CN210058226U - Difluoroethanol reaction dehydration system - Google Patents
Difluoroethanol reaction dehydration system Download PDFInfo
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- CN210058226U CN210058226U CN201920182750.3U CN201920182750U CN210058226U CN 210058226 U CN210058226 U CN 210058226U CN 201920182750 U CN201920182750 U CN 201920182750U CN 210058226 U CN210058226 U CN 210058226U
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Abstract
A difluoroethanol reaction dehydration system belongs to the field of organic chemistry. It is characterized in that a stirring device is arranged in the reaction kettle; the upper end of the reaction kettle is provided with a guide outlet and a guide inlet, the guide outlet is connected with an upper inlet of a glass condenser through a glass gas phase pipe, and a lower outlet of the glass condenser is connected back to the guide inlet through a discharge main pipe; a reflux valve is arranged on the main discharge pipe, the front end of a branch discharge pipe is connected to the main discharge pipe between the reflux valve and the glass condenser, the rear end of the branch discharge pipe is connected with the upper inlet of the glass water separator, and the lower outlet of the glass water separator is connected with a liquid discharge pipe; and a flow dividing liquid outlet is formed in the middle of the glass water separator and is connected with a main discharge pipe between the reflux valve and the introducing port through a flow guide pipe. The utility model discloses can carry out dehydration to the solution midbody that difluoroethanol reaction process produced to retrieve and recycle, supplementary promotion productivity.
Description
Technical Field
The utility model belongs to the field of organic chemistry, a difluoroethanol reaction dewatering system is related to.
Background
2, 2-difluoroethanol is an important aliphatic fluorine-containing intermediate. Because of the special structure of difluoromethyl, the chemical property of the compound is different from that of other alcohols, the compound can participate in various organic synthesis reactions, and has wide application in the aspects of fluorine-containing pesticides, medicines, fluorine polymers and cleaning agents. 2, 2-difluoroethanol is mainly used for synthesizing penoxsulam in pesticides, and is the species with the widest herbicidal spectrum in the herbicide for the rice field at present; 2, 2-difluoroethanol is mainly used for constructing difluoroethoxy in medicine, and the obtained medicine can be used for treating pain, inflammation and antibiotics; the 2, 2-difluoroethanol reacts with the fluorine-containing polymer to lead difluoroethoxy to be introduced into the polymer, so that various properties of the polymer can be improved. In addition, the difluoroethanol can also be used for preparing a cleaning agent with good thermal stability. With the rapid development of the related technical field, the demand of domestic and foreign markets for the difluoroethanol is gradually increased, and the development and production prospects of the difluoroethanol are very wide.
Chinese patent CN107739298A provides a method for preparing difluoroethanol, comprising the following steps:
(1) adding a certain amount of solvent and potassium hydroxide into a reaction kettle, and reacting under stirring at the temperature of 110-200 ℃ for 0.5-12 hours;
(2) after the reaction in the step (1) is finished, slowly adding 2-chloro-1, 1-difluoroethane into a reaction kettle, reacting at the temperature of 170-250 ℃ for 6-24 hours, and then separating and collecting 2, 2-difluoroethanol from the reaction product.
In the process, water is generated in the reaction process, the product is subjected to flash evaporation after the reaction, and incompletely reacted 2-chloro-1, 1-difluoroethane, a product difluoroethanol and a small amount of water are separated, wherein most of the water is remained in the solvent. In this case, the solvent is not dehydrated and the yield of difluoroethanol is lowered when the solvent is reused, so that the solvent must be dehydrated.
In the prior art in the field, no suitable device is available for carrying out scientific and efficient dehydration treatment, and in view of the above, the applicant designs the set of dehydration system, which can solve the technical problems.
Disclosure of Invention
The utility model aims to solve the technical problem that a difluoroethanol reaction dewatering system is provided, can carry out dehydration to the solution midbody that difluoroethanol reaction process produced to retrieve and recycle, supplementary promotion productivity.
In order to solve the technical problem, the technical scheme of the utility model is that: the difluoroethanol reaction dehydration system is characterized by comprising a reaction kettle, a stirring device, a glass gas phase pipe, a glass condenser, a main discharge pipe, a branch discharge pipe, a glass water separator, a glass return pipe, a flow guide pipe and a liquid discharge pipe, wherein the stirring device is arranged in the reaction kettle; the upper end of the reaction kettle is provided with a guide outlet and a guide inlet, the guide outlet is connected with an upper inlet of a glass condenser through a glass gas phase pipe, and a lower outlet of the glass condenser is connected back to the guide inlet through a discharge main pipe; an air guide valve is arranged on the glass gas phase pipe; a reflux valve is arranged on the discharge main pipe, the front end of a discharge branch pipe is connected on the discharge main pipe between the reflux valve and the glass condenser, the rear end of the discharge branch pipe is connected with an upper inlet of a glass water separator, a liquid distribution valve is arranged on the discharge branch pipe, a lower outlet of the glass water separator is connected with a liquid discharge pipe, and a liquid discharge valve is arranged on the liquid discharge pipe; and a flow dividing liquid outlet is formed in the middle of the glass water separator and is connected with a main discharge pipe between the reflux valve and the introducing port through a flow guide pipe.
Preferably, the stirring device comprises a stirring motor, and a motor shaft of the stirring motor is connected with the stirring rod; the stirring rod is a corrosion-resistant high-strength ceramic rod body, one end of the stirring rod inserted into the reaction kettle is sleeved with a metal sheath, and a plurality of metal stirring wings are arranged on the metal sheath.
Preferably, the reaction kettle comprises a metal shell and a non-metal corrosion-resistant inner lining, and the non-metal corrosion-resistant inner lining is arranged in the metal shell; a hollow interlayer is arranged between a metal shell at the bottom of the reaction kettle and the non-metal corrosion-resistant lining, a high-frequency induction coil is arranged in the hollow interlayer, and the high-frequency induction coil is connected with a high-frequency power supply.
Preferably, an electronic thermometer is arranged in the reaction kettle.
Preferably, the reaction kettle comprises a metal shell and a non-metal corrosion-resistant lining, a heating guide pipe is spirally wound between the metal shell and the non-metal corrosion-resistant lining, the front end of the heating guide pipe is connected with a liquid outlet of the heat-conducting oil tank through a heat-conducting oil pump, and the rear end of the heating guide pipe is connected back to a liquid inlet of the heat-conducting oil tank; and a ceramic electric heating rod is arranged in the heat-conducting oil tank.
Compared with the prior art, the beneficial effects of the utility model are that:
the invention mainly aims at the problem that the solvent needs to be dehydrated after the reaction in the difluoroethanol production process, and designs an economic and energy-saving dehydration equipment system. The difluoroethanol production system has the advantages that the reaction kettle is connected with the glass condenser and the glass water separator through the pipeline, the reaction kettle and the glass water separator can be separated by utilizing the characteristic that the density of water is greater than that of a reaction solvent, the solvent flows back to the reaction kettle for continuous use, most of water is discharged, and a small amount of residual water is evaporated and separated, so that the dehydration time of the solvent is shortened, and the reaction time is greatly saved.
Drawings
Fig. 1 is a schematic structural diagram (embodiment one) of the present invention;
FIG. 2 is a schematic view of the structure of the reaction vessel of the present invention (example two)
In the figure: 1. a glass gas phase tube; 2. a gas guide valve; 3. a stirring motor; 4. a corrosion-resistant high-strength ceramic rod body; 5. a metal stirring fin; 6. a metal sheath;
7. a reaction kettle: 7.1, a metal shell; 7.2, a non-metal corrosion-resistant inner lining;
8. a main discharge pipe; 9. a reflux valve; 10. a lead-out port; 11. a flow guide pipe; 12. an inlet port; 13. a liquid discharge pipe; 14. a drain valve; 15. a glass water separator; 16. a liquid separating valve; 17. a discharge branch pipe; 18. a glass condenser; 19. a high-frequency induction coil.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Example one
As shown in fig. 1, the difluoroethanol reaction dehydration system of the present invention comprises a reaction kettle 7, a stirring device, a glass gas phase pipe 1, a glass condenser 18, a main discharging pipe 8, a branch discharging pipe 17, a glass water separator 15, a glass return pipe, a flow guide pipe 11 and a liquid discharge pipe 13, wherein the stirring device is arranged in the reaction kettle 7; the upper end of the reaction kettle 7 is provided with an outlet 10 and an inlet 12, the outlet 10 is connected with the upper inlet of a glass condenser 18 through a glass gas phase pipe 1, and the lower outlet of the glass condenser 18 is connected back to the inlet 12 through a main discharging pipe 8; an air guide valve 2 is arranged on the glass gas phase pipe 1; a reflux valve 9 is arranged on the discharge main pipe 8, the front end of a discharge branch pipe 17 is connected on the discharge main pipe 8 between the reflux valve 9 and the glass condenser 18, the rear end of the discharge branch pipe 17 is connected with the upper inlet of a glass water separator 15, a liquid separation valve 16 is arranged on the discharge branch pipe 17, the lower outlet of the glass water separator 15 is connected with a liquid discharge pipe 13, and a liquid discharge valve 14 is arranged on the liquid discharge pipe 13; a flow splitting liquid outlet is formed in the middle of the glass water separator 15 and is connected with a main discharge pipe 8 between the reflux valve 9 and the introducing port 12 through a flow guide pipe 11.
An electronic thermometer was disposed in the reaction vessel 7.
When the device is used, materials and an organic solvent are firstly added into a reaction kettle 7, and the solvent and moisture enter a glass condenser 18 through a glass gas phase pipe 1 in the heating reaction process; during the reaction, the mixture of solvent and water is introduced as vapor into the glass condenser 18 through the glass vapor phase tube 1, and the reflux valve 9 is closed. The mixed steam is changed into a liquid state in the glass condenser 18 and flows into the glass water separator 15 through the main discharging pipe 8 and the branch discharging pipe 17; the organic solvent which exceeds a shunting liquid outlet of the glass water separator 15 flows back to the reaction kettle 7 through the guide pipe 11 and the introducing port 12; when the water phase liquid level in the glass water separator 15 approaches the split liquid outlet, a liquid discharge valve 14 on a liquid discharge pipe 13 is opened to discharge the water phase liquid; in the reaction process, the glass water separator 15 is observed at any time, and the liquid level of the water phase is always kept not to exceed the flow dividing liquid outlet of the glass water separator 15.
Example two
As shown in fig. 2, in the present embodiment, the stirring device includes a stirring motor 3, and a motor shaft of the stirring motor 3 is connected to a stirring rod; the stirring rod is a corrosion-resistant high-strength ceramic rod body 4, one end of the stirring rod inserted into the reaction kettle 7 is sleeved with a metal sheath 6, and a plurality of metal stirring wings 5 are arranged on the metal sheath 6.
The reaction kettle 7 comprises a metal shell 7.1 and a non-metal corrosion-resistant inner liner 7.2, wherein the non-metal corrosion-resistant inner liner 7.2 is arranged in the metal shell 7.1; a hollow interlayer is arranged between a metal shell 7.1 at the bottom of the reaction kettle 7 and a non-metal corrosion-resistant inner liner 7.2, a high-frequency induction coil 19 is arranged in the hollow interlayer, and the high-frequency induction coil 19 is connected with a high-frequency power supply.
Since the reaction of the materials in the reaction vessel 7 is carried out at a predetermined temperature, a necessary heating measure is required. A high-frequency induction coil 19 is arranged in a hollow interlayer at the bottom of the reaction kettle 7, the high-frequency induction coil 19 is connected with a high-frequency power supply, and by utilizing the electromagnetic induction phenomenon, namely, alternating current is utilized to generate an alternating magnetic field with constantly changed direction through a coil, vortex current (the reason can refer to Faraday's law of electromagnetic induction) will appear in a conductor in the alternating magnetic field, which is caused by the vortex electric field pushing the current carriers (electrons but no iron atoms in a pot) in the conductor to move; the joule heating effect of the eddy current heats the conductor, thereby achieving heating.
The rest of the structure and the using method are the same as those of the first embodiment, and are not described again.
EXAMPLE III
The reaction kettle 7 comprises a metal shell 7.1 and a non-metal corrosion-resistant lining 7.2, a heating guide pipe is spirally wound between the metal shell 7.1 and the non-metal corrosion-resistant lining 7.2, the front end of the heating guide pipe is connected with a liquid outlet of a heat-conducting oil tank through a heat-conducting oil pump, and the rear end of the heating guide pipe is connected back to a liquid inlet of the heat-conducting oil tank; and a ceramic electric heating rod is arranged in the heat-conducting oil tank.
In this embodiment, can heat the conduction oil in the heat conduction oil tank through the ceramic electric heating rod, wait to heat to the regulation temperature after, coil reation kettle 7 by heating honeycomb duct with the conduction oil by the heat conduction oil pump and carry out circulating outer wall heating. The heating mode of this embodiment is more safe convenient, can be according to the nimble adjustment of outside climatic change.
The rest of the structure and the using method are the same as those of the first embodiment, and are not described again.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention. The technical solution of the present invention is not to be departed from, and any simple modification, equivalent change and modification made to the above embodiments according to the technical substance of the present invention still belong to the protection scope of the technical solution of the present invention.
Claims (5)
1. A difluoroethanol reaction dehydration system is characterized by comprising a reaction kettle, a stirring device, a glass gas phase pipe, a glass condenser, a main discharge pipe, a branch discharge pipe, a glass water separator, a glass reflux pipe, a diversion pipe and a liquid discharge pipe, wherein the stirring device is arranged in the reaction kettle; the upper end of the reaction kettle is provided with a guide outlet and a guide inlet, the guide outlet is connected with an upper inlet of a glass condenser through a glass gas phase pipe, and a lower outlet of the glass condenser is connected back to the guide inlet through a discharge main pipe; an air guide valve is arranged on the glass gas phase pipe; a reflux valve is arranged on the discharge main pipe, the front end of a discharge branch pipe is connected on the discharge main pipe between the reflux valve and the glass condenser, the rear end of the discharge branch pipe is connected with an upper inlet of a glass water separator, a liquid distribution valve is arranged on the discharge branch pipe, a lower outlet of the glass water separator is connected with a liquid discharge pipe, and a liquid discharge valve is arranged on the liquid discharge pipe; and a flow dividing liquid outlet is formed in the middle of the glass water separator and is connected with a main discharge pipe between the reflux valve and the introducing port through a flow guide pipe.
2. A difluoroethanol reaction dehydration system as recited in claim 1 further characterized by: the stirring device comprises a stirring motor, and a motor shaft of the stirring motor is connected with the stirring rod; the stirring rod is a corrosion-resistant high-strength ceramic rod body, one end of the stirring rod inserted into the reaction kettle is sleeved with a metal sheath, and a plurality of metal stirring wings are arranged on the metal sheath.
3. A difluoroethanol reaction dehydration system as recited in claim 2 further characterized by: the reaction kettle comprises a metal shell and a non-metal corrosion-resistant lining, and the non-metal corrosion-resistant lining is arranged in the metal shell; a hollow interlayer is arranged between a metal shell at the bottom of the reaction kettle and the non-metal corrosion-resistant lining, a high-frequency induction coil is arranged in the hollow interlayer, and the high-frequency induction coil is connected with a high-frequency power supply.
4. A difluoroethanol reaction dehydration system according to claim 3 characterized by: an electronic thermometer is arranged in the reaction kettle.
5. A difluoroethanol reaction dehydration system as recited in claim 1 further characterized by: the reaction kettle comprises a metal shell and a non-metal corrosion-resistant lining, a heating guide pipe is spirally wound between the metal shell and the non-metal corrosion-resistant lining, the front end of the heating guide pipe is connected with a liquid outlet of the heat-conducting oil tank through a heat-conducting oil pump, and the rear end of the heating guide pipe is connected back to a liquid inlet of the heat-conducting oil tank; and a ceramic electric heating rod is arranged in the heat-conducting oil tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920182750.3U CN210058226U (en) | 2019-02-01 | 2019-02-01 | Difluoroethanol reaction dehydration system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920182750.3U CN210058226U (en) | 2019-02-01 | 2019-02-01 | Difluoroethanol reaction dehydration system |
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| Publication Number | Publication Date |
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| CN210058226U true CN210058226U (en) | 2020-02-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201920182750.3U Active CN210058226U (en) | 2019-02-01 | 2019-02-01 | Difluoroethanol reaction dehydration system |
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| CN (1) | CN210058226U (en) |
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- 2019-02-01 CN CN201920182750.3U patent/CN210058226U/en active Active
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