CN216458779U - Perfluorohexylethanol refining plant - Google Patents
Perfluorohexylethanol refining plant Download PDFInfo
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- CN216458779U CN216458779U CN202122504378.3U CN202122504378U CN216458779U CN 216458779 U CN216458779 U CN 216458779U CN 202122504378 U CN202122504378 U CN 202122504378U CN 216458779 U CN216458779 U CN 216458779U
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Abstract
The utility model belongs to the field of chemical products, and discloses a perfluorohexyl ethanol refining device which comprises an original auxiliary feeding system, a reaction kettle, a distillation kettle, a rectifying tower and a product extraction system which are sequentially connected through pipelines. The original auxiliary feeding system is provided with a pipe orifice at the upper end socket of the reaction kettle to be communicated with the reaction kettle; the feeding flowmeter and the feeding stop valve are arranged on the feeding pipe of the reaction kettle, and the feeding flowmeter, the feeding stop valve and the feeding pipe of the reaction kettle are connected by flanges. The utility model recycles the by-product resources of the C6 ester and the C6 methyl ester which are difficult to process, and converts the by-product resources into perfluorohexylethanol with high added value. The utility model improves the accuracy and precision of the process control in the production process of the perfluorohexyl ethanol, reduces the random error of production operation, reduces the labor intensity of workers and lightens the pressure of environmental protection.
Description
Technical Field
The utility model belongs to chemical products, and particularly relates to a perfluorohexyl ethanol refining device.
Background
At present, with the rapid upgrading of industrial transformation, the demands of related industries such as automobiles, electronics, light industry, new energy, environmental protection, aerospace and the like on high-performance fluoropolymers, novel refrigerants and fluorine-containing fine chemicals are increasingly urgent, the demand of fluorides is continuously increased, and a wider market space is provided for the industry of fluorine industry. The fluorine chemical industry is an important branch of the chemical new material industry, and is also an important matched material required for developing other strategic emerging industries such as high-end manufacturing industry, environmental protection, new energy and the like and promoting the traditional industry.
However, due to the technical monopoly of fluorine-containing fine chemicals by foreign companies, the markets for fluorosurfactants, emulsifiers and fabric finishes have been monopolized by foreign companies. Meanwhile, due to the complexity and monopoly of related production technologies, a large amount of unusable and difficultly-treated byproducts exist in the process of producing C6 ester and C6 methyl ester, so that the environment-friendly treatment difficulty is increased, and a large amount of fluoride resources are lost. Therefore, the development of the process control of the perfluorohexylethanol has important practical significance.
At present, perfluorohexylethyl iodide is mostly adopted in the traditional process to prepare perfluorohexylethanol, the process of the existing product is improved and optimized, on one hand, a large amount of unusable byproduct resources which are difficult to treat are fully recycled and converted into perfluorohexylethanol with high added value, and waste is changed into valuable, so that the advantages of the technology are reflected in energy consumption, cost, economic benefit and environmental protection benefit; on the other hand, a set of relatively perfect perfluorohexylethanol preparation and refining device is established, so that the operation safety is improved, and the problem of high manual operation strength is solved.
Through the above analysis, the problems and defects of the prior art are as follows:
(1) during the production of the C6 ester and C6 methyl ester, there are a large number of unusable and difficult to handle by-products.
(2) In the traditional process, perfluorohexylethyl iodide is mostly adopted to prepare perfluorohexylethanol, byproducts which are difficult to treat exist, a perfluorohexylethanol preparation and refining device is incomplete, the safety needs to be improved, and the manual operation intensity is high.
(3) The original method for preparing perfluorohexylethanol by using perfluorohexylethyl iodide has the characteristics of corrosive catalyst, poor recovery effect and the like, increases the environmental protection difficulty caused by sewage discharge, and has certain potential safety hazard in production operation.
SUMMERY OF THE UTILITY MODEL
Aiming at the problems in the prior art, the utility model provides a preparation method, a refining device and application of perfluorohexylethanol.
The utility model is realized in such a way that a perfluorohexyl ethanol refining device comprises an original auxiliary feeding system, a reaction kettle, a distillation kettle, a rectifying tower and a product extraction system which are sequentially connected through pipelines.
Further, the original auxiliary feeding system is communicated with the reaction kettle through a pipe orifice at the upper end socket of the reaction kettle;
the feeding flowmeter and the feeding cut-off valve are arranged on the feeding pipe of the reaction kettle and are connected with the feeding pipe of the reaction kettle by flanges;
a flow totalizing value window is arranged on the feeding flowmeter and used for displaying the feeding flow;
the perfluorohexyl ethanol refining device also comprises a cooling reaction system; the temperature reduction reaction system comprises a thermal resistor arranged on the reaction kettle, a pipe orifice is formed on the inner side surface of the reaction kettle container, and the thermal resistor is connected with the pipe orifice of the reaction kettle by threads;
the cooling reaction system also comprises a 0 ℃ cold brine inlet and outlet pipe which is additionally arranged on the side surface of the jacket of the reaction kettle, and a reaction kettle refrigerant inlet and outlet regulating valve is arranged on the 0 ℃ cold brine inlet pipe;
the perfluorohexyl ethanol refining device also comprises a pressure boosting and purging system;
the pressure boosting and purging system is arranged on an upper end socket of the reaction kettle, the pressure boosting and purging system comprises a remote transmission pressure transmitter arranged on the reaction kettle, a reaction kettle pipe orifice is opened at the upper end socket of the reaction kettle, the remote transmission pressure transmitter and the reaction kettle pipe orifice are connected through a pressure guide pipe, and a nitrogen gas cut-off valve is arranged on a nitrogen gas inlet pipe at the top of the reaction kettle.
Further, a thermal resistor is arranged on the distillation still, a distillation still pipe opening is formed in the position of a lower end enclosure of the distillation still, the thermal resistor is in threaded connection with the distillation still pipe opening, a steam and steam condensate water inlet and outlet pipe is additionally arranged on the side surface of a distillation still jacket, and a distillation still steam regulating valve is arranged on the steam inlet pipe;
the product extraction system is characterized in that an extraction regulating valve and an extraction flowmeter are additionally arranged between a condenser and a collecting tank pipeline, the extraction regulating valve, the extraction flowmeter and a collecting tank feeding pipe are connected by flanges, an extraction viewing mirror is additionally arranged on the condenser and collecting tank pipeline, a reflux viewing mirror is additionally arranged on the condenser and rectifying tower pipeline, and an instantaneous flow value window is arranged on the extraction flowmeter;
the collecting tank is connected with a vacuum pump through a buffer pipe.
The utility model also aims to provide the application of the preparation method of the perfluorohexyl ethanol in preparation of fluorine-containing fine chemicals in automobile, electron, light industry, new energy, environmental protection and aerospace related industries.
By combining all the technical schemes, the utility model has the advantages and positive effects that:
(1) the automatic control of reation kettle feeding is realized to reation kettle feeding flowmeter and feeding trip valve interlocking, effectively solves reation kettle's feeding measurement problem, and the material ratio of accuse perfluorohexyl ethanol is accurate, and to a great extent reduces the artifical ratio error of throwing the material and causing, the running cost of control production.
(2) The reaction kettle temperature and the reaction kettle jacket 0 ℃ cold salt water inlet regulating valve are interlocked to realize the automatic control of the reaction kettle reaction temperature, the phenomenon of unstable reaction temperature caused by manual regulation of the opening degree is effectively overcome, and the self-aggregation amount of the reaction liquid is increased, thereby influencing the reaction effect of the reaction kettle.
(3) The nitrogen cut-off valve of the reaction kettle is automatically closed, the problem of overhigh pressure rise caused by manual operation in the past is effectively solved, frequent purging is needed due to the particularity of reaction liquid, on one hand, if the subsequent reaction is difficult due to incomplete purging, on the other hand, the safety risk of maintenance can be improved, meanwhile, pressure change conditions of the reaction kettle can be closely observed through pressure remote transmission, and necessary solutions are timely taken.
(4) The automatic control of still temperature is realized to still temperature and still jacket steam control valve interlocking, can effectively in time judge the interior fraction condition of still to set up the warning of temperature high limit, can in time prejudge, guarantee steam operation on the one hand and avoid manual control's security, on the other hand is according to the timely temperature range of adjusting of fraction boiling point, and to a great extent has reduced the production of accessory substance, thereby has improved the product yield.
(5) Through the automatic control of the instantaneous flow of the extraction regulating valve and the extraction flowmeter, the problem that the extraction flow cannot be accurately judged in the process control can be effectively solved. If the extraction flow is too large, on one hand, the sampling purity is influenced, so that the product quality is influenced, and on the other hand, excessive front fraction is generated, so that the product yield is reduced; if the extraction flow is too small, on one hand, the long-time investment of combustion kinetic energy consumption is increased, and on the other hand, the production efficiency is reduced, so that the labor cost is increased. Therefore, the extraction flowmeter and the extraction regulating valve are arranged between the condenser and the pipeline of the collecting tank, the precise control of the rectification extraction amount is realized, the energy consumption and the labor cost are saved, the product yield is improved, and considerable economic benefits are brought.
(6) The utility model provides a perfluorohexylethanol preparation and refining device, which recycles the byproduct resources which are difficult to treat in C6 ester and C6 methyl ester, changes waste into valuable, can effectively solve the defects of the traditional process, improves the process control, obtains considerable performance from the aspects of energy consumption, cost, economic benefit and environmental protection benefit, and has certain innovation. Meanwhile, the reliability and the safety of field operation are improved.
Drawings
FIG. 1 is a schematic view of a perfluorohexylethanol purification apparatus according to an embodiment of the present invention.
In the figure: 1. a reaction kettle; 2. a distillation kettle; 3. a rectifying tower; 4. a condenser; 5. collecting tank; 6. a buffer tube; 7. a vacuum pump.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the utility model and are not intended to limit the utility model.
In view of the problems in the prior art, the present invention provides a device for preparing and refining perfluorohexylethanol, which is described in detail below with reference to the accompanying drawings.
As shown in figure 1, the utility model provides a perfluorohexyl ethanol refining device which comprises an original auxiliary feeding system, a reaction kettle 1, a distillation kettle 2, a rectifying tower 3 and a product extraction system which are sequentially connected through pipelines.
In one embodiment of the utility model, the original auxiliary feeding system is communicated with the reaction kettle through a pipe orifice at the upper end socket of the reaction kettle;
the feeding flowmeter and the feeding cut-off valve are arranged on the feeding pipe of the reaction kettle and are connected with the feeding pipe of the reaction kettle by flanges;
a flow totalizing value window is arranged on the feeding flowmeter and used for displaying the feeding flow;
in an embodiment of the present invention, the perfluorohexylethanol refining apparatus further includes a temperature reduction reaction system; the temperature reduction reaction system comprises a thermal resistor arranged on the reaction kettle, a pipe orifice is formed on the inner side surface of the reaction kettle container, and the thermal resistor is connected with the pipe orifice of the reaction kettle by threads;
the cooling reaction system also comprises a 0 ℃ cold brine inlet and outlet pipe which is additionally arranged on the side surface of the jacket of the reaction kettle, and a reaction kettle refrigerant inlet and outlet regulating valve is arranged on the 0 ℃ cold brine inlet pipe;
in an embodiment of the present invention, the perfluorohexyl ethanol refining device further includes a pressure boosting purging system;
the pressure boosting and purging system is arranged on an upper end socket of the reaction kettle, the pressure boosting and purging system comprises a remote transmission pressure transmitter arranged on the reaction kettle, a reaction kettle pipe orifice is opened at the upper end socket of the reaction kettle, the remote transmission pressure transmitter and the reaction kettle pipe orifice are connected through a pressure guide pipe, and a nitrogen gas cut-off valve is arranged on a nitrogen gas inlet pipe at the top of the reaction kettle.
In one embodiment of the utility model, a thermal resistor is arranged on the distillation still, a distillation still pipe orifice is formed at the lower seal head of the distillation still, the thermal resistor is in threaded connection with the distillation still pipe orifice, a steam and steam condensate water inlet and outlet pipe is additionally arranged on the side surface of a distillation still jacket, and a distillation still steam regulating valve is arranged on the steam inlet pipe;
in one embodiment of the utility model, the product extraction system is additionally provided with an extraction regulating valve and an extraction flowmeter between pipelines from a condenser 4 to a collecting tank 5, the extraction regulating valve, the extraction flowmeter and a collecting tank feeding pipe are connected by flanges, an extraction sight glass is additionally arranged on the pipeline from the condenser to the collecting tank, a reflux sight glass is additionally arranged on the pipeline from the condenser to a rectifying tower, and an instantaneous flow value window is arranged on the extraction flowmeter;
the collection tank 5 is connected via a buffer tube 6 to a vacuum pump 7.
The technical solution of the present invention is further described below with reference to application examples.
Application example
The utility model relates to a perfluorohexylethanol preparation and refining device with a reaction system, which is characterized by automatic feeding, cutting and interlocking, automatic cooling and regulating interlocking, automatic boosting and cutting interlocking, a rectification system, automatic heating and regulating interlocking and automatic discharging and regulating interlocking.
Specifically, the method for preparing perfluorohexylethanol comprises the following steps:
1. the reaction kettle is in a feeding state, a feeding cut-off valve of the reaction kettle can be opened, and the feeding cut-off valve of the reaction kettle is automatically closed after the flow accumulated value on the feed flowmeter of the reaction kettle reaches a set value.
2. The reactor is fed with materials completely and has a cooling condition, the reactor jacket 0 ℃ cold brine inlet adjusting valve can be opened, the reactor jacket is supplied with 0 ℃ cold brine to cool materials in the reactor, and after the temperature in the reactor is close to a required set value, the opening degree of the 0 ℃ cold brine inlet adjusting valve is automatically adjusted.
3. The reation kettle ejection of compact finishes and possesses the condition of stepping up, can open reation kettle nitrogen gas trip valve, after reation kettle pressure rose to required pressure value, self-closing reation kettle nitrogen gas trip valve.
4. The distillation still is ready for stripping and has a temperature rise condition, the steam regulating valve of the distillation still jacket can be opened to supply steam to the distillation still jacket, and the opening degree of the steam regulating valve can be automatically regulated when the temperature in the distillation still is close to the boiling point set value of the fraction according to the difference of the boiling points of different fractions.
5. When the rectifying tower is in rectification and the reflux sight glass is in a liquid-full stable state, the extraction regulating valve between the condenser and the pipeline of the collecting tank can be properly opened, the discharging operation is started, the extraction condition of the extraction sight glass and the instantaneous flow of the extraction flowmeter are observed, after the instantaneous flow value is close to a working condition set value, the opening degree of the extraction regulating valve is automatically regulated, the front fraction continuous extraction state is started, and when the sampling purity meets the working condition requirement, the front fraction collecting tank is switched to.
The technical solution of the present invention will be further described with reference to the application effects
The original method for preparing perfluorohexylethanol by using perfluorohexylethyl iodide has the characteristics of corrosive catalyst, poor recovery effect and the like, increases the environmental protection difficulty caused by sewage discharge, and has certain potential safety hazard in production operation. The utility model provides a perfluorohexylethanol preparation and refining device, which recycles the byproduct resources which are difficult to treat in C6 ester and C6 methyl ester, changes waste into valuable, can effectively solve the defects of the traditional process, improves the process control, obtains considerable performance from the aspects of energy consumption, cost, economic benefit and environmental protection benefit, and has certain innovation. Meanwhile, the reliability and the safety of field operation are improved.
In the description of the present invention, "a plurality" means two or more unless otherwise specified; the terms "upper", "lower", "left", "right", "inner", "outer", "front", "rear", "head", "tail", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing and simplifying the description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, should not be construed as limiting the utility model. Furthermore, the terms "first," "second," "third," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the utility model, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the utility model as defined by the appended claims.
Claims (8)
1. The perfluorohexyl ethanol refining device is characterized by comprising an original auxiliary feeding system, a reaction kettle, a distillation kettle, a rectifying tower and a product extraction system which are sequentially connected through pipelines.
2. The perfluorohexyl ethanol refining device according to claim 1, wherein the original auxiliary feeding system is communicated with the reaction kettle through a pipe orifice at the upper end socket of the reaction kettle;
the feeding flowmeter and the feeding cut-off valve are arranged on the feeding pipe of the reaction kettle and are connected with the feeding pipe of the reaction kettle by flanges;
and a flow totalizing value window is arranged on the feeding flowmeter and used for displaying the feeding flow.
3. The perfluorohexylethanol purification apparatus according to claim 1, further comprising a temperature-lowering reaction system; the cooling reaction system comprises a thermal resistor arranged on the reaction kettle, a pipe orifice is formed on the inner side surface of the reaction kettle container, and the thermal resistor is connected with the pipe orifice of the reaction kettle by threads.
4. The apparatus for refining perfluorohexylethanol according to claim 1, wherein the temperature-lowering reaction system further comprises a 0 ℃ cold brine inlet/outlet pipe provided on the side of the jacket of the reaction vessel, and a reaction vessel coolant inlet/outlet valve provided on the 0 ℃ cold brine inlet pipe.
5. The perfluorohexylethanol purification apparatus according to claim 1, further comprising a pressure-boosting purge system;
the pressure boosting and purging system is arranged on an upper end socket of the reaction kettle, the pressure boosting and purging system comprises a remote transmission pressure transmitter arranged on the reaction kettle, a reaction kettle pipe orifice is opened at the upper end socket of the reaction kettle, the remote transmission pressure transmitter and the reaction kettle pipe orifice are connected through a pressure guide pipe, and a nitrogen gas cut-off valve is arranged on a nitrogen gas inlet pipe at the top of the reaction kettle.
6. The perfluorohexyl ethanol refining device according to claim 1, wherein a thermal resistor is arranged on the distillation still, a distillation still pipe opening is formed at the lower seal head of the distillation still, the thermal resistor is in threaded connection with the distillation still pipe opening, a steam and steam condensate water inlet and outlet pipe is additionally arranged on the side surface of the distillation still jacket, and a distillation still steam regulating valve is arranged on the steam inlet pipe.
7. The perfluorohexyl ethanol refining device according to claim 1, wherein the product extraction system is additionally provided with an extraction regulating valve and an extraction flowmeter between a condenser and a collection tank pipeline, the extraction regulating valve, the extraction flowmeter and a collection tank feeding pipe are connected by flanges, an extraction sight glass is additionally arranged on the condenser and collection tank pipeline, a reflux sight glass is additionally arranged on the condenser and rectifying tower pipeline, and an instantaneous flow value window is arranged on the extraction flowmeter.
8. The apparatus for refining perfluorohexylethanol according to claim 7, wherein the collection tank is connected to a vacuum pump through a buffer tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122504378.3U CN216458779U (en) | 2021-10-18 | 2021-10-18 | Perfluorohexylethanol refining plant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122504378.3U CN216458779U (en) | 2021-10-18 | 2021-10-18 | Perfluorohexylethanol refining plant |
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| Publication Number | Publication Date |
|---|---|
| CN216458779U true CN216458779U (en) | 2022-05-10 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202122504378.3U Active CN216458779U (en) | 2021-10-18 | 2021-10-18 | Perfluorohexylethanol refining plant |
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|---|---|
| CN (1) | CN216458779U (en) |
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2021
- 2021-10-18 CN CN202122504378.3U patent/CN216458779U/en active Active
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: A Perfluorohexyl Ethanol Refining Device Effective date of registration: 20230925 Granted publication date: 20220510 Pledgee: Industrial and Commercial Bank of China Limited Sanming Sanyuan Branch Pledgor: FUJIAN SANNONG NEW MATERIALS CO.,LTD. Registration number: Y2023980058306 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |