone is not lower than 60%, feedback information is sent to a DCS system, after the DCS system receives the feedback signal, a filter 9, a valve 10 and a feed pump 11 are opened, primary effluent is introduced into a second reaction kettle 13, and then the filter 9, the valve 10 and the feed pump 11 are closed; the DCS system controls the reaction temperature in the second reaction kettle 13 to be 100 ℃, preferably 80-120 ℃, so as to obtain a second-stage output liquid of the yield of the p-methoxyacetophenone.
(4) In the second reaction kettle 13, when the concentration detector detects that the yield of the p-methoxyacetophenone is not lower than 85%, feedback information is sent to a DCS system, the DCS system starts a filter 14, a valve 15 and a feed pump 16, secondary effluent is introduced into an atmospheric distillation tower 17, and then the filter 14, the valve 15 and the feed pump 16 are closed; the DCS system controls the system temperature of the atmospheric distillation tower 17 to be 130 ℃, preferably 90-150 ℃, and after the atmospheric distillation is completed, the condenser 20 is started to remove unreacted acylating reagent and generated small molecules in the atmospheric distillation tower 17, so as to obtain a first-stage tower bottom product liquid of the p-methoxyacetophenone.
(5) In the normal pressure distillation process, when the concentration detector detects that the mass fraction of the p-methoxyacetophenone is not less than 90%, feedback information is sent to a DCS system, the DCS system opens a valve 18 and a feed pump 19, a first-stage tower bottom effluent of the normal pressure distillation tower 17 is introduced into a reduced pressure distillation tower 23, and then the valve 18 and the feed pump 19 are closed; 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 completed, a condenser 24 is started, a vacuum connecting pipe is connected to a reduced pressure liquid storage tank 27, and unreacted anisole in the reduced pressure distillation tower 23 is removed, so that a second-stage tower bottom product liquid of the p-methoxyacetophenone is obtained.
(6) In the reduced pressure distillation process, when the concentration detector detects that the mass fraction of the p-methoxyacetophenone is not less than 95%, feedback information is sent to a DCS system, the DCS system opens a valve 22 and a feed pump 25, a secondary tower bottom effluent is introduced into a tubular heat exchanger 26, the DCS system controls the temperature of the effluent at the outlet of the tubular heat exchanger 26 to be 200 ℃, preferably between 120 and 220 ℃, the tubular heat exchanger 26 heats the secondary tower bottom effluent to 200 ℃ and then introduces the heated effluent into a rectifying tower 28, and the DCS system closes the valve 22 and the feed pump 25; the feed pump 29 and the kettle reboiler 34 are started to reboil the effluent in the rectifying tower 28, and the DCS system controls the system temperature of the kettle reboiler 34 to be 190 ℃, preferably between 120 ℃ and 220 ℃, so as to obtain the overhead distillate of the p-methoxyacetophenone.
In the rectification process, when the tower top distillate is introduced into a reflux tank 31, a concentration detector detects the concentration of the p-methoxyacetophenone, and when the mass fraction is detected to be less than 99.5%, a DCS system opens a valve 32, and the tower top distillate enters a 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%, the DCS system closes the valve 32, opens the valve 33, and the tower top distillate enters the crystallizer 36.
(7) Introducing the tower top distillate into a crystallizer, cooling and crystallizing, and separating out the p-methoxyacetophenone to obtain pure white crystals.
The top distillate in the rectifying tower 28 enters a crystallizer 36, the crystallizer 36 starts a cooling cycle, the top distillate is cooled and crystallized, the temperature of the crystallizer is controlled to be 3 ℃, preferably between-10 ℃ and 10 ℃ by a DCS system, and finally the p-methoxyacetophenone is crystallized and separated to obtain pure white crystals.
Example 1:
preheating the anisole preparation tank 3 to 60 ℃ and the acylating agent preparation tank 4 to 50 ℃, preheating the first reaction kettle 8 to 80 ℃ and preheating the second reaction kettle 13 to 100 ℃ through DCS control; the temperature in the atmospheric distillation column 17 was preheated to 130 ℃, the temperature in the vacuum distillation column 23 was preheated to 80 ℃, and the temperature in the rectification column 28 was preheated to 200 ℃.
162g of anisole and 78g of acetyl chloride, znAl in a first reaction kettle 8 2 O 4 15.6g of catalyst and ZnAl in a second reaction kettle 13 2 O 4 7.8g of catalyst; obtain the first-order output liquid p-methoxyThe yield of acetophenone is 65.86%, the yield of p-methoxyacetophenone from the second-stage effluent is 85.31%, the yield of p-methoxyacetophenone is 93.18% after atmospheric distillation, the yield of p-methoxyacetophenone is 96.80% after vacuum distillation, and the yield of p-methoxyacetophenone is 99.76% after rectification.
Example 2:
unlike example 1, the temperature in the second reaction vessel 13 was controlled to 120℃and the other reaction conditions were maintained. The yield of the first-grade output liquid p-methoxyacetophenone is 66.89%, the yield of the second-grade output liquid p-methoxyacetophenone is 89.15%, the yield of the p-methoxyacetophenone after normal pressure distillation is 94.20%, the yield of the p-methoxyacetophenone after reduced pressure distillation is 97.38%, and the yield of the p-methoxyacetophenone after rectification is 99.81%.
Example 3:
unlike example 1, the acylating agent was acetic anhydride, the acetic anhydride charge was 102g, and the catalyst used in the first reactor 8 and the second reactor 13 was HPW/Fe 2 O 3 The feeding amounts are 20.4g and 10.2g respectively, and other reaction conditions are unchanged. The yield of the first-grade output liquid p-methoxyacetophenone is 72.16 percent, the yield of the second-grade output liquid p-methoxyacetophenone is 86.05 percent, the yield of the p-methoxyacetophenone after normal pressure distillation is 91.58 percent, the yield of the p-methoxyacetophenone after reduced pressure distillation is 96.62 percent, and the yield of the p-methoxyacetophenone after rectification is 99.80 percent.
Example 4:
unlike example 3, the temperature in the second reactor 13 was 120℃and the other reaction conditions were unchanged. The yield of the first-grade output liquid p-methoxyacetophenone is 72.53 percent, the yield of the second-grade output liquid p-methoxyacetophenone is 89.86 percent, the yield of the p-methoxyacetophenone after normal pressure distillation is 92.50 percent, the yield of the p-methoxyacetophenone after reduced pressure distillation is 97.08 percent, and the yield of the p-methoxyacetophenone after rectification is 99.89 percent.
The p-methoxyacetophenone continuous production equipment and method provided by the invention have the advantages that the raw materials adopted in the process are 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 problems of catalyst activity loss and carbon deposition are effectively solved, the reaction time is short, and the recycling rate of the catalyst is improved; the continuous production method of the p-methoxyacetophenone has simple process, is easy to realize continuous and automatic production, and improves the industrial production efficiency of the p-methoxyacetophenone; the produced p-methoxy acetophenone has uniform grain size distribution, and the product quality is greatly improved.
It should be understood that the foregoing detailed description of the present invention is provided for illustration only and is not limited to the technical solutions described in the embodiments of the present invention, and those skilled in the art should understand that the present invention may be modified or substituted for the same technical effects; as long as the use requirement is met, the invention is within the protection scope of the invention.
Claims (9)
1. The p-methoxyacetophenone continuous production method is characterized in that p-methoxyacetophenone is produced in p-methoxyacetophenone continuous production equipment, and the p-methoxyacetophenone continuous production equipment 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 the input pipeline of the reaction unit and comprises a first batching tank and a second batching tank connected with the first batching tank in parallel;
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;
the p-methoxyacetophenone continuous production method comprises the following steps:
(1) Preparing anisole hot solution with the temperature of 60-80 ℃ in a first material mixing tank, and preparing acylating reagent hot solution with the temperature of 40-50 ℃ in a second material mixing tank;
(2) Introducing the prepared anisole hot solution and the acylation reagent hot solution into a first reaction kettle, and obtaining a first-stage output liquid with the yield of the p-methoxyacetophenone not lower than 60% after a first-stage reaction;
(3) Introducing the first-stage output liquid into a second reaction kettle, and obtaining a second-stage output liquid with the yield of the p-methoxyacetophenone not lower than 85% after a second-stage reaction;
(4) Introducing the second-stage effluent into a first distillation tower, and obtaining a first-stage tower bottom effluent with the mass fraction of p-methoxyacetophenone not less than 90% after first-stage distillation;
(5) Introducing the first-stage tower bottom effluent into a second distillation tower, and obtaining a second-stage tower bottom effluent with the mass fraction of p-methoxyacetophenone not less than 95% after second-stage distillation;
(6) Introducing the second-stage tower bottom product liquid into a third distillation tower, and obtaining tower top distillate with the mass fraction of the p-methoxyacetophenone not less than 99.5% after three-stage distillation;
(7) Introducing the tower top distillate into a crystallizer, cooling and crystallizing, and separating out the p-methoxyacetophenone to obtain pure white crystals.
2. The continuous production method of p-methoxyacetophenone as claimed in claim 1, wherein the temperature in the first reaction vessel is controlled to be between 40 ℃ and 80 ℃ and the temperature in the second reaction vessel is controlled to be 80 DEG C
-120 ℃.
3. The continuous production process of p-methoxyacetophenone as claimed in claim 1, 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 ℃.
4. The continuous production method of p-methoxyacetophenone according to claim 1, wherein a first control valve and a second control valve are respectively arranged on connecting pipelines between the first material mixing tank and the second material mixing tank and the first reaction kettle, and the first material mixing tank and the second material mixing tank are respectively connected with the first reaction kettle through heat insulation pipelines.
5. The continuous production method of p-methoxyacetophenone according to claim 4, wherein filters are arranged at the bottom ends of the first reaction kettle and the second reaction kettle, a third control valve and a first feed pump are arranged on a connecting pipeline between the first reaction kettle and the second reaction kettle, and a fourth control valve and a second feed pump are arranged on a connecting pipeline between the second reaction kettle and the first distillation tower.
6. The continuous production method of p-methoxyacetophenone according to claim 5, wherein 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 also arranged between the fourth feed pump and the third distillation tower.
7. The continuous production method of p-methoxyacetophenone according to claim 1, wherein a first condenser and a normal pressure liquid storage tank are sequentially connected in series to the top end of the first distillation tower, a second condenser and a decompression liquid storage tank are sequentially connected in series to the top end of the second distillation tower, a third condenser and a reflux tank are sequentially connected in series to the top end of the third distillation tower, the bottom ends of the reflux tanks are respectively connected with the third distillation tower and the crystallizer through a seventh valve and an eighth valve, and the bottom end of the third distillation tower is connected with a kettle type reboiler through a fifth feed pump.
8. The continuous production method of p-methoxyacetophenone according to claim 1, wherein temperature detectors are respectively arranged at bottoms of the first material distribution tank, the second material distribution 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 back temperature detection signals to the DCS system.
9. The continuous production method of p-methoxyacetophenone according to claim 1, wherein concentration detectors are respectively arranged at the bottom ends of the first reaction kettle, the second reaction kettle, the first distillation tower, the second distillation tower and the top end of the third distillation tower, and the concentration detectors feed back concentration detection signals to the DCS system.
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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 |
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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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