CN100486706C - Distillation dewatering set and its dewatering process using it - Google Patents
Distillation dewatering set and its dewatering process using it Download PDFInfo
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- CN100486706C CN100486706C CNB2005101347000A CN200510134700A CN100486706C CN 100486706 C CN100486706 C CN 100486706C CN B2005101347000 A CNB2005101347000 A CN B2005101347000A CN 200510134700 A CN200510134700 A CN 200510134700A CN 100486706 C CN100486706 C CN 100486706C
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Abstract
The present invention provides a kind of distillation dewatering set and its dewatering process. The distillation dewatering set includes one distilling flask, one distilling column with heater, and one condensator. During distillation dewatering with the distillation dewatering set, the distilling column may be heated with the heater, so as to avoid condensation of water vapor in the distilling column and avoid explosive boiling in the distilling flask caused by condensed water dropping.
Description
Technical field
The dewatering that the invention relates to a kind of distillation dehydration device and use this device.
Background technology
In carrying out crude oil evaluation or analysis of oil process,, then can have a direct impact the sample determination result if contain water in the sample.For example, the analysis projects such as ash content of 100 ℃ viscosity, crude oil and heavy oil of former oil flash point, heavy oil can't be carried out, though the density of some project such as sample, condensation point can be measured, measurement result is inaccurate.Therefore, if contain water in the sample, before carrying out crude oil evaluation and analysis of oil, dewater.At present the dewatering of crude oil, viscous crude and heavy oil is generally comprised microwave method, ultrasonic method, centrifugal process, airtight electricity and take off method, autoclave pressure evaporation and distillation dehydration method.Wherein autoclave pressure evaporation and distillation dehydration method are more commonly used.
The distillation dehydration method steams the gasoline component in water and the crude oil, and the interface of water and gasoline is clear, can separate fully.The distillation dehydration method is generally carried out in the distillation dehydration device.For example, the oil instrument, 1999,13 (1), 46-47 discloses a kind of indoor SHYT type viscous crude fast dewatering device, and this dehydrator adopts atmospheric distillation.As shown in Figure 1, this dehydrator comprises condenser 1, separator tube 2, return valve 3, discharging valve 4, oil vessel 5, interior heating resistor 6, outer heating resistor 7 and control section 8, wherein, oil vessel 5 is made by transparent quartz glass, and the top of oil vessel 5 has a segment pipe to link to each other with condenser 1 (generally this segment pipe being called distillation column).
In dehydration, wet crude is placed in the oil vessel 5, heat through interior heating resistor 6 and outer heating resistor 7, light components and water in (common 80 ℃-120 ℃) crude oil will be evaporated at a certain temperature, the mist that is evaporated is cooled into liquid state one by one and is deposited in the separator tube 2 along upwards migration of condenser 1.When using this dehydrator that viscous crude and heavy oil are dewatered, because viscous crude and heavy oil light fraction are few, water can not in time be taken out of, and is condensate on the distillation column.But the sample temperature in the oil vessel 5 constantly raises, and when sample temperature surpassed 100 ℃, the condensing drip on the distillation column was fallen in the oil vessel 5, and bumping appears in gasification rapidly, expansion easily.
Summary of the invention
The objective of the invention is to overcome the shortcoming that bumping appears in existing distillation dehydration device easily, a kind of distillation dehydration device that does not have bumping is provided.
Another object of the present invention provides the dewatering that uses this distillation dehydration device.
The invention provides a kind of distillation dehydration device, this device comprises cucurbit, distillation column and condenser, and wherein, distillation column is equipped with the distillation column heater.
The present invention also provides a kind of distillation dehydration method, and this method comprises the aqueous specimen in the cucurbit is heated, and makes water be transformed into steam; Steam enters condenser by distillation column, and condensation in condenser wherein, in the process that the aqueous specimen in the cucurbit is heated, is heated distillation column.
Because the distillation column of distillation dehydration device provided by the invention is equipped with the distillation column heater, therefore in the distillation dehydration process, can heat distillation column by the distillation column heater, prevent that steam is condensed into water droplet and falls in the cucurbit on distillation column, thereby avoid occurring bumping.
Description of drawings
Fig. 1 is the schematic diagram of the existing dehydrator of expression;
Fig. 2 is an expression distillation dehydration schematic representation of apparatus provided by the invention;
Fig. 3 is an expression distillation dehydration schematic representation of apparatus provided by the invention.
The specific embodiment
Below in conjunction with Fig. 2 and Fig. 3 distillation dehydration device provided by the invention is described in detail.
As shown in Figure 2, distillation dehydration device provided by the invention comprises cucurbit 11, distillation column 12 and condenser 13, and wherein, distillation column 12 is equipped with distillation column heater 14.
According to distillation dehydration device provided by the invention, in use, distillation column 12 is installed in cucurbit 11 tops and links to each other with cucurbit 11, distillation column 12 links to each other with condenser 13.
According to distillation dehydration device provided by the invention, there is no particular limitation to the shape of distillation column heater 14 and position, as long as can play the effect to the distillation column heating.Under the preferable case, distillation column heater 14 is a heating jacket, is enclosed within whole outer surfaces of distillation column 12, can heat whole distillation column like this, prevents steam condensation on the distillation column inwall.
In order accurately to control the temperature of distillation column 12, distillation column 12 can be equipped with distillation column temperature controller 16 and distillation column temperature sensor 17.Distillation column temperature sensor 17 is installed in the inside of distillation column, and is preferably mounted at the inner and upper of distillation column.Distillation column temperature controller 16 and distillation column temperature sensor 17 can use conventional temperature controller and temperature sensor respectively.Distillation column temperature sensor 17 is preferably the gas phase temperature sensor.Distillation column temperature controller 16 is electrically connected with distillation column temperature sensor 17 and distillation column heater 14 respectively.Distillation column temperature sensor 17 can be surveyed the temperature of distillation column 12, and temperature and design temperature that distillation column temperature controller 16 is surveyed distillation column temperature sensor 17 compare, control distillation column heater 14.
Can use various external heat sources such as electric furnace to cucurbit 11 heating, under the preferable case, cucurbit 11 is equipped with cucurbit heater 15.In order accurately to control the temperature of the sample in the cucurbit 11, cucurbit temperature controller 18 and cucurbit temperature sensor 19 can be installed on cucurbit.Cucurbit temperature sensor 19 can be installed in cucurbit 11 inside, also can be installed between cucurbit heater 15 and the cucurbit 11 (as shown in Figures 2 and 3).Cucurbit temperature controller 18 and cucurbit temperature sensor 19 can use conventional temperature controller and temperature sensor respectively.Cucurbit temperature sensor 19 is preferably the liquidus temperature sensor.Cucurbit temperature controller 18 is electrically connected with cucurbit temperature sensor 19 and cucurbit heater 15 respectively.Cucurbit temperature sensor 19 can be surveyed the temperature of sample in the cucurbit 11, and temperature and design temperature that cucurbit temperature controller 18 is surveyed cucurbit temperature sensor 19 compare, control cucurbit heater 15.
There is no particular limitation to the shape of cucurbit 11 in the present invention, for example can be sphere as shown in Figure 2.Under the preferable case, as shown in Figure 3, cucurbit 11 is a column tube.In this case, cucurbit heater 15 is preferably heating jacket, is enclosed within whole outer surfaces of cucurbit 11, can heat whole cucurbit like this, prevents steam condensation on the cucurbit inwall.And compare with the spherical cucurbit with volume, the heating surface (area) (HS of cylindricality cucurbit is big, is convenient to transmit heat, makes sample temperature even.Cucurbit 11 can be integrated with distillation column 12, for example with the bottom of column tube as cucurbit 11, the top of column tube is as distillation column 12.Cucurbit 11 can also be installed sample valve 22 in the bottom, and dehydration is opened sample valve 22 after finishing, and can collect the sample after the dehydration easily.
Be communicated with by conduit between distillation column 12 and the condenser 13.In order to prevent condensate return in distillation column 12, this conduit is tilted to down (be positioned at one section of condenser below).The structure of condenser 13 and principle have been conventionally known to one of skill in the art, there is no particular limitation to condenser 13 in the present invention, can use existing various condenser, as dividing wall type condenser, submerged condenser, spraying condenser and mixing condenser, condenser pipe belongs to a kind of common dividing wall type condenser, and the present invention preferably uses condenser pipe.
Distillation dehydration device provided by the invention can also comprise separator tube 20, and this separator tube is installed in the below of condenser 13.The liquid of condensation flow into the separator tube 20 from condenser 13 and since the liquid of condensation comprise water and with the inconsistent liquid of water, so the liquid of condensation layering in separator tube 20.The bottom of separator tube 20 can also be equipped with valve 21, can separate with water and with the inconsistent liquid of water by this valve 21.Separator tube 20 can also have the condensation function, in this case, preferably uses condenser pipe as separator tube 20.It is subzero below 20 degrees centigrade that the temperature of separator tube 20 can reach, and for example uses the subzero cooling fluid below 20 degrees centigrade that produces by refrigeration machine in as the condenser pipe of separator tube 20.
Describe distillation dehydration method provided by the invention in detail below with reference to Fig. 2 and Fig. 3.
Distillation dehydration method provided by the invention comprises the aqueous specimen in the cucurbit 11 is heated, and makes water be transformed into steam; Steam enters condenser 13 by distillation column 12, and condensation in condenser 13 wherein, in the process that the aqueous specimen in the cucurbit 11 is heated, is heated distillation column 12.
Described aqueous specimen can be the sample of various suitable use distillation dehydration methods.In the present invention, aqueous specimen comprises various oil products, as crude oil, viscous crude and heavy oil.
When distillation column 12 is equipped with distillation column temperature controller 16 and distillation column temperature sensor 17 and cucurbit 11 cucurbit heater 15, cucurbit temperature controller 18 and cucurbit temperature sensor 19 is installed, effect by said temperature controller, temperature sensor and heater, at 130 ℃ or be higher than 130 ℃, preferably in 130-200 ℃ temperature range, heat the aqueous specimen in the cucurbit 11, and the temperature that makes distillation column 12 remains on 130 ℃ or be higher than 130 ℃, preferably at 130-200 ℃.For example,, the aqueous specimen in the cucurbit 11 is slowly heated, make the heating rate of sample be not more than 5 ℃/minute, be preferably 1-4 ℃/minute in the starting stage of heating up; Distillation column 12 heats up with the heating rate greater than 5 ℃/minute simultaneously, and therefore in the starting stage, the temperature of distillation column 12 is greater than the temperature of cucurbit 11.For example, when the temperature of distillation column 12 reached 130 ℃, the temperature of cucurbit 11 may only be elevated to 70 ℃.When the temperature of distillation column 12 reaches 130 ℃ or when being higher than 130 ℃, make the temperature of distillation column 12 remain on 130 ℃ or be higher than 130 ℃, preferably in 130-200 ℃ temperature range.
As shown in Figure 3, when cucurbit 11 is a column tube, when cucurbit 11 can be integrated with distillation column 12, as cucurbit 11, the top of column tube was as distillation column 12 with the bottom of column tube.Effect by temperature controller, temperature sensor and heater, at 130 ℃ or be higher than 130 ℃, the preferred aqueous specimen in the heating column pipe bottom in 130-200 ℃ temperature range, and make the temperature on column tube top remain on 130 ℃ or be higher than 130 ℃, preferably at 130-200 ℃.For example, the starting stage heating up, make the heating rate of column tube bottom be not more than 5 ℃/minute, the heating rate on column tube top is greater than 5 ℃/minute, and therefore in the starting stage, the temperature on column tube top is greater than the temperature of column tube bottom.For example, when the temperature on column tube top reached 130 ℃, the temperature of column tube bottom may only be elevated to 70 ℃.When the temperature of column tube bottom reaches 130 ℃ or when being higher than 130 ℃, make the temperature of column tube bottom remain on 130 ℃ or be higher than 130 ℃, preferably in 130-200 ℃ temperature range.
According to distillation dehydration method provided by the invention, when aqueous specimen was crude oil, viscous crude and/or heavy oil, the process of distillation can be with reference to GB/T2538 crude oil test method(s).For example, the aqueous specimen in the cucurbit 11 is heated to 130-200 ℃, and under this temperature, stopped 10-20 minute, all steam to guarantee the water in the sample.
In still-process, water and light component in the sample are transformed into gaseous form, flow in the condenser 13.When condenser 13 was condenser pipe, the temperature of condenser pipe was lower than 5 ℃, was preferably below-20 ℃.
When the distillation dehydration device that provides when invention comprised separator tube 20, the liquid of condensation flow into the separator tube 20 from condenser 13.The liquid of condensation is divided into two-layer up and down in separator tube 20, and the upper strata is the little light component of proportion, and lower floor is heavy water.When the bottom of separator tube 20 is equipped with valve 21, water and light component can be separated by this valve 21.The temperature of separator tube 20 is set to earlier than higher temperature such as 5-20 ℃, after water being bled off by valve 21, temperature that can separator tube 20 is set to lower temperature as-5 ℃ to-40 ℃, can avoid the volatilization of light component like this, and be adsorbed on the ice that water on the separator tube inwall becomes solid, do not flow out, improved the separative efficiency of light component and water with light component.The light component that flows out can be joined again in the sample after the distillation.Through behind the distillation dehydration, the water content in the sample is less than 0.03 weight %.
Below by embodiment the present invention is described in more detail.
This embodiment is used to illustrate distillation dehydration device and method provided by the invention.
In dry oil, add entry, obtain the aqueous specimen that water content is 5 weight %.As shown in Figure 2, be that the aqueous specimen of 5 weight % is put in the cucurbit 11 with water content.Open distillation column heater 14, open cucurbit heater 15 simultaneously, control distillation column heater 14 and cucurbit heater 15 respectively by distillation column temperature controller 16 and cucurbit temperature controller 18, cucurbit 11 is heated up with 2 ℃/minute speed, when the temperature of distillation column temperature sensor 17 detection distillation columns 12 is 135 ℃, make the temperature of distillation column 12 remain on 135 ℃.Continuation, stopped 18 minutes under this temperature when the temperature of cucurbit temperature sensor 19 detection cucurbits 11 is 135 ℃ cucurbit 11 heating.The temperature of distillation column 12 is consistent with the temperature of cucurbit 11.
Water and light component in the aqueous specimen are transformed into gaseous form, flow in the condenser 13.Being connected with temperature in the partition of condenser pipe 13 is subzero 40 ℃ cooling fluid (cooling fluid is that volume ratio is water and the ethylene glycol of 1:1), and the water of gaseous state and light component be the liquefy form in condenser pipe, and flow in the separator tube 20.Valve 21 is opened in the layering in separator tube 20 of the liquid of condensation, and the water of lower floor is bled off.Then, continuing to feed temperature in the partition of separator tube is subzero 30 ℃ cooling fluid (cooling fluid is that volume ratio is water and the ethylene glycol of 1:1), becomes after the ice being adsorbed on water on the separator tube inwall, opens valve 21, and the light component of liquid state is emitted.
At last the light component of the above-mentioned liquid state that obtains from separator tube 20 is mixed the crude oil after obtaining dewatering with remaining sample the cucurbit 11.The water content of measuring the crude oil after dewatering according to the method for stipulating in the GB/T8929 detecting crude oil water content method is less than 0.03 weight % (being limited to 0.03 weight % under the detection of this method of testing).
This embodiment is used to illustrate distillation dehydration device and method provided by the invention.
In anhydrous heavy oil, add entry, obtain the aqueous specimen that water content is 5 weight %.As shown in Figure 3, the aqueous specimen that is 5 weight % with the above-mentioned water content that is obtained by anhydrous heavy oil is put in the cucurbit 11.Open distillation column heater 14, open cucurbit heater 15 simultaneously, control distillation column heater 14 and cucurbit heater 15 respectively, cucurbit 11 is heated up with 2 ℃/minute speed by distillation column temperature controller 16 and cucurbit temperature controller 18.When the temperature of distillation column temperature sensor 17 detection distillation columns 12 is 130 ℃, make the temperature of distillation column 12 remain on 130 ℃.Continuation is to cucurbit 11 heating, when the temperature of surveying cucurbits 11 when cucurbit temperature sensor 19 is 130 ℃, makes distillation column 12 and cucurbit 11 all with 2 ℃/minute speed intensification.The temperature of surveying cucurbit 11 when cucurbit temperature sensor 19 is 185 ℃, when the temperature that distillation column temperature sensor 17 is surveyed distillation column 12 is 185 ℃, stops 12 minutes under this temperature.The temperature of distillation column 12 is consistent with the temperature of cucurbit 11.
Water and light component in the aqueous specimen are transformed into gaseous form, flow in the condenser 13.Being connected with temperature in the partition of condenser pipe 13 is subzero 10 ℃ cooling fluid (cooling fluid is that volume ratio is water and the ethylene glycol of 1:1), and the water of gaseous state and light component be the liquefy form in condenser pipe, and flow in the separator tube 20.The layering in separator tube 20 of the liquid of condensation at 20 ℃, is opened valve 21, and the water of lower floor is bled off.Then, continuing to feed temperature in the partition of separator tube is subzero 10 ℃ cooling fluid (cooling fluid is that volume ratio is water and the ethylene glycol of 1:1), becomes after the ice being adsorbed on water on the separator tube inwall, opens valve 21, and the light component of liquid state is emitted.
At last, open sample valve 22 remaining sample in the cucurbit 11 is emitted, and described remaining sample is mixed the heavy oil after obtaining dewatering with the light component of the above-mentioned liquid state that obtains from separator tube 20.The water content of measuring the crude oil after dewatering according to the method for stipulating in the GB/T8929 detecting crude oil water content method is less than 0.03 weight %.
The property testing of oil product
Measure the various character of the crude oil of the dehydration that dry oil and embodiment 1 obtain respectively according to the method for stipulating in the GB/T2538 crude oil test method(s), measurement result is as shown in table 1.
Table 1
Measure the various character of the heavy oil of the dehydration that anhydrous heavy oil and embodiment 2 obtain respectively according to the method for stipulating in the GB/T2538 crude oil test method(s), measurement result is as shown in table 2.
Table 2
Find out from the data of table 1 and table 2, adopt the physicochemical properties of the sample after distillation dehydration device provided by the invention and dewatering dewater and the original dry-out sample that does not add water to compare, almost do not have difference.Show that sample after the dehydration satisfies the requirement to the sample moisture content of crude oil evaluation (GB/T17280 crude distillation standard test method requires crude oil water content less than 0.1%) and analysis of oil fully.
Claims (15)
1, a kind of distillation dehydration device, this device comprises cucurbit, distillation column and condenser, it is characterized in that, distillation column is equipped with the distillation column heater, distillation column also is equipped with distillation column temperature controller and distillation column temperature sensor, the distillation column temperature sensor is installed in the inside of distillation column, and the distillation column temperature controller is electrically connected with distillation column temperature sensor and distillation column heater respectively.
2, distillation dehydration device according to claim 1 wherein, in use, is contained in cucurbit top with distillation column and links to each other with cucurbit, and distillation column links to each other with condenser.
3, distillation dehydration device according to claim 1, wherein, the distillation column heater is a heating jacket, this heating jacket is sleeved on the outer surface of distillation column.
4, distillation dehydration device according to claim 1, wherein, the distillation column temperature sensor is the gas phase temperature sensor.
5, distillation dehydration device according to claim 1, wherein, cucurbit is equipped with cucurbit heater, cucurbit temperature controller and cucurbit temperature sensor, and the cucurbit temperature controller is electrically connected with cucurbit temperature sensor and cucurbit heater respectively.
6, distillation dehydration device according to claim 1, wherein, cucurbit is a column tube, and cucurbit is equipped with the cucurbit heater, and the cucurbit heater is a heating jacket, and this heating jacket is sleeved on the outer surface of cucurbit.
7, distillation dehydration device according to claim 1, wherein, cucurbit is a column tube, and cucurbit and distillation column are integrated, and column tube top is distillation column, and the column tube bottom is a cucurbit.
8, distillation dehydration device according to claim 1, wherein, the bottom of cucurbit is equipped with sample valve.
9, distillation dehydration device according to claim 1, wherein, condenser is a condenser pipe.
10, distillation dehydration device according to claim 1, wherein, this device also comprises separator tube, the bottom of separator tube is equipped with valve, in use, this separator tube is connected the below of condenser.
11, a kind of distillation dehydration method, this method comprise the heating of the aqueous specimen in the cucurbit, make water be transformed into steam; Steam enters condenser by distillation column, condensation in condenser, it is characterized in that, the distillation dehydration device that described distillation dehydration process is used comprises cucurbit, distillation column and condenser, distillation column links to each other above cucurbit and with cucurbit, distillation column links to each other with condenser, distillation column is equipped with the distillation column heater, distillation column also is equipped with distillation column temperature controller and distillation column temperature sensor, the distillation column temperature sensor is installed in the inside of distillation column, and the distillation column temperature controller is electrically connected with distillation column temperature sensor and distillation column heater respectively; In process to the heating of the aqueous specimen in the cucurbit, the distillation column temperature sensor is surveyed the temperature of distillation column, the distillation column temperature controller compares the temperature and the design temperature of distillation column, according to comparative result control distillation column heater, distillation column is heated.
12, method according to claim 11, wherein, the design temperature of distillation column is at least 130 ℃.
13, method according to claim 12, wherein, the design temperature of distillation column is 130-200 ℃.
14, method according to claim 11, wherein, the distillation dehydration device also comprises separator tube, separator tube is connected the below of condenser, the bottom of separator tube is equipped with valve, the liquid of condensation flow into the separator tube from condenser, by this valve water in the liquid of condensation and light component is separated.
15, method according to claim 11, wherein, cucurbit is a column tube, and cucurbit and distillation column are integrated, and column tube top is distillation column, and the column tube bottom is a cucurbit, aqueous specimen heats in the cucurbit of bottom.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103091474B (en) * | 2011-10-27 | 2015-11-25 | 中国石油化工股份有限公司 | A kind of device for measuring heavy distillate boiling range |
| CN103091475B (en) * | 2011-10-27 | 2015-11-25 | 中国石油化工股份有限公司 | A kind of method measuring fraction oil of petroleum boiling range |
| CN102645526B (en) * | 2012-05-10 | 2015-03-11 | 大连交通大学 | Device for determining water content in petroleum products by using distillation method and method for device |
| CN104155168A (en) * | 2014-06-18 | 2014-11-19 | 中国石油天然气股份有限公司 | Laboratory preparation method of trace water contained thickened oil and trace thickened oil dehydrating instrument |
| CN105623706B (en) * | 2014-10-27 | 2017-07-25 | 中国石油化工股份有限公司 | Crude oil continuous still dewatering |
| CN105623707B (en) * | 2014-10-27 | 2017-10-03 | 中国石油化工股份有限公司 | Continuous still dehydrator and crude oil continuous still dehydration device |
| CN107340312A (en) * | 2017-07-07 | 2017-11-10 | 四川西普石油物资装备有限公司 | The method for avoiding producing bumping in way of distillation measure crude oil water content |
| CN108091229B (en) * | 2018-01-30 | 2023-08-01 | 福州大学 | Double-liquid system gas-liquid equilibrium phase diagram boiling point instrument with intelligent temperature compensation system |
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- 2005-12-19 CN CNB2005101347000A patent/CN100486706C/en active Active
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