CN205435720U - Preparation facilities of fluorine carbon mellow wine - Google Patents
Preparation facilities of fluorine carbon mellow wine Download PDFInfo
- Publication number
- CN205435720U CN205435720U CN201521130125.2U CN201521130125U CN205435720U CN 205435720 U CN205435720 U CN 205435720U CN 201521130125 U CN201521130125 U CN 201521130125U CN 205435720 U CN205435720 U CN 205435720U
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- China
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- flasks
- many mouthfuls
- thermometer
- preparation facilities
- utility
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Abstract
The utility model relates to a preparation facilities of fluorine carbon mellow wine, including many mouthfuls of flasks, put in the ice -water bath thermotank bottom of many mouthfuls of flasks, be connected with solid feed hopper, backward flow condenser pipe, thermometer on the connector of many mouthfuls of flasks respectively, solid feed hopper's the charge door of upper portion for being equipped with the closing cap, the reinforced screw rod of below for being used for controlling the solid feed rate of charge door, backward flow condenser pipe below is provided with the water inlet of comdenstion water, and the top is provided with the delivery port of comdenstion water, even there is the air duct on backward flow condenser pipe top, the air duct is connected with the cross -connection pipe, the cross -connection pipe still is connected with oil vacuole ware, nitrogen gas steel bottle and vacuum pump, compared with the prior art, the beneficial effects of the utility model are that: can control the feed rate through rotatory reinforced screw rod, through the temperature that reaction liquid was observed to the thermometer registration, can ensure under the protection of nitrogen gas moreover that reaction product is stable, reduces the appearance of accessory substance.
Description
Technical field
This utility model relates to technical field of fine, particularly relates to the preparation facilities of a kind of fluorocarbon alcohol.
Background technology
Fluorocarbon alcohol compounds is the compounds that the carbon atom upper part hydrogen of Organic Alcohol is replaced by fluorine, special stability and physiologically active due to its molecule, this compounds has been widely used at the aspect such as medicine, pesticide, fluorine-containing surfactant, dyestuff, energy tool, is a kind of important, fluoro-containing intermediate that development prospect is good.
The synthetic method of fluorocarbon alcohol, including electrofluorination method, telomerization method and esterification water solution.Hydrogen atom in the active corresponding hydrocarbon carboxylic of fluorine atom direct replacement that electrofluorination method is produced by electrolysis or hydrocarbon sulfonic acid molecules completes fluorination reaction, needed in this method, perfluorocarboxylic acid reduction generates the corresponding reaction containing fluoroalkyl alcohol, condition is relatively more violent, is not suitable for large-scale industrial production.In telomerisation with politef and lower alcohol as raw material, the influence factor of the reaction such as the concentration of initiator used, reaction pressure, temperature, lower alcohol is more, and the control of process conditions is the harshest.In esterification water solution due to reaction condition alkalescence relatively by force, being susceptible to side reaction, generate the by-product of perfluoro alkyl ethylene and perfluoroalkyl methyl ether, this by-product is close with the character of target product fluorocarbon alcohol, it is difficult to realize separating, and causes the yield reacted relatively low.
Applicant has applied for the patent of invention of the preparation method and applications about a kind of fluorocarbon alcohol simultaneously, is with hexafluoropropylene oxide polymer as raw material, and lower alcohol (methanol, ethanol, propanol) is solvent, NaBH4For reducing agent, under certain condition raw material is esterified, reduces and can prepare highly purified fluorocarbon alcohol.Preparation method technical process is simple, product yield is high for this, and safety, economy, suitable large-scale industrial production.
Utility model content
The purpose of this utility model is to provide the preparation facilities of a kind of fluorocarbon alcohol, and this process units is easy to control solids feed rates, it can be ensured that product composition is stable and no coupling product generates.
The preparation facilities of a kind of fluorocarbon alcohol is the technical scheme is that, it is characterised in that include that many mouthfuls of flasks, the bottom of described many mouthfuls of flasks are put in ice-water bath temperature chamber by realizing the purpose of this utility model；It is connected to solid charging hopper, reflux condensing tube, thermometer on the connector of described many mouthfuls of flasks；The top of described solid charging hopper is the charge door being provided with capping, and the lower section of charge door is the feed-screw for controlling solids feed rates；It is provided with the water inlet of condensed water below described reflux condensing tube, is provided above the outlet of condensed water；Described reflux condensing tube top is connected with airway, and described airway connects has four-way connecting tube, described four-way connecting tube to be also associated with oil vacuole device, nitrogen cylinder and vacuum pump.
The bottom of described thermometer is ground structure, and the bottom of this thermometer is placed in described many mouthfuls of flasks in reactant liquor, but does not contacts with the bottom bottle wall of many mouthfuls of flasks.
Operation principle of the present utility model is: when device air-tightness is good on inspection, by the air emptying in system, is passed through nitrogen wherein and makes system external and internal pressure consistent；In course of reaction, solids feed rates is controlled by the feed-screw on rotary feeding funnel, make the solid material in charging hopper at the uniform velocity join in reaction bulb, the existence of feed-screw simultaneously can avoid in course of reaction produce steam rise to charging hopper internal contamination solid material；The steam produced in course of reaction can not all be condensed when refluxing, and will be discharged by oil vacuole device；Oil vacuole device is not only able to discharge the gas of reaction system, also has the effect of liquid seal, i.e. prevents the air in the external world from being entered in reaction system by oil vacuole device.
Compared with prior art; the beneficial effects of the utility model are: can control solids feed rates by the feed-screw on rotary feeding funnel; make the solid material in charging hopper at the uniform velocity join in reaction bulb; guarantee that the reactivity in system is basically identical; and under the protection of nitrogen, it is able to ensure that product is stable, reduce the appearance of by-product；Package unit is built simply, operates safety, and low cost, is suitable to apply in industry's enlarging production.
Accompanying drawing explanation
Fig. 1 show the structural representation of the preparation facilities of a kind of fluorocarbon alcohol.
Detailed description of the invention
Below in conjunction with specific embodiment, this utility model is described in further detail.Should be appreciated that specific embodiment described herein, only in order to explain this utility model, is not used to limit this utility model.
Embodiment:
Being illustrated in figure 1 the preparation facilities of a kind of fluorocarbon alcohol, including many mouthfuls of flasks 4, the bottom of described many mouthfuls of flasks is ice-water bath temperature chamber 5, and the top of described many mouthfuls of flasks is provided with three entrances, is connected to solid charging hopper 1, reflux condensing tube 2 and thermometer 3；Described solid charging hopper 1 top is solid feed inlet 1-1, is feed-screw 1-2 below solid feed inlet, is minim pipette 1-3 below described feed-screw 1-2, is connected with many mouthfuls of flasks 4 by ground bottom minim pipette 1-3；Being provided with the water inlet 2-2 of condensed water below described reflux condensing tube 2, be provided above the outlet 2-1 of condensed water, described reflux condensing tube top connects four-way connecting tube 9；Described four-way connecting tube 9 its be also associated with oil vacuole device 6, nitrogen cylinder 7 and vacuum pump 8.
Solid material is joined in solid charging hopper 1 by described solid feed inlet 1-1, by rotating described feed-screw 1-2, can control charging rate makes solid reaction raw material joining at the uniform velocity carry out chemical reaction in many mouthfuls of flasks 4, and described delivery tube 1-3 can make solid reaction raw material arrive smoothly in many mouthfuls of flasks 4.
Described thermometer 3 is used to refer to reacting liquid temperature, to guarantee reacting balance.
Described reflux condensing tube 2 is used in condensing reflux course of reaction the steam produced.
The reaction heat that described ice-water bath temperature chamber 5 is unnecessary in being used for absorbing many mouthfuls of flasks 4, is carried out at low ambient temperatures to guarantee to react.
Described vacuum pump 8 is used for discharging the air in reaction system and verifying attachment air-tightness.
Described oil vacuole device 6 is commercially available prod, equipped with the silicone oil not reacted with fluorocarbon alcohol or paraffin inside it.If the process units of fluorocarbon alcohol in this utility model is used for the synthesis of other products, need the liquid in oil vacuole device 6 is replaced with the liquid substance not reacted.
Operation principle of the present utility model i.e. step is:
1, when device air-tightness is good on inspection, open vacuum pump 8, air in system is drained, be full of nitrogen.
2, in the fluorine carbon ester type compound that need to reduce is joined in many mouthfuls of flasks 4, and stirring is opened.
3, in solid charging hopper, reducing agent NaBH is added through charge door 1-14, and lid is built；Mixture of ice and water is added in ice-water bath temperature chamber 5；Being connected with tap water by the water inlet 2-2 of reflux condensing tube 2, outlet 2-1 is connected with drain pipe.
4, rotary feeding screw rod 1-2, carries out chemical reaction, the registration of recording thermometer 3 in slow for the solid in charging hopper 1 and continuous print are joined many mouthfuls of flasks 5；This reaction is exothermic reaction, and when solids feed rates is very fast, boron hydride is more violent with the reaction of fluorine carbon ester type compound, and the temperature of reactant liquor can raise, and now, by rotary feeding screw rod scalable charging rate, thus controls the chemical reaction velocity of material；Steam in many mouthfuls of flasks meets cold liquefaction, and condenser 2 arises that backflow.
Compared with prior art; the beneficial effects of the utility model are: can control solids feed rates by the feed-screw 1-2 on rotary feeding funnel 1; make the solid material in charging hopper at the uniform velocity join in reaction bulb 5; guarantee that the reactivity in system is basically identical; and under the protection of nitrogen, it is able to ensure that product is stable, reduce the appearance of by-product；Package unit is built simply, operates safety, and low cost, is suitable to apply in industry's enlarging production.
The above is only preferred implementation of the present utility model; it should be noted that; for those skilled in the art; on the premise of without departing from this utility model principle; can also make some improvements and modifications, these improvements and modifications also should be regarded as protection domain of the present utility model.
Claims (2)
1. the preparation facilities of a fluorocarbon alcohol, it is characterised in that include that many mouthfuls of flasks, the bottom of described many mouthfuls of flasks are put in ice-water bath temperature chamber；It is connected to solid charging hopper, reflux condensing tube, thermometer on the connector of described many mouthfuls of flasks；The top of described solid charging hopper is the charge door being provided with capping, and the lower section of charge door is the feed-screw for controlling solids feed rates；It is provided with the water inlet of condensed water below described reflux condensing tube, is provided above the outlet of condensed water；Described reflux condensing tube top is connected with airway, and described airway connects has four-way connecting tube, described four-way connecting tube to be also associated with oil vacuole device, nitrogen cylinder and vacuum pump.
The preparation facilities of a kind of fluorocarbon alcohol the most according to claim 1, it is characterised in that the bottom of described thermometer is ground structure, the bottom of this thermometer is placed in described many mouthfuls of flasks in reactant liquor, but does not contacts with the bottom bottle wall of many mouthfuls of flasks.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201521130125.2U CN205435720U (en) | 2015-12-31 | 2015-12-31 | Preparation facilities of fluorine carbon mellow wine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201521130125.2U CN205435720U (en) | 2015-12-31 | 2015-12-31 | Preparation facilities of fluorine carbon mellow wine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN205435720U true CN205435720U (en) | 2016-08-10 |
Family
ID=56598828
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201521130125.2U Expired - Fee Related CN205435720U (en) | 2015-12-31 | 2015-12-31 | Preparation facilities of fluorine carbon mellow wine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN205435720U (en) |
-
2015
- 2015-12-31 CN CN201521130125.2U patent/CN205435720U/en not_active Expired - Fee Related
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160810 Termination date: 20181231 |