CN103071308A - Rectification head - Google Patents
Rectification head Download PDFInfo
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- CN103071308A CN103071308A CN2013100541578A CN201310054157A CN103071308A CN 103071308 A CN103071308 A CN 103071308A CN 2013100541578 A CN2013100541578 A CN 2013100541578A CN 201310054157 A CN201310054157 A CN 201310054157A CN 103071308 A CN103071308 A CN 103071308A
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- reflux ratio
- ratio control
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- pipe
- control valve
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Abstract
The invention provides a rectification head, which comprises a reflux ratio control pipe, a steam through pipe and a constant-pressure connection pipe, wherein a steam pipeline and a reflux pipeline are arranged between the reflux ratio control pipe and the steam through pipe, a liquid discharging pipe is arranged between the reflux ratio control pipe and the constant-pressure connection pipe, a condenser, a liquid collection hopper, a drainage hopper and an extraction hopper are sequentially arranged in the reflux ratio control pipe from top to bottom, an outlet end of the extraction hopper is communicated with the liquid discharging pipe, the drainage hopper is provided with a magnet, and the position of the magnet is changed under the effect of an electromagnetic relay so as to drive the position of the drainage hopper to be changed, so that the liquid in the drainage hopper can flow into the extraction hopper. Due to the adoption of the rectification head, not only can the reflux ratio be precisely adjusted in the pressure-reduction rectification process, but also the sample can be collected at any time, and a receiving bottle can be replaced at any time.
Description
Technical field
The present invention relates to the rectification and purification technical field, relate in particular to a kind of rectifying head that is applied in the small-sized rectifying column.
Background technology
The small-size glass rectifying column is a kind of rectifying device that is usually used in separating the close compound of boiling point in the laboratory, and the rectifying head is in critical positions in this equipment.The reflux ratio that is used for regulating distillation process that the rectifying head is main.
There is following problem in common rectifying head in the laboratory at present: the first, can not regulate accurately reflux ratio.The second, can not use easily in the rectification under vacuum experiment.After keeping under the decompression state, can not unloading the front-end volatiles receiving flask, and change new receiving flask, the 3rd, there is not sample tap at the rectifying head, can't in distillation process, take a sample.
As everyone knows, composition is usually very complicated in the mixture to be separated, and wherein every kind of material has one fixedly to go out to heat up in a steamer point (normally a scope, for example 157.5 ~ 158.8 ℃) under certain pressure.Need in the stable situation of system pressure, each component in the mixture just can under suitable reflux ratio, be plucked out of successively.If the cut of extraction goes out to heat up in a steamer a some temperature a larger variation (for example temperature descend first rise again) occuring, show next cut out, just need to change a receiving flask this moment.So in this case, we just need to keep in the constant situation of system pressure, the receiving flask that more renews.
Summary of the invention
For the deficiencies in the prior art part, the invention provides a kind of rectifying head, this rectifying head is energy fine adjustment reflux ratio in distillation process, and can keep carrying out sample analysis and replacing receiving flask in the system pressure stability situation.
To achieve these goals, the technology that the present invention adopts is a kind of rectifying head, comprise the reflux ratio control valve, steam siphunculus and constant voltage tube connector, be provided with jet chimney and reflux line between described reflux ratio control valve and the steam siphunculus, be provided with drain pipe between described reflux ratio control valve and the constant voltage tube connector, be provided with successively from top to bottom condenser in the described reflux ratio control valve, the liquid collecting funnel, drainage funnel and extraction funnel, the port of export of described extraction funnel communicates with drain pipe, described drainage funnel is provided with magnet, described magnet changes the position under the effect of electromagnetic relay, thereby the position that drives drainage funnel changes, so that the liquid on the drainage funnel flows in the extraction funnel.
In a preferred embodiment provided by the invention, wherein said drain pipe is provided with probe tube, and described drain pipe and probe tube intersection are provided with stop,threeway.
In a preferred embodiment provided by the invention, wherein said constant voltage tube connector is divided into the upper and lower, is provided with vacuum exhaust pipe between described top and the reflux ratio control valve, and described drain pipe communicates with the bottom.
In a preferred embodiment provided by the invention, wherein said upper and lower connecting place is provided with blow-down pipe, and described blow-down pipe and constant voltage tube connector junction are provided with stop,threeway.
In a preferred embodiment provided by the invention, also be provided with vacuum interface on the wherein said top.
In a preferred embodiment provided by the invention, be provided with thermometer in the wherein said steam siphunculus, described thermometer stretches into the steam siphunculus in the open top end from the steam siphunculus.
In a preferred embodiment provided by the invention, wherein said condenser is selected coil condenser.
Compared with prior art, rectifying head provided by the invention both can be implemented in the rectification under vacuum process can the fine adjustment reflux ratio, again collected specimens and change receiving flask at any time.
Description of drawings
Fig. 1 is the structural representation of rectifying head provided by the invention.
In the accompanying drawing: the lower port of 1-steam siphunculus, 2-steam siphunculus, the upper port of 3-steam siphunculus, 4-jet chimney, the 5-reflux line, 6-condenser, 7-vacuum exhaust pipe, the 8-vacuum interface, 9-stop,threeway, 10-blow-down pipe, 11-constant voltage tube connector, 12-drain pipe, 13-liquid collecting funnel, the 14-drainage funnel, 15-extraction funnel, 16-stop,threeway, the 17-probe tube, the lower port of 18-constant voltage tube connector, 19-reflux ratio control valve.
The specific embodiment
The invention provides a kind of rectifying head, this rectifying head can be in the rectification under vacuum process both can the fine adjustment reflux ratio, collected specimens and change receiving flask at any time again.
By the following examples rectifying head provided by the invention is described in further detail, in order to better understand the content of the invention, but the content of embodiment does not limit the protection domain of the invention
Rectifying head provided by the invention mainly is comprised of reflux ratio control valve 19, steam siphunculus 2 and constant voltage tube connector 11, be provided with jet chimney 4 and reflux line 5 between reflux ratio control valve 19 and the steam siphunculus 2, steam enters in the reflux ratio control valve 19 by jet chimney 4 from steam siphunculus 2, after steam was cooled to liquid, liquid can flow back to steam siphunculus 4 by reflux line 5.Be provided with drain pipe 12 between reflux ratio control valve 19 and the constant voltage tube connector 11, the liquid of collecting in the reflux ratio control valve 19 flows in the constant voltage tube connector 11 by drain pipe 12.
Be provided with successively from top to bottom condenser 6, liquid collecting funnel 13, drainage funnel 14 and extraction funnel 15 in the described reflux ratio control valve 19.The Reflux Control System that liquid collecting funnel 13, drainage funnel 14 and extraction funnel 15 form in the rectifying head.The port of export of extraction funnel 15 communicates with drain pipe 12, described drainage funnel 14 is provided with magnet, can change according to setpoint frequency the orientation of magnet on the drainage funnel 14 by the electromagnetic relay of the energising controlled that an adds frequency, thereby the position that drives drainage funnel 14 changes, so that the liquid on the drainage funnel 14 flows in the extraction funnel 15.Under the effect that does not have magnetic force, drainage funnel 14 is in the natural gravity state, and the liquid in the drainage funnel 14 can flow to reflux line 5.Having under the magneticaction, the position of drainage funnel 14 changes, and lower the chewing of funnel just aimed at extraction funnel 15, so just can play the effect of control reflux ratio.Drain pipe 12 is provided with probe tube 17, and described drain pipe 12 is provided with stop,threeway with probe tube 17 intersections.
Constant voltage tube connector 11 is divided into the upper and lower, is provided with vacuum exhaust pipe 7 between described top and the reflux ratio control valve 19, also is provided with vacuum interface 8 on the described top, and described drain pipe 12 communicates with the bottom.Described upper and lower connecting place is provided with blow-down pipe 10, and described blow-down pipe 10 and constant voltage tube connector 11 junctions are provided with stop,threeway.
Can also be provided with thermometer in that steam siphunculus 2 is interior, described thermometer stretches into the steam siphunculus 2 in the open top end from steam siphunculus 2.Can read into the temperature of cooling steam intuitively by thermometer.
Be provided with stop,threeway in the rectifying head provided by the invention, can effectively control the channel direction in the rectifying head.Can realize in the use procedure only having the arbitrary portion pipeline communicate, all pipeline communicate or each pipeline between not connected, by regulating the channel direction of stop,threeway, can take a sample easily and change receiving flask.
The working condition of rectifying head provided by the invention is described by the following examples:
At first, stop,threeway 9 and stop,threeway 16 all are adjusted to not connected state, and lower port 18 places of probe tube 17 and constant voltage tube connector all connect receiving flask, and drainage funnel 14 is not having magneticaction situation (electromagnetic relay that namely adds is off-position).Blow-down pipe 10 is connected the vacuum oil pump, regulate pressure at 5mmHg.At first, steam enters the rectifying head from the lower port 1 of steam siphunculus, enters condenser system through steam siphunculus 2 and jet chimney 4, and the device 6 that is condensed is condensed into liquid.Then, liquid enters liquid collecting funnel 13 under action of gravitation, in drainage funnel 14 and the reflux line 5.Finally, be back in the rectifying column by lower port 1, i.e. the infinite reflux state.Along with the carrying out of infinite reflux, the temperature of the upper port 3 of steam siphunculus begins to stablize 70 ℃, and be adjusted to lower-left communicating state with stop,threeway 16 this moment, and the reflux ratio of drainage funnel 14 is adjusted to 10:1.At this moment, probe tube 17 receiving flasks just have liquid and flow into, and when the amount of sample in the receiving flask is enough analyzed, at once stop,threeway 9 are adjusted to the bottom right communicating state, and stop,threeway 16 is adjusted to the bottom right state.At this moment, just can take off probe tube 17, carry out at once purity analysis (purity of A).If purity is undesirable, then strengthen reflux ratio, for example be transferred to 15:1 from 10:1, the analysis of resampling is until meet the requirements.
When if purity reaches requirement, at once stop,threeway 9 is adjusted to up and down communicating state, stop,threeway 16 is adjusted to left and right sides communicating state, and at this moment, the sample A of the purity that meets the requirements will be accepted by the lower port 18 of constant voltage tube connector.After the A in the mixture separated fully, the temperature indication of upper port 3 can change.At this moment, just need to change the receiving flask at lower port 18 places.At first regulate stop,threeway 16 and be not connected state, again stop,threeway 9 is adjusted to the bottom right communicating state, so just can take off the receiving flask at port one 8 places, the receiving flask that more renews.After changing the receiving flask at lower port 18 places, again stop,threeway 9 is adjusted to not connected state.When the temperature stabilization at upper port 3 places during at 78 ℃, repeat again above-mentioned step from probe tube 17 samplings, carry out sample analysis.When analysis result meets the requirements, with regard to extraction sample B, otherwise, continue to strengthen the reflux ratio at drainage funnel 14 places, until meet the requirements.Same process, sample C also can separated extraction.By above process, utilize the rectifying head provided by the invention can easily be with A, B, the C mixture separates.
More than specific embodiments of the invention are described in detail, but it is as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that this practicality is carried out and substituting also all among category of the present invention.Therefore, not breaking away from impartial conversion and the modification of doing under the spirit and scope of the present invention, all should contain within the scope of the invention.
Claims (7)
1. rectifying head, comprise reflux ratio control valve (19), steam siphunculus (2) and constant voltage tube connector (11), be provided with jet chimney (4) and reflux line (5) between described reflux ratio control valve (19) and the steam siphunculus (2), be provided with drain pipe (12) between described reflux ratio control valve (19) and the constant voltage tube connector (11), it is characterized in that, be provided with successively from top to bottom condenser (6) in the described reflux ratio control valve (19), liquid collecting funnel (13), drainage funnel (14) and extraction funnel (15), the port of export of described extraction funnel (15) communicates with drain pipe (12), described drainage funnel (14) is provided with magnet, described magnet changes the position under the effect of electromagnetic relay, thereby the position that drives drainage funnel (14) changes, so that the liquid on the drainage funnel (14) flows in the extraction funnel (15).
2. described rectifying head according to claim 1 is characterized in that described drain pipe (12) is provided with probe tube (17), and described drain pipe (12) is provided with stop,threeway with probe tube (17) intersection.
3. described rectifying head according to claim 1 is characterized in that described constant voltage tube connector (11) is divided into the upper and lower, is provided with vacuum exhaust pipe (7) between described top and the reflux ratio control valve (19), and described drain pipe (12) communicates with the bottom.
4. described rectifying head according to claim 3 is characterized in that described upper and lower connecting place is provided with blow-down pipe (10), and described blow-down pipe (10) and constant voltage tube connector (11) junction are provided with stop,threeway.
5. described rectifying head according to claim 3 is characterized in that, also is provided with vacuum interface (8) on the described top.
6. described rectifying head according to claim 1 is characterized in that be provided with thermometer in the described steam siphunculus (2), described thermometer stretches into the steam siphunculus (2) in the open top end from steam siphunculus (2).
7. described rectifying head according to claim 1 is characterized in that described condenser (6) is selected coil condenser.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100541578A CN103071308A (en) | 2013-02-20 | 2013-02-20 | Rectification head |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100541578A CN103071308A (en) | 2013-02-20 | 2013-02-20 | Rectification head |
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| CN103071308A true CN103071308A (en) | 2013-05-01 |
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| CN2013100541578A Pending CN103071308A (en) | 2013-02-20 | 2013-02-20 | Rectification head |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104771923A (en) * | 2015-03-16 | 2015-07-15 | 泰州市华晨仪器有限公司 | Water quality positive-pressure distillation instrument |
| CN104906822A (en) * | 2015-06-02 | 2015-09-16 | 湖南湘江关西涂料有限公司 | Device and method for eliminating and recycling organic solvent from cathode electrophoresis emulsion |
| CN105688433A (en) * | 2016-02-24 | 2016-06-22 | 佛山高富中石油燃料沥青有限责任公司 | Vacuum distillation instrument using segmentation cutting |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2098873A (en) * | 1981-05-19 | 1982-12-01 | Coal Industry Patents Ltd | Distillation apparatus |
| CN1114305A (en) * | 1994-06-09 | 1996-01-03 | 武汉大学 | Rectifying process for preparing ethyl lactate |
| CN201445822U (en) * | 2009-04-14 | 2010-05-05 | 南京师范大学 | External condensing type reflux splitter |
| CN102441289A (en) * | 2012-02-02 | 2012-05-09 | 常州市常顺精细化学品有限公司科技研究所 | Cluster rectification device |
| CN102909106A (en) * | 2012-11-05 | 2013-02-06 | 济南大学 | Reduced-pressure distillation device |
| CN203154857U (en) * | 2013-02-20 | 2013-08-28 | 上海煦旻化工科技发展有限公司 | Rectifying head |
-
2013
- 2013-02-20 CN CN2013100541578A patent/CN103071308A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2098873A (en) * | 1981-05-19 | 1982-12-01 | Coal Industry Patents Ltd | Distillation apparatus |
| CN1114305A (en) * | 1994-06-09 | 1996-01-03 | 武汉大学 | Rectifying process for preparing ethyl lactate |
| CN201445822U (en) * | 2009-04-14 | 2010-05-05 | 南京师范大学 | External condensing type reflux splitter |
| CN102441289A (en) * | 2012-02-02 | 2012-05-09 | 常州市常顺精细化学品有限公司科技研究所 | Cluster rectification device |
| CN102909106A (en) * | 2012-11-05 | 2013-02-06 | 济南大学 | Reduced-pressure distillation device |
| CN203154857U (en) * | 2013-02-20 | 2013-08-28 | 上海煦旻化工科技发展有限公司 | Rectifying head |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104771923A (en) * | 2015-03-16 | 2015-07-15 | 泰州市华晨仪器有限公司 | Water quality positive-pressure distillation instrument |
| CN104771923B (en) * | 2015-03-16 | 2016-09-07 | 泰州市华晨仪器有限公司 | A kind of water quality malleation distillation apparatus |
| CN104906822A (en) * | 2015-06-02 | 2015-09-16 | 湖南湘江关西涂料有限公司 | Device and method for eliminating and recycling organic solvent from cathode electrophoresis emulsion |
| CN104906822B (en) * | 2015-06-02 | 2017-03-22 | 湖南湘江关西涂料有限公司 | Device and method for eliminating and recycling organic solvent from cathode electrophoresis emulsion |
| CN105688433A (en) * | 2016-02-24 | 2016-06-22 | 佛山高富中石油燃料沥青有限责任公司 | Vacuum distillation instrument using segmentation cutting |
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Application publication date: 20130501 |