CN219482688U - Reaction device for continuously producing 2, 3-pentanedione - Google Patents
Reaction device for continuously producing 2, 3-pentanedione Download PDFInfo
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- CN219482688U CN219482688U CN202320805326.6U CN202320805326U CN219482688U CN 219482688 U CN219482688 U CN 219482688U CN 202320805326 U CN202320805326 U CN 202320805326U CN 219482688 U CN219482688 U CN 219482688U
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Abstract
The utility model discloses a reaction device for continuously producing 2, 3-pentanedione, and relates to the technical field of continuous reaction devices. The reaction device comprises a continuous reaction device, an oil-water separator, a continuous desolventizing tower and a condenser which are sequentially connected. The continuous reaction device is a customized tubular reactor, the lining is made of corrosion-resistant materials, and the continuous reaction device comprises four parts connected in sequence: the device comprises a material mixing section, a heating reaction section, a reaction liquid cooling section and an extraction section. The raw materials can continuously react in the tubular reactor, so that continuous production of 2, 3-pentanedione is realized, the production efficiency and the product stability are improved, the safety is high, the labor cost is reduced, and the occupied area of continuous flow equipment is reduced. Compared with kettle type reaction, the tubular reaction reduces the reaction time, shortens the high-temperature time of raw materials and products, reduces the deterioration phenomenon of the raw materials and the products, ensures that the products are more stable, and improves the reaction yield and the production efficiency.
Description
Technical Field
The utility model relates to the technical field of continuous reaction devices, in particular to a reaction device for continuously producing 2, 3-pentanedione.
Background
2, 3-pentanedione is a edible spice which is yellow green oily liquid, has sweet white, cream and caramel fragrance and has nut bottom fragrance. Can be used as spice of food essence, gelatin hardener, photo binder, etc., and can be used as synthetic raw material of 2-ethyl-3-methyl pyrazine and imidazole, and also can be used as intermediate for preparing medicine, antiseptic, bactericide, etc.
There are many methods for synthesizing 2, 3-pentanedione, among which the synthesis of 2, 3-pentanedione using hydroxyacetone and paraldehyde as raw materials is the most commonly used synthesis method. The natural sources of hydroxyacetone are wide, and paraldehyde is easily available, and the route is the first choice. The current device for synthesizing 2, 3-pentanedione by adopting the route is batch reaction equipment, and specifically comprises a conventional reaction kettle: and (3) putting raw materials into a synthesis reaction kettle, reacting for several hours until the conversion of the raw materials is completed, cooling, transferring the materials to another kettle for extraction, pumping the separated organic phase into a desolventizing kettle, cooling to discharge a crude product after solvent is stripped, and rectifying the crude product in a rectifying tower. The intermittent reaction kettle is used for preparing the 2, 3-pentanedione, so that the operation is complex, the reaction time is long, more manpower is required, and the labor cost is high. Because the thermal stability of the raw materials and the products is poor, the high-temperature reaction time is too long, the raw materials and the products are deteriorated, and the batch kettle reaction yield is not high.
Disclosure of Invention
Aiming at the defects existing in the prior art, the utility model aims to provide a reaction device for continuously producing 2, 3-pentanedione, raw materials can continuously react in the continuous reaction device, so that the continuous production of the 2, 3-pentanedione is realized, and the production efficiency and the reaction yield are improved.
In order to achieve the above object, the present utility model is realized by the following technical scheme:
the utility model provides a reaction device for continuously producing 2, 3-pentanedione, which comprises a continuous reaction device, an oil-water separator, a continuous desolventizing tower and a condenser which are sequentially connected.
The continuous reaction device comprises four parts which are connected in sequence: the device comprises a material mixing section, a heating reaction section, a reaction liquid cooling section and an extraction section.
And the outlet of the extraction section is connected with a blanking pipe of the oil-water separator.
And an organic phase liquid outlet of the oil-water separator is communicated with a feed pipe D of the continuous desolventizing tower.
The bottom of the continuous desolventizing tower is provided with a discharge port, and the top of the continuous desolventizing tower is provided with a riser which is connected to a condenser.
The continuous reaction apparatus is a tubular reactor.
The front end of the material mixing section is connected with an anti-corrosion metering pump A, a feed pipe B connected with the anti-corrosion metering pump B extends into the continuous reaction device from the side surface of the material mixing section, and a mixer B is arranged at the material mixing section behind the opening of the feed pipe B.
The rear part of the material mixing section is provided with a heating reaction section, the outer side of the material mixing section is provided with a heating sleeve B, and the heating reaction section is uniformly distributed with temperature sensors and pressure sensors.
The rear part of the heating reaction section is a reaction liquid cooling section, the outer side of the heating reaction section is a cooling sleeve B, circulating cooling water flows in the cooling sleeve B, and a temperature sensor is arranged in the reaction liquid cooling section.
The rear of the reaction liquid cooling section is an extraction section, a feeding pipe C connected with a metering pump C extends into the continuous reaction device from the side surface of the extraction section, and a mixer C is arranged in the extraction section behind the opening of the feeding pipe C.
The oil-water separator is vertically arranged, the discharging pipe is inserted into the middle position of the oil-water separator, an organic phase liquid outlet is arranged on the side face of the oil-water separator, and the organic phase liquid outlet is communicated with a feeding pipe D of the continuous desolventizing tower.
And (3) adjusting the wastewater flow of the regulating valve A and the organic phase extraction flow of the regulating valve B according to the feeding flow rates of the anti-corrosion metering pump A and the anti-corrosion metering pump B and the feeding flow rate of the extraction solvent of the metering pump C.
The continuous desolventizing tower is vertically arranged, a heating sleeve C is arranged outside a feeding pipe D, a heating device is arranged below the inner part of the desolventizing tower, a discharging hole is arranged at the bottom of the desolventizing tower, a gas lifting pipe is arranged at the top of the continuous desolventizing tower and is connected to a condenser, temperature sensors and pressure sensors are distributed and arranged in the gas lifting pipe, and a solvent recovery hole is arranged at the bottom of the condenser.
The beneficial effects of the utility model are as follows:
1. the continuous flow reaction device is used for producing the 2, 3-pentanedione, can realize continuous production, is easy to operate and implement, has low energy consumption and high safety, reduces labor cost and reduces occupied area of continuous flow equipment.
2. Compared with kettle type reaction, the tubular reaction can reduce the reaction time, shorten the high-temperature time of raw materials and products, reduce the deterioration phenomenon of the raw materials and the products, lead the products to be more stable and improve the reaction yield and the production efficiency.
Drawings
The accompanying drawings, which are included to provide a further understanding of the utility model and are incorporated in and constitute a part of this specification, illustrate embodiments of the utility model and together with the description serve to explain the utility model.
In the figure: the mutual spacing or dimensions are exaggerated for the purpose of showing the positions of the various parts, and the schematic illustrations are used for illustration only.
FIG. 1 is a schematic view of a continuous reaction apparatus in the examples.
FIG. 2 is a schematic diagram of an oil-water separator in an embodiment.
FIG. 3 is a schematic diagram of a continuous desolventizing column and condenser in an example.
Wherein 1, an anti-corrosion metering pump A,2, an anti-corrosion metering pump B,3, a feed pipe B,4, a mixer B,5, a heating sleeve B,6, a temperature sensor, 7, a pressure sensor, 8, a cooling sleeve B,9, a temperature sensor, 10, a metering pump C,11, a feed pipe C,12, a mixer C,13, an oil-water separator, 14 and a blanking pipe, 15, regulating valves A,16, flow meters A,17, organic phase liquid outlets 18, regulating valves B,19, flow meters B,20, a continuous desolventizing tower, 21, a feed pipe D,22, a heating sleeve C,23, a heating device, 24, a riser, 25, a condenser, 26, a discharge outlet, 27, a temperature sensor, 28, a pressure sensor, 29 and a solvent recovery port.
Detailed Description
The utility model will be further described with reference to the drawings and examples.
Example 1:
the utility model provides a reaction device for continuously producing 2, 3-pentanedione, which comprises a continuous reaction device, an oil-water separator, a continuous desolventizing tower and a condenser which are sequentially connected.
The continuous reaction device is a customized tubular reactor, the lining is made of corrosion-resistant materials, and the continuous reaction device comprises four parts which are sequentially connected: the device comprises a material mixing section, a heating reaction section, a reaction liquid cooling section and an extraction section.
The tubular reactor is a carbon steel tube and is lined with polytetrafluoroethylene or enamel.
Or the tubular reactor is a stainless steel tube, lined with polytetrafluoroethylene or enamel.
The total length of the tubular reactor is 100-500 m, and the inner diameter is 2cm-10cm.
As shown in fig. 1, the front end of the material mixing section is connected with an anti-corrosion metering pump A1, a feed pipe B3 connected with an anti-corrosion metering pump B2 extends into the tubular reactor from the side surface of the material mixing section, the outer diameter of the feed pipe B3 is smaller than the inner diameter of the material mixing section, the opening part of the tail end of the feed pipe B3 is in conical shrinkage, the direction of the conical tail end is the same as the material flowing direction, and a mixer B4 is arranged in the material mixing section behind the opening of the feed pipe B.
The anti-corrosion metering pump A1 is used for feeding a hydroxyacetone dilute hydrochloric acid solution, and the anti-corrosion metering pump B2 is used for feeding paraldehyde; the inner diameter of the feed pipe B3 is 1-6cm, the length of the conical part at the tail end is 3-12cm, the conical part is perforated, and the aperture is 2-5mm; the material of the feeding pipe B3 is polytetrafluoroethylene.
The mixer B4 is a static mixer, so that the materials are fully mixed.
The rear part of the material mixing section is provided with a heating reaction section, the outer side of the material mixing section is provided with a heating sleeve B5, and the heating reaction section is uniformly distributed with a temperature sensor 6 and a pressure sensor 7, so that the material temperature and the pressure in the reaction section can be monitored in real time.
Hot water circularly flows in the heating sleeve B5, and the reaction temperature of materials in the heating reaction section is kept stable.
The rear part of the heating reaction section is a reaction liquid cooling section, the outer side of the heating reaction section is a cooling sleeve B8, circulating cooling water flows in the cooling sleeve B8, and a temperature sensor 9 is arranged in the reaction liquid cooling section.
The rear of the reaction liquid cooling section is an extraction section, a feeding pipe C11 connected with a metering pump C10 extends into the tubular reactor from the side surface of the extraction section, the outer diameter of the feeding pipe C11 is smaller than the inner diameter of the extraction section, the opening part of the tail end is in conical shrinkage, the direction of the conical tail end is the same as the material flowing direction, and a mixer C12 is arranged in the extraction section behind the opening of the feeding pipe C.
The metering pump C10 is used for feeding an extraction solvent, the inner diameter of the feeding pipe C11 is 1-6cm, the length of the conical part at the tail end is 3-12cm, the conical part is perforated, and the aperture is 2-5mm; the material of the feeding pipe C11 is polytetrafluoroethylene; the mixer C12 is a static mixer, and mixes the extraction solvent and the reaction solution sufficiently.
The outlet of the extraction section is connected with a blanking pipe 14 in fig. 2, as shown in fig. 2, the oil-water separator 13 is vertically arranged, the blanking pipe 14 is inserted into the middle position of the oil-water separator 13, a regulating valve A15 and a flowmeter A16 are arranged at the bottom of the oil-water separator 13 and used for controlling the outflow of wastewater, an organic phase liquid outlet is arranged on the side surface of the separator, the position of the organic phase liquid outlet 17 is higher than the tail end position of the blanking pipe 14, a regulating valve B18 and a flowmeter B19 are arranged on a pipeline of the organic phase liquid outlet 17, and the pipeline of the organic phase liquid outlet 17 is communicated with a feeding pipe D21 of the continuous desolventizing tower 20 in fig. 3.
The flow rate of the wastewater and the organic phase removed is adjusted by the control device automatically or manually according to the feeding flow rate and the feeding flow rate of the extraction solvent.
As shown in fig. 3, the continuous desolventizing tower 20 is vertically arranged, a heating sleeve C22 is arranged outside the feeding pipe D21 to heat the organic phase, most of the solvent enters the desolventizing tower 20 in a gaseous state, a heating device 23 is arranged below the inner part of the desolventizing tower, a riser 24 at the top of the tower is communicated with a condenser 25, and a discharge port 26 is arranged at the bottom of the tower.
The pressure sensor 28 and the temperature sensor 27 are installed in the riser 24, the pressure sensor 28 is used for detecting the pressure in the tower and preventing the pressure from being held back in the tower, the temperature sensor 27 is used for detecting the temperature of the tower top, and the pressure sensor 28 can also be moved to the tower body of the continuous desolventizing tower 20.
The bottom of the condenser 25 has a solvent recovery port 29 for discharging the liquid solvent.
When the continuous reaction device provided by the utility model is used for preparing 2, 3-pentanedione, the preparation process comprises the following steps:
(1) Feeding the hydroxy acetone dilute hydrochloric acid solution into a material mixing section by an anti-corrosion metering pump A1, feeding the paraldehyde into the material mixing section by an anti-corrosion metering pump B2, and fully mixing the hydroxy acetone dilute hydrochloric acid solution and the paraldehyde by a mixer B4 to form a mixed material;
(2) Continuously reacting the mixed materials in a heating reaction section, heating the sleeve B5 to 80-90 ℃ hot water, and maintaining the reaction temperature to 70-75 ℃;
(3) The extraction solvent is introduced into an extraction section by a metering pump C10, the cooled reaction liquid and the extractant are fully mixed by a mixer C12, and the extraction process is completed in the extraction section to form an extracted material;
(4) The extracted material enters an oil-water separator 13 and is separated into wastewater and an organic phase, the wastewater is discharged through a regulating valve A15 and a flowmeter A16, and the organic phase enters a continuous desolventizing tower 20;
(5) The solvent in the organic phase becomes gas under the heating of the heating sleeve C22 and the heating device 23, the gasified solvent rises to the top of the tower, enters the condenser 25 from the riser 24 at the top of the continuous desolventizing tower 20, is further recovered and is used for the extraction operation; the heating temperature of the heating sleeve C22 and the heating device 23 is lower than the product gasification temperature in the organic phase, and the product flows to the bottom of the continuous desolventizing tower 20 in a liquid state and is discharged from a discharge port 26 at the bottom, thus obtaining a crude product.
The reaction time of the mixed material in the heating reaction section is about 15-20nim, the purity of the crude product reaches 95-97%, the solvent residue is less than 2%, and the reaction yield is improved by 8% -10% compared with the conventional kettle type reaction; under the condition of the same floor space of a workshop, the productivity is 5 times of that of the batch reaction of the raw materials.
The above description is only of the preferred embodiments of the present utility model and is not intended to limit the present utility model, but various modifications and variations can be made to the present utility model by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present utility model should be included in the protection scope of the present utility model.
Claims (10)
1. The reaction device for continuously producing 2, 3-pentanedione is characterized by comprising a continuous reaction device, an oil-water separator, a continuous desolventizing tower and a condenser which are sequentially connected from front to back;
the continuous reaction device comprises four parts which are connected in sequence: the device comprises a material mixing section, a heating reaction section, a reaction liquid cooling section and an extraction section;
the outlet of the extraction section is connected with a blanking pipe of the oil-water separator;
an organic phase liquid outlet of the oil-water separator is communicated with a feed pipe D of the continuous desolventizing tower;
the bottom of the continuous desolventizing tower is provided with a discharge port, and the top of the continuous desolventizing tower is provided with a riser which is connected to a condenser.
2. The reaction device for continuously producing 2, 3-pentanedione according to claim 1, wherein the continuous reaction device is a tubular reactor, the tubular reactor is a carbon steel tube, lined with polytetrafluoroethylene or enamel;
or the tubular reactor is a stainless steel tube, lined with polytetrafluoroethylene or enamel.
3. A reaction apparatus for continuously producing 2, 3-pentanedione according to claim 1, wherein,
the front end of the material mixing section is connected with an anti-corrosion metering pump A, a feed pipe B connected with an anti-corrosion metering pump B extends into the continuous reaction device from the side surface of the material mixing section, a mixer B is arranged in the material mixing section behind the opening of the feed pipe B, the anti-corrosion metering pump A is used for feeding hydroxyacetone dilute hydrochloric acid solution, and the anti-corrosion metering pump B is used for feeding paraldehyde.
4. The reaction device for continuously producing 2, 3-pentanedione according to claim 3, wherein the outer diameter of the feed pipe B is smaller than the inner diameter of the material mixing section, the opening part of the tail end of the feed pipe B is tapered and contracted, and the direction of the tapered tail end is the same as the material flowing direction;
the end conical portion of the feed tube B was perforated and the mixer B was a static mixer.
5. A reaction apparatus for continuously producing 2, 3-pentanedione according to claim 1, wherein,
the rear part of the material mixing section is provided with a heating reaction section, the outer side of the material mixing section is provided with a heating sleeve B, and temperature and pressure sensors are uniformly distributed in the heating reaction section;
the rear part of the heating reaction section is provided with a reaction liquid cooling section, and the outer side of the heating reaction section is provided with a cooling sleeve B.
6. A reaction apparatus for continuously producing 2, 3-pentanedione according to claim 1, wherein,
the rear of the reaction liquid cooling section is an extraction section, a feeding pipe C connected with a metering pump C extends into the continuous reaction device from the side face of the extraction section, a mixer C is arranged in the extraction section behind the opening of the feeding pipe C, and the metering pump C is used for feeding extraction solvent.
7. The reaction apparatus for continuously producing 2, 3-pentanedione according to claim 6, wherein,
the outer diameter of the feed pipe C is smaller than the inner diameter of the extraction section, the opening part of the tail end of the feed pipe C is tapered and contracted, and the direction of the tapered tail end is the same as the material flowing direction;
the end conical portion of the feed tube C was perforated and the mixer C was a static mixer.
8. A reaction apparatus for continuously producing 2, 3-pentanedione according to claim 1, wherein,
the oil-water separator is vertically arranged, the discharging pipe is inserted into the middle position of the oil-water separator, an organic phase liquid outlet is arranged on the side surface of the oil-water separator, and the position of the organic phase liquid outlet is higher than the end position of the discharging pipe;
the bottom of the oil-water separator is provided with a regulating valve A and a flowmeter A.
9. A reaction apparatus for continuously producing 2, 3-pentanedione according to claim 1, wherein,
the continuous desolventizing tower is vertically arranged, a heating sleeve C is arranged on the outer side of the feeding pipe D, a heating device is arranged below the inner part of the desolventizing tower, and temperature sensors and pressure sensors are distributed in the riser.
10. The reaction device for continuously producing 2, 3-pentanedione according to claim 1, wherein the pipeline of the organic phase liquid outlet is provided with a regulating valve B and a flowmeter B.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320805326.6U CN219482688U (en) | 2023-04-12 | 2023-04-12 | Reaction device for continuously producing 2, 3-pentanedione |
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| CN202320805326.6U CN219482688U (en) | 2023-04-12 | 2023-04-12 | Reaction device for continuously producing 2, 3-pentanedione |
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| CN202320805326.6U Active CN219482688U (en) | 2023-04-12 | 2023-04-12 | Reaction device for continuously producing 2, 3-pentanedione |
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