CN101121898A - Fast emulsion breaking method - Google Patents
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- CN101121898A CN101121898A CNA2007100123177A CN200710012317A CN101121898A CN 101121898 A CN101121898 A CN 101121898A CN A2007100123177 A CNA2007100123177 A CN A2007100123177A CN 200710012317 A CN200710012317 A CN 200710012317A CN 101121898 A CN101121898 A CN 101121898A
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Abstract
The invention relates to a rapid emulsion breaking method, including microwave radiation. Emulsion breaker is added according to the water content of the rolly oil (calculated by weight percent), the mass ratio of the water and emulsion breaker is 1:0.5*10-4 to 5*10-4, and microwave is adopted for emulsion breaking. The emulsion breaker is one or more than two types of mixtures of polyamine polyoxy-propylene polyoxyethylene ether, resin polyoxy-propylene polyoxyethylene ether, higher-alcohol initiator emulsion breaker or propylene glvcol emulsion breaker. The microwave radiation and microwave radiation frequency are 2450MHz or 915MHz. Under the synergistic reaction, water-in-oil emulsion liquid is broken within a relatively short period, a bigger anhydration rate is achieved, and the emulsion-breaking efficiency is improved. In the circumstance of a little emulsion breaker, microwave radiation breaking method can be adopted, and the emulsion breaking speed is increased by 1-2 orders of magnitude compared with the traditional emulsion breaking by heating. The method is easy to implement, energy efficient, rapid in emulsion breaking, and the emulsion breaking effect is good.
Description
Technical field:
The present invention relates to a kind of breaking method of emulsion, particularly a kind of breaking method to water-in-oil type emulsion.
Background technology:
Dehydrating of crude oil always is one of most important link in oil production and the processing.The existence of oil-water emulsion can increase the burden of oil gas accumulating, easily causes pipeline corrosion, and it is unfavorable that refining of petroleum is utilized.For production is normally carried out, these milk sap must be processed, thereby reach oily water separation.And the key of dehydrating of crude oil is the breakdown of emulsion of crude oil emulsion.
Present breaking method mainly contains: 1. settling process; 2. heating or distillation under normal pressure; 3. heating under high pressure or distillation; 4. electric power; 5. chemical; 6. centrifugal; 7. filter; 8. ultrasonic wave.Domestic most employing chemical demulsification, this method exist the medicament add-on big, take off deficiencies such as back water quality inferiority, contaminate environment, equipment be perishable, and other some ordinary methods, reduce greatly again on breakdown of emulsion efficient as gravity settling, therefore, be badly in need of seeking a kind of new, breaking method efficiently.
Klaika and Wolf have at first proposed the notion of microwave radiation breakdown of emulsion.Klaika has carried out the test in place of microwave radiation breakdown of emulsion in Louisiana, United States (Louisana) oil field, use microwave radiation 18.2h, and the total energy of consumption is 417.5kWh, and separation of emulsion goes out 146 barrels of (bbls) corrected oils and 42 barrels of (bbls) clear water.Fang etc. have reported that the result shows that under suitable condition dehydration rate can reach more than 80% to the microwave radiation breakdown of emulsion of 1:1 and 3:7 water-in-oil-type mould oil system milk sap.
The appearance of microwave demulsifying method has partly solved this difficult problem, and especially little to viscous crude and salinity height, profit relative density difference, heavy-gravity polymkeric substance well liquid has effect preferably, but microwave exists limited, the shortcoming uniformly inadequately of breakdown of emulsion useful area.
Summary of the invention:
In order to address the above problem, the invention provides a kind of fast emulsion breaking method, by the synergy of emulsion splitter and microwave radiation, can carry out breakdown of emulsion to Water in Oil emulsion in the short period of time, and obtain bigger dehydration rate, improve breakdown of emulsion efficient.
The technical solution used in the present invention is: a kind of fast emulsion breaking method, comprise microwave radiation, and to press emulsified coarse-oil contained water amount mass parts and add emulsion splitter, water is 1: 0.5 * 10 with the mass parts ratio of emulsion splitter
-4～5 * 10
-4, carry out breakdown of emulsion with microwave.
Described emulsion splitter is one or more of polyamines class polyoxy third rare Soxylat A 25-7, resene polyoxy third rare Soxylat A 25-7, high-carbon alcohols initiator emulsion splitter or propandiols emulsion splitter.
Described polyamines class polyoxy third rare Soxylat A 25-7 is a kind of of polyethylene polyamine polyoxyethylene oxypropylene ether (HD-5) or four ethylidene hexylamine polyoxyethylene polyoxypropylene ethers (AE-121) or two kinds.
Described resene polyoxy third rare Soxylat A 25-7 is a kind of of phenol amine polyoxyethylene oxypropylene ether (TA-1031) or polyoxyethylene polyoxypropylene propylene glycol monoether (PR-23) or two kinds.
Described high-carbon alcohols initiator is that stearyl alcohol polyoxyethylene polyoxypropylene ether (SP-169) or higher alcohols polyoxyethylene polyoxypropylene segmented copolymer (DY-1) are a kind of or two kinds.
Described propandiols emulsion splitter is a kind of of polyoxyethylene polyoxypropylene propylene glycol (BPE2070) or propylene glycol polyoxyethylene polyoxypropylene block copolymer (BP-169) or two kinds.
Described microwave radiation, microwave radiation frequency are 2450MHz or 915MHz.
Emulsion splitter and microwave radiation all have the effect of breakdown of emulsion, emulsion splitter by its " absorption " in water-oil interface, " replacements " and to liquid pearl " flocculation ", " coalescence " thus act on the characteristic of change interfacial film, reduce the water-oil interface film strength, reach breakdown of emulsion.Microwave radiation is destroyed the Zeta potential of oil-water interfacial film on the one hand, and on the other hand, the oil in the interfacial film is owing to be heated and solubleness increases, make interfacial film the physical strength step-down and reach breakdown of emulsion.
The present invention adopts the effect of following laboratory test checking emulsion splitter and microwave radiation synergy breakdown of emulsion.
1, the preparation of emulsion:
Material: water; Crude oil; Kerosene;
Arlacel-80 (Span-80): main component: sorbitol monooleate
The place of production: chemical plant, Lvshun, Liaoning;
The preparation of emulsion: oil phase: with 0.3652g Span-80, join in the mixed solution of 9.1307g crude oil and 27.3921g kerosene, mix.In test tube, accurately pipette oil phase 1.5ml, add entry 3.5ml, concussion is 3 minutes on the whirlpool mixed instrument, makes the w/o type emulsion.This emulsion 5.0ml, moisture 3.5ml is a breakdown of emulsion experiment consumption.
2, breaking method experiment
Experimental example 1
In emulsion, divide and add 3.5 * 10 in addition
-4G emulsion splitter HD-5, AE-121, TA-1031, PR-23, SP-169, DY-1, BPE2070, BP-169, vibration is dissolved emulsion splitter fully, insert then in the microwave generator, start microwave generator, the microwave radiation frequency is 2450MHz, observe and measure in the test tube volume of water.The results are shown in Table 1.Reference examples is directly carried out the microwave radiation breakdown of emulsion for not adding emulsion splitter.
Table 1 water volume is with the variation of microwave irradiation time
| Time s emulsion splitter | 0 | 20 | 30 | 40 | 50 | 60 | 100 | 200 | 300 | 400 |
| HD-5 | 0 | 0.37 | 3.00 | 3.45 | ||||||
| AE-121 | 0 | 0.47 | 3.17 | 3.5 | ||||||
| TA-1031 | 0 | 2.8 | 3.0 | 3.1 | 3.5 | |||||
| PR-23 | 0 | 2.6 | 3.1 | 3.5 | ||||||
| SP-169 | 0 | 0.17 | 0.67 | 1.30 | 2.13 | 3.50 | ||||
| DY-1 | 0 | 0.10 | 0.55 | 1.00 | 2.05 | 3.40 | ||||
| BPE2070 | 0 | 3.05 | 3.12 | 3.15 | 3.50 | |||||
| BP-169 | 0 | 3.12 | 3.15 | 3.31 | 3.50 | |||||
| Reference examples | 0 | 0 | 0 | 1.96 | 2.13 | 2.88 | 3.00 | 3.20 | 3.40 | 3.40 |
From table 1 result as seen, add emulsion splitter obviously than not adding emulsion splitter, the breakdown of emulsion time shortens 7～10 times.
Experimental example 2
In emulsion, add the emulsion splitter of different amounts respectively, vibration is dissolved emulsion splitter fully, inserts then in the microwave generator, and the microwave radiation frequency is 2450MHz, observes and measures the complete breakdown of emulsion time.The results are shown in Table 2.
Table 2 water volume is with the variation of microwave irradiation time
| Consumption g emulsion splitter | 1.75×10 -4 | 5.25×10 -4 | 7.0×10 -4 | 10.5×10 -4 | 14×10 -4 | 17.5×10 -4 |
| HD-5 | 63 | 40 | 37 | 35 | 32 | 29 |
| AE-121 | 60 | 39 | 35 | 30 | 29 | 27 |
| TA-1031 | 79 | 49 | 43 | 40 | 38 | 37 |
| PR-23 | 62 | 48 | 43 | 41 | 38 | 37 |
| SP-169 | 80 | 58 | 53 | 50 | 48 | 46 |
| DY-1 | 83 | 60 | 57 | 53 | 50 | 48 |
| BPE2070 | 76 | 48 | 42 | 40 | 37 | 36 |
| BP-169 | 82 | 45 | 42 | 40 | 39 | 37 |
From the result of table 2, add emulsion splitter and can shorten the breakdown of emulsion time, originally de-emulsification speed is fast, slowly increases thereafter, so the add-on of emulsion splitter is 1: 1 * 10 with the mass parts ratio of water and emulsion splitter
-4～3 * 10
-4For preferably.
Experimental example 3
In emulsion, add two or more emulsion splitter respectively, vibration is dissolved emulsion splitter fully, inserts then in the microwave generator, and the microwave radiation frequency is 2450MHz, observes and measures the complete breakdown of emulsion time.
(1) emulsion splitter: AE-121 0.5 * 10
-4G SP-169 3.0 * 10
-4g
The breakdown of emulsion time: 35 seconds
(2) emulsion splitter: AE-121 1.5 * 10
-4G TA-1031 2.0 * 10
-4g
The breakdown of emulsion time: 39 seconds
(3) emulsion splitter: SP-169 1.6 * 10
-4G DY-1 1.9 * 10
-4g
The breakdown of emulsion time: 41 seconds
(4) emulsion splitter: DY-1 3.1 * 10
-4G BP-169 0.4 * 10
-4g
The breakdown of emulsion time: 43 seconds
(5) emulsion splitter: AE-121 1.1 * 10
-4G SP-169 1.2 * 10
-4G BPE2070 1.2 * 10
-4g
The breakdown of emulsion time: 35 seconds
(6) emulsion splitter: TA-1031 0.8 * 10
-4G SP-169 1.3 * 10
-4G BP-169 1.4 * 10
-4g
The breakdown of emulsion time: 32 seconds
(7) emulsion splitter: PR-23 1.5 * 10
-4G BP-169 2.0 * 10
-4g
The breakdown of emulsion time: 39 seconds
(8) emulsion splitter: DY-1 1.5 * 10
-4G BP-169 2.0 * 10
-4g
The breakdown of emulsion time: 39 seconds
Comparative Examples
In emulsion, add 3.5 * 10 respectively
-4G emulsion splitter AE-121 and SP-169, vibration is dissolved emulsion splitter fully, inserts then in 60 ℃ of waters bath with thermostatic control, and breakdown of emulsion is carried out in heating, observes and measures in the test tube, the volume of water.Reference examples directly places water bath with thermostatic control for not adding emulsion splitter, the results are shown in Table 3.
Table 3 water volume is with the variation of heat-up time
| Time (min) water volume (ml) | 0 | 10 | 20 | 30 | 40 | 50 | 60 |
| AE-121 | 0 | 0.20 | 3.00 | 3.00 | 3.10 | 3.20 | 3.20 |
| SP-169 | 0 | 0 | 0.50 | 0.70 | 0.70 | 0.70 | 0.70 |
| Reference examples | 0 | 0 | 0 | 0 | 0 | 0 | 0 |
The invention has the beneficial effects as follows: experimental example and Comparative Examples can draw, and utilize the synergy of emulsion splitter and microwave radiation, can carry out breakdown of emulsion to Water in Oil emulsion in the short period of time, and obtain bigger dehydration rate, improve breakdown of emulsion efficient.Under the condition that a small amount of emulsion splitter exists, utilize the microwave radiation breakdown of emulsion, improved 1～2 order of magnitude than conventional heating demulsification type speed.The present invention is simple to operate, and is energy-conservation, and de-emulsification speed is fast, and demulsification is good.
Embodiment:
Embodiment 1
Get 100g emulsified crude oil (water content 80%, source Shengli Oil Field), in the container of packing into, the mass parts ratio by water and emulsion splitter is 1: 1 * 10 respectively
-4, 1: 2 * 10
-4, 1: 3 * 10
-4, add emulsion splitter AE-121 and SP-169, vibration is dissolved emulsion splitter fully, places microwave generator then, frequency 2450MHz, power 850W writes down the complete breakdown of emulsion time, the results are shown in Table 4.Reference examples is not for adding emulsion splitter.
Table 4
| Consumption g | Breakdown of emulsion time s | Consumption g | Breakdown of emulsion time s | Consumption g | Breakdown of emulsion time s | |
| AE-121 | 80×10 -4 | 35 | 160×10 -4 | 32 | 240×10 -4 | 30 |
| SP-169 | 80×10 -4 | 48 | 160×10 -4 | 46 | 240×10 -4 | 42 |
| Reference examples | 462 | |||||
Embodiment 2
Get 100g emulsified crude oil (water content 75%, source Shengli Oil Field), in the container of packing into, the mass parts ratio by water and emulsion splitter is 1: 0.5 * 10 respectively
-4, 1: 1.5 * 10
-4, 1: 5 * 10
-4, adding emulsion splitter AE-121 and SP-169, vibration is dissolved emulsion splitter fully, places microwave generator then, frequency 2450MHz, power 850W writes down the complete breakdown of emulsion time, the results are shown in Table 5.Reference examples is not for adding emulsion splitter.
Table 5
| Consumption g | Breakdown of emulsion time s | Consumption g | Breakdown of emulsion time s | Consumption g | Breakdown of emulsion time s | |
| AE-121 | 37.5×10 -4 | 39 | 112.5×10 -4 | 37 | 375×10 -4 | 35 |
| SP-169 | 37.5×10 -4 | 56 | 112.5×10 -4 | 53 | 375×10 -4 | 50 |
| Reference examples | 493 | |||||
Embodiment 3
Get 100g emulsified crude oil (water content 65%, source Shengli Oil Field), in the container of packing into, the mass parts ratio by water and emulsion splitter is 1: 0.8 * 10 respectively
-4, 1: 2.5 * 10
-4, 1: 3.5 * 10
-4, add emulsion splitter AE-121 and SP-169, vibration is dissolved emulsion splitter fully, places microwave generator then, frequency 2450MHz, power 850W writes down the complete breakdown of emulsion time, the results are shown in Table 6.Reference examples is not for adding emulsion splitter.
Table 6
| Consumption g | Breakdown of emulsion time s | Consumption g | Breakdown of emulsion time s | Consumption g | Breakdown of emulsion time s | |
| AE-121 | 52×10 -4 | 37 | 162.5×10 -4 | 35 | 227.5×10 -4 | 33 |
| SP-169 | 52×10 -4 | 50 | 162.5×10 -4 | 48 | 227.5×10 -4 | 46 |
| Reference examples | 563 | |||||
Embodiment 4
Repeat embodiment 1, just microwave frequency is adjusted to 915MHz.The results are shown in Table 7
Table 7
| Consumption g | Breakdown of emulsion time s | Consumption g | Breakdown of emulsion time s | Consumption g | Breakdown of emulsion time s | |
| AE-121 | 80×10 -4 | 33 | 160×10 -4 | 30 | 240×10 -4 | 28 |
| SP-169 | 80×10 -4 | 45 | 160×10 -4 | 42 | 240×10 -4 | 41 |
Claims (8)
1. a fast emulsion breaking method comprises microwave radiation, it is characterized in that: press emulsified coarse-oil contained water amount mass parts and add emulsion splitter, water is 1: 0.5 * 10 with the mass parts ratio of emulsion splitter
-4～5 * 10
-4, carry out breakdown of emulsion with microwave.
2. a kind of fast emulsion breaking method according to claim 1 is characterized in that: described water is 1: 1 * 10 with the mass parts ratio of emulsion splitter
-4～3 * 10
-4
3. a kind of fast emulsion breaking method according to claim 1 is characterized in that: described emulsion splitter is one or two or more kinds mixing of polyamines class polyoxy third rare Soxylat A 25-7, resene polyoxy third rare Soxylat A 25-7, high-carbon alcohols initiator emulsion splitter or propandiols emulsion splitter.
4. a kind of fast emulsion breaking method according to claim 3 is characterized in that: described polyamines class polyoxy third rare Soxylat A 25-7 is polyethylene polyamine polyoxyethylene oxypropylene ether or four ethylidene hexylamine polyoxyethylene polyoxypropylene ethers.
5. a kind of fast emulsion breaking method according to claim 3 is characterized in that: described resene polyoxy third rare Soxylat A 25-7 is phenol amine polyoxyethylene oxypropylene ether or polyoxyethylene polyoxypropylene propylene glycol monoether.
6. a kind of fast emulsion breaking method according to claim 3 is characterized in that: described high-carbon alcohols initiator is stearyl alcohol polyoxyethylene polyoxypropylene ether or higher alcohols polyoxyethylene polyoxypropylene segmented copolymer.
7. a kind of fast emulsion breaking method according to claim 3 is characterized in that: described propandiols emulsion splitter is polyoxyethylene polyoxypropylene propylene glycol or propylene glycol polyoxyethylene polyoxypropylene block copolymer.
8. a kind of fast emulsion breaking method according to claim 1 is characterized in that: described microwave radiation, microwave radiation frequency are 2450MHz or 915MHz.
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|---|---|---|---|
| CN2007100123177A CN101121898B (en) | 2007-07-30 | 2007-07-30 | Fast emulsion breaking method |
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| CN102802751A (en) * | 2010-03-15 | 2012-11-28 | 陶氏环球技术有限责任公司 | Coalescer device and separation method |
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|---|---|---|---|---|
| CA1205021A (en) * | 1982-03-29 | 1986-05-27 | Conoco Inc. | Use of microwave radiation in separating emulsions and dispersions of hydrocarbons and water |
| CN1295007C (en) * | 2005-01-07 | 2007-01-17 | 辽宁大学 | Demulsifying process for emulsified crude oil |
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- 2007-07-30 CN CN2007100123177A patent/CN101121898B/en not_active Expired - Fee Related
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