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| GB Patent # | GB953906 |
| Link to this page | http://www.wikipatents.com/gb/953906.html |
| Inventor(s) | not available |
| Abstract | Abstract of
GB953906
953,906. Determination of the end-points in the distillation of liquids. BRITISH PETROLEUM CO. Ltd., and W. H. TOPHAM. June 14, 1962 [July 6, 1961], No. 24459/61. Heading B1B. [Also in Division Gl] In an apparatus for the determination of the end-point in the distillation of a liquid, the supply of heat to the still is reduced or cut-off electrically by a temperature controller 8 responsive to a signal received from e.g. a thermocouple 7, located in the still bottom or in the heater, when the temperature of the still bottom rises above a preselected temperature. The overhead temperature is detected and recorded electrically and, preferably, the detector 4 is disconnected from the electric recorder 5 by the action of controller 8 so that the recorder 5 registers a peak value of the overhead temperature at the end point of the distillation. Preferably the heater used is an electrical heater. At the start of the determination, switch 11 is closed, and push button 14 is depressed to connect relay 10 with a source of electricity. When relay 10 is energized, it closes contacts 12, thus maintaining the circuit between relay 10 and the source of electricity. The relay also closes contacts 9, thus supplying electric current to heater 6, and opens contacts 13. When the still bottom reaches the preselected temperature, the controller 8 opens switch 11 to disconnect relay 10. Contacts 9 and 12 then spring open, thus switching off heater 6, and contacts 13 close, thus shorting out detector 4.
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Drawing from GB Patent 953906 |
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Apparatus for use in the control of distillation |
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| Applicant |
BRITISH PETROLEUM COWILLIAM HENRY TOPHAM |
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| Publication Date |
1964-04-02 |
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| Int. Classification |
B01D3/42; G01N25/14; B01D3/42; G01N25/00; |
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| European Classification |
B01D3/42; G01N25/14 |
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| Application number |
GB19610024459 19610706 |
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| Priority number(s) |
GB19610024459 19610706 |
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| Also published as |
DE1498555 (A1) |
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**WARNING** start of CLMS field may overlap end of DESC **.
point in time. The preselected temperature is suitably about30"--70" C. above the expected end point of the distillation.
According to the present invention there is provided apparatus comprising (a) a distillation still, heated by a heater, the still having electrical means responsive to overhead temperature in the still for produced a signal A proportional to the overhead temperature, the still bottom having electrical means responsive to the temperature of the still bottom for producing a signal B proportional to the still bottom temperature (b) a temperature recorder, responsive to signal A and (c) a temperature controller responsive to signal B, adapted to reduce or cut off the supply of energy to the heater when the temperature of the still bottom rise above a pre-selected temperature.
According to a modification of the present invention there is provided apparatus comprising (a) a distillation still, heated by an electrical heater, the still having electrical means responsive to overhead temperature in the still for producing a signal
A proportional to the overhead temperature, the heater having electrical means responsive to the heater temperature for producing a signal C proportional to the heater temperature, (b), a temperature recorder, rsponsive to signal A and (c) a temperature controller, responsive to signal C, adapted to reduce or cut off the supply of electricity to the heater when the temperature of the heater rises above a pre-selected temperature.
Preferably the electrical means comprisethelmocouples.
Preferably the apparatus comprises a relay adapted, whende-energised, to short cut the electrical means responsive to the overhead temperature in the still head.
Preferably the temperature controller is adapted, on receipt of signal B or signal C to de-energise the relay when the temperature of the still bottom or the heater rises above their respective pre-selected values.
Preferably the temperature controller is adapted, on receipt of signal C, to break contacts in a lead supplying electricity to the heater when the temperature of the heater rises above its pre-selected value.
The invention is illustrated by but not limited with reference to Figures 1 and 2 of the drawings accompanying the Provisional Specification where Figure 1 is a schematic diagram of apparatus according to the invention and Figure 2 is circuit diagram of the apparatus described with reference to Figure 1.
With reference to Figure1: -
The apparatus comprises a distillation flask 1 fitted with an inlet 2 and a side arm 3. A thermocouple 4 is fitted into the head of the flask 1 and is connected to a temperature recorder 5. The flask is heated by a low capacity electrical heater 6, fitted with a thermocouple 7 connected to a temperature control 8 which controls the supply of electricity to the heater 6.
With reference to Figures 1 and2: -
A voltage is applied across the heater 6, current flowing to the heater by way of the contacts 9. A voltage is applied across a relay 10, current flowing to the relay by way of the switch 11 and contacts 12. Contacts 13 are provided which are held by the relay 10, when energised, in an open position. A push button 14 is provided to energise the relay 10 at the start of a determination. The button 14, when depressed, shorts out the contacts 12.
When the temperature of the heater 6 as detected by the thermocouple 7 rises above a pre-selected temperature the temperature controller 8 opens the switch 11, thereby de-energising the relay 10 which thereupon (a) opens the contacts 9, thereby switching off the heater 6, (b) closes the contacts 13, thereby shorting out the thermocouple 4 connected to the temperature recorder 5, and (c) opens the contacts 12, thereby ensuring that the relay 10 does not become re-energised merely because the temperature of the heater 6 drops below the pre-selected temperature. The temperature recorder 5 is thus caused to drop to a zero reading; the maximum temperature recorded in the course of a distillation is therefore the end point.
WHAT WE CLAIMIS:-
1. Apparatus comprising (a) a distilla -tion still, heated by a heater, the still having electrical means responsive to overhead temperature in the still for producing a signal A proportional to the overhead temperature, the still bottom having electrical means responsive to the temperature of the still bottom for producing a signal B proportional to the still bottom temperature, (b) a temperature recorder, responsive to signal A and (c) a temperature controller responsive to signal B, adapted to reduce or cut off the supply of energy to the heater when the temperature of the still bottom rises above a pre-selected temperature.
2. Apparatus comprising (a) a distillation still, heated by an electrical heater, the still having electrical means responsive to overhead temperature in the still for producing a signal A proportional to the overhead temperature, the heater having electrical means responsive to the heater temperature for producing a signal C proportional to the heater temperature, (b), a temperature recorder, responsive to signal A and(c) a temperature controller, responsive to signal C adapted to reduce or cut off the supply of electricity to the heater when the
temperature of the heater rises above a pre-selected temperature.
3. Apparatus according to Claim 1 or 2 wherein the electrical means are thermocouples.
4. Apparatus according to any of the preceding claims comprising relayadapted, when de-energised, to short out the electrical means responsive to the overhead temperature in the still head.
5. Apparatus according to Claim 4 wherein the temperature controller, is adapted, on receipt of signal B or signal C to de-energise the relay when the temperature of the still bottom or the heater rises above their respective preselected values.
6. Apparatus according to any of Claims25 comprising contacts in a lead which, in use, supplies electricity to the heater, the contacts being adapted to be broken by the temperature controller on receipt of signal
C when the temperature of the heater rises above its preselected value.
7. Apparatus as hereinbefore described with reference to Figures 1 and 2 of the drawings accompanying the Provisional
Specification.
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COMPLETE SPECIFICATION.
Apparatus for Use in the Control of Distillation.
We, THE BRITISH PETROLEUM COMPANY
LIMITED, of Britannic House, Finsbury
Circus, London, E.C.2, a British Joint-Stock
Corporation, and WILLIAM HENRY TOPHAM,d BP Refinery (Kent) Limited, Isle of
Grain, near Rochester, Kent, and of British nationality, do herebydeclare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the followingstatement:
This invention relatesto apparatus suitable for use in the determination of the end point in the distillation of a liquid. The apparatus, without modification, is suitable for use in the determination of the end points of liquids of end points up to380"
C. The apparatus, with modification for distilling under reduced pressure, is suitable for use in the determination of the end points of liquids of higher end points.
In the large scale continuous distillation of feed stocks which contain many components and which, in consequence, boil over a range of temperatures,small variations in the nature and proportions of components will tend to produce variations in the boiling ranges of the distillation products; these variations will normally be compensated or off set by adjustment of the distillation conditions, usually by control ofthe feedstock supply or of the product withdrawal or by control of the heat input to the distillation column, or through variation in the amount of heat withdrawn from the system, by control of reflux proportions and temperature.
These adjustments are made on the basis of an analysis of the feedstock and/or at least certain of the products.
It has been found that in the case of certain products, for example, special boilingpoint solvents, it is desirable that the products should be distilled to meet end point specifications.
Usually the determination of end points involves the batch laboratory distillation of samples taken over a period of time. This method is very time consuming and involves considerable attention on the part of an operator.
It is an object of this invention to provideimproved apparatus suitable for use in the control of continuous distillation by providing essential information rapidly and accurately. It is a further object to provide improved apparatus for use in the determination of the end point of a liquid.
When a heater is used to heat a still into which a liquid sample has been introduced, the temperatured the still bottom, during distillation, is only slightly above the temperature of the boiling liquid. When the end point of the distillation is reached, however, the temperature of the still bottom increases rapidly.
When a low capacity electrical heater is used to heat a still into which a liquid sample has been introduced the temperature of the heater, during distillation, is only slightly above the temperature of the boiling liquid. When the end point of the distillation is reached, however, the temperature of the heater increases rapidly.
We have found that it is possible to detect the end point of the distillation by detecting either of these rapid increases in temperature and that the increase may be detected by detecting the point in time at which the still bottom temperature or the heater temperature reaches a pre-selected temperature which is above the highest temperature reached tin the course of a distillation. The end point is detected by noting the temperature in the still head at this point in time. The preselected temperature is suitably about30"--70" C. above the expected end point of the distillation.
According to the present invention there is provided apparatus comprising (a) a distillation still, heated by a heater, the still having electrical means responsive to overhead temperature in the still for produced a signal A proportional to the overhead temperature, the still bottom having electrical means responsive to the temperature of the still bottom for producing a signal B proportional to the still bottom temperature (b) a temperature recorder, responsive to signal A and (c) a temperature controller responsive to signal B, adapted to reduce or cut off the supply of energy to the heater when the temperature of the still bottom rise above a pre-selected temperature.
According to a modification of the present invention there is provided apparatus comprising (a) a distillation still, heated by an electrical heater, the still having electrical means responsive to overhead temperature in the still for producing a signal
A proportional to the overhead temperature, the heater having electrical means responsive to the heater temperature for producing a signal C proportional to the heater temperature, (b), a temperature recorder, rsponsive to signal A and (c) a temperature controller, responsive to signal C, adapted to reduce or cut off the supply of electricity to the heater when the temperature of the heater rises above a pre-selected temperature.
Preferably the electrical means comprisethelmocouples.
Preferably the apparatus comprises a relay adapted, whende-energised, to short cut the electrical means responsive to the overhead temperature in the still head.
Preferably the temperature controller is adapted, on receipt of signal B or signal C to de-energise the relay when the temperature of the still bottom or the heater rises above their respective pre-selected values.
Preferably the temperature controller is adapted, on receipt of signal C, to break contacts in a lead supplying electricity to the heater when the temperature of the heater rises above its pre-selected value.
The invention is illustrated by but not limited with reference to Figures 1 and 2 of the drawings accompanying the Provisional Specification where Figure 1 is a schematic diagram of apparatus according to the invention and Figure 2 is circuit diagram of the apparatus described with reference to Figure 1.
With reference to Figure1: -
The apparatus comprises a distillation flask 1 fitted with an inlet 2 and a side arm 3. A thermocouple 4 is fitted into the head of the flask 1 and is connected to a temperature recorder 5. The flask is heated by a low capacity electrical heater 6, fitted with a thermocouple 7 connected to a temperature control 8 which controls the supply of electricity to the heater 6.
With reference to Figures 1 and2: -
A voltage is applied across the heater 6, current flowing to the heater by way of the contacts 9. A voltage is applied across a relay 10, current flowing to the relay by way of the switch 11 and contacts 12. Contacts 13 are provided which are held by the relay 10, when energised, in an open position. A push button 14 is provided to energise the relay 10 at the start of a determination. The button 14, when depressed, shorts out the contacts 12.
When the temperature of the heater 6 as detected by the thermocouple 7 rises above a pre-selected temperature the temperature controller 8 opens the switch 11, thereby de-energising the relay 10 which thereupon (a) opens the contacts 9, thereby switching off the heater 6, (b) closes the contacts 13, thereby shorting out the thermocouple 4 connected to the temperature recorder 5, and (c) opens the contacts 12, thereby ensuring that the relay 10 does not become re-energised merely because the temperature of the heater 6 drops below the pre-selected temperature. The temperature recorder 5 is thus caused to drop to a zero reading; the maximum temperature recorded in the course of a distillation is therefore the end point.
WHAT WE CLAIMIS:-
1. Apparatus comprising (a) a distilla -tion still, heated by a heater, the still having electrical means responsive to overhead temperature in the still for producing a signal A proportional to the overhead temperature, the still bottom having electrical means responsive to the temperature of the still bottom for producing a signal B proportional to the still bottom temperature, (b) a temperature recorder, responsive to signal A and (c) a temperature controller responsive to signal B, adapted to reduce or cut off the supply of energy to the heater when the temperature of the still bottom rises above a pre-selected temperature.
2. Apparatus comprising (a) a distillation still, heated by an electrical heater, the still having electrical means responsive to overhead temperature in the still for producing a signal A proportional to the overhead temperature, the heater having electrical means responsive to the heater temperature for producing a signal C proportional to the heater temperature, (b), a temperature recorder, responsive to signal A and(c) a temperature controller, responsive to signal C adapted to reduce or cut off the supply of electricity to the heater when the
**WARNING** end of DESC field may overlap start of CLMS **.
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