CN107011937A - A kind of waxy crude oil rheological characteristic ameliorative way - Google Patents
A kind of waxy crude oil rheological characteristic ameliorative way Download PDFInfo
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- CN107011937A CN107011937A CN201710276946.4A CN201710276946A CN107011937A CN 107011937 A CN107011937 A CN 107011937A CN 201710276946 A CN201710276946 A CN 201710276946A CN 107011937 A CN107011937 A CN 107011937A
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- crude oil
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
- C10G31/06—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for by heating, cooling, or pressure treatment
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1033—Oil well production fluids
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Abstract
The present invention relates to a kind of waxy crude oil rheological characteristic ameliorative way, belong to Colloid and interface chemistry, micro Nano material, petroleum pipeline conveying technology field.The present invention is by adding oil-dispersing property microballoon into waxy crude oil, utilize the spherical morphology of its excellent oil-dispersing property and rule, in waxy crude oil temperature-fall period, the effect for producing steric hindrance suppresses the formation and development of the brilliant three-dimensional net structure of wax, and then gel point, apparent viscosity and the structure yields value of waxy crude oil are significantly reduced, so as to improve the low-temperature rheology characteristics of waxy crude oil.Oil-dispersing property microballoon of the present invention can be selected from organosilicon microballoon or crosslinking polymer microballoon.The effect of oil-dispersing property microballoon is added into waxy crude oil and grain type, particle size distribution is interval and granule density is closely related.
Description
Technical field
It is micro- by adding oil-dispersing property into waxy crude oil the present invention relates to a kind of ameliorative way of waxy crude oil rheological characteristic
Ball, hinders the formation of the brilliant three-dimensional net structure of wax in temperature-fall period, so as to improve waxy crude oil low-temperature rheology characteristics, is related to colloid
With surface chemistry, micro Nano material, petroleum pipeline conveying technology field.
Background technology
Most of crude oil of each elephant production of China is waxy crude oil, and the topmost feature of this quasi-oil is when temperature drop
When below to its wax precipitation point, the wax itself being dissolved in fluid oil starts gradually to separate out to form wax crystalline substance and as temperature drop is further long
Greatly.These waxes crystalline substance has very high surface energy, in the case where amount of precipitation is seldom, mutually will irregularly overlap, stack, twines
Around the continuous three-dimensional network shape space structure of formation.This three-dimensional network-like structure makes flowable oil content be wrapped in wherein,
So as to cause fluid oil not flow, macroscopically crude oil is set to be gelled, the maximum temperature point for occurring waxy crude oil gelling is crude oil
Condensation point.As temperature is reduced, analysis wax amount increases, and crude oil jelling structure will further enhance.The complicated rheological characteristic of waxy crude oil
Its safe transport of verifying proposes significant challenge.Therefore need to carry out waxy crude oil certain processing, make the low temperature stream of crude oil
Change nature disclosure satisfy that engine request, and ensure safe, reliable, efficient to the processing of crude oil, so as to improve the warp of enterprise
Ji benefit, the research on this aspect always is the focus and emphasis of Oil ＆ Gas Storage industry.By heating crude oil to anomalistic point
Although the rheological property of waxy crude oil can effectively be ensured by carrying out heated transportation above or more than wax precipitation point to it, exist
Power consumption is high, heating crude oil potential safety hazard, the problems such as required equipment is more.At present, suitable polymer-type is added into waxy crude oil
Pour-point depressant carries out chemical modification conveying to waxy crude oil, is a kind of economical and effective measures.Polymer-type pour-point depressant is typically same
Shi Hanyou polar groups and non-polar group, can and wax trichite generation core, absorption, the effect such as eutectic, change the brilliant size of wax and
Shape, makes the ability that wax crystalline substance forms three-dimensional space net structure die down, thus enhances the mobility of crude oil；Also make low temperature simultaneously
The yield value of lower crude oil is substantially reduced, and is conducive to the low temperature of crude oil to convey, is reduced stopped flow injection analysis pressure and increase safety in shutdown
Time.At present, polymer-type pour-point depressant has been successfully applied to a plurality of domestic and international oil pipeline and has achieved significant economic effect
Benefit, but polymer-type pour-point depressant still suffers from many deficiencies：It is ageing poor, it is impossible to meet the defeated requirement of pipe；Anti-shearing and anti-repetition
Heating ability is poor；Treatment with PPD is sensitive to temperature recovery, there is temperature recovery and deteriorates interval；There is a possibility that pipeline wax is heavy
Product increase；Pour-viscosity reduction effect to high wax content oil is undesirable etc..
In order to overcome traditional polymer type pour-point depressant applying upper many deficiencies, there is scholar at present by nano material and biography
System polymer-type pour-point depressant is added into waxy crude oil to improve the performance of polymer-type pour-point depressant jointly.Patent
CN102108292A discloses a kind of pour point depression of crude oil viscosity reduction nanometer substrate composite, by nanometer base material and the compound system of pour point depressant for crude oil
, added in crude oil after, in temperature-fall period with wax is brilliant is separated out by the way that eutectic effect is common, improve low-temperature wax crystalline form looks, make
Viscosity of crude declines, and with well ageing.Patent CN104154421A discloses one kind and is grafted to polar group
Inorganic nano-particle：Such as nano-calcium carbonate, nanomete talc powder, nano montmorillonite, the surface of nano silicon, obtain by table
The pour point depressant for crude oil nanoscale base material that face is modified.The nanoscale base material is added in crude oil to be dropped under cryogenic to crude oil
Solidifying viscosity reduction.But the invention needs to carry out physical absorption or chemically grafting and modifying in advance to nanoscale base material, and preparation process is more numerous
It is trivial, and used particle size distribution is in nanoscale.Prepare one kind and have hybrid property concurrently, with oil-based system phase
Capacitive is good, while the oil-dispersing property microballoon of the well-regulated spherical microscopic appearance of tool, makes it individually play drop in waxy crude oil
Solidifying viscosity reduction effect, very with potentiality.
Polyorganosilsesquioande (PSQ) microballoon is, by trifunctional silane, in the aqueous solution or water/fat liquor, to lead to
The product crossed obtained by an one-step hydrolysis polycondensation.The special chemical constitution of PSQ microballoons and monodisperse spherical pattern, make it have nothing concurrently
The performance of machine/organic Hybrid Materials and micro-size particles, shows excellent heat resistance, hydrophobicity, ageing-resistant, hardness high, resistance to
The characteristics such as salt, resistance to oxidation, chemicals-resistant burn into electrical insulating property, be widely used in coating, optical articles, rubber plastic industry and
The fields such as cosmetics.Simultaneously as the diversity of silicon source, PSQ microsphere particle Surface coatings have diversified organic group, such as
Methyl, vinyl, phenyl, mercapto propyl group etc., it is possible to further carry out the modification such as physical absorption, chemical graft.
Crosslinked polymer microballoon is with polymer (polystyrene, styrene-to benzene diene copolymers, polymethylacrylic acid
Methyl esters etc.) for matrix, the spheric granules being crosslinked, granularity can be distributed between hundreds of nanometers to tens microns, with good
Absorption property, acid and alkali-resistance, rigidity strong, high temperature resistant, surface-active and recuperability, application be related to standard metering,
Every field, the particularly biomedical sectors such as food chemistry, medicine and pharmacology, bioengineering, information engineering microelectric technique, to facing
The Research Significance of bed diagnosis, inspection, immunological technique, cytology etc. is extremely great.
Up to the present cut-off, not yet has and oil-dispersing property microballoon is separately added in waxy crude oil to improve its low temperature stream
The report of denaturation.
The content of the invention
It is an object of the invention to provide a kind of waxy crude oil rheological characteristic ameliorative way, to be effectively reduced the glue of waxy crude oil
Condensation point, apparent viscosity and structure yields value, and have the advantages of preparing simple, with low cost concurrently.
The present invention utilizes to realize that the technical scheme that its purpose is used is the addition oil-dispersing property microballoon into waxy crude oil
The spherical morphology of its excellent oil-dispersing property and rule, in waxy crude oil temperature-fall period, the effect for producing steric hindrance suppresses
The formation and development of wax crystalline substance three-dimensional net structure, and then significantly reduce gel point, apparent viscosity and the structure yields of waxy crude oil
Value, so as to improve the low-temperature rheology characteristics of waxy crude oil, it is characterized in that realizing according to the following steps：By oil-dispersing property microballoon with
10mg/kg~400mg/kg concentration is added in waxy crude oil, and uniform stirring when more than waxy crude oil wax precipitation point temperature
20~40 minutes, then crude oil non-newtonian fluid temperature range is cooled to 0.5 DEG C/min rate of temperature fall, measurement waxy crude oil
Gel point, apparent viscosity and structure yields value；Described oil-dispersing property microballoon is selected from organosilicon microballoon or crosslinking polymer is micro-
Ball；The size distribution of oil-dispersing property microballoon is 0.2 μm~10 μm.
Described oil-dispersing property microballoon, can be selected from organosilicon microballoon, such as polymethylsilsesquioxane (PMSQ), poly- ethyl
One or more in silsesquioxane (PESQ), polyvinylsilesquioxane, poly-phenyl silsesquioxane microballoon etc.；Also may be used
With selected from crosslinking polymer microballoon, such as polystyrene, polystyrene-to benzene diene copolymers, polymethacrylates microballoon
One or more in；It is also an option that in microballoon based on above-mentioned particle after physical absorption or chemically grafting and modifying etc.
One or more；
Described oil-dispersing property microsphere particle size is distributed as 0.2 μm~10 μm, preferably 0.5 μm~2 μm；
Addition concentration of the described oil-dispersing property microballoon in waxy crude oil is 10mg/kg~400mg/kg, preferably 50mg/
Kg~200mg/kg.
It is excellent using oil-dispersing property microballoon the beneficial effects of the invention are as follows by adding oil-dispersing property microballoon into waxy crude oil
The microcosmic spherical morphology of different oil dispersed property and rule, in waxy crude oil temperature-fall period, is pressed down by the effect of steric hindrance
The formation and development of the brilliant three-dimensional net structure of wax processed, and then it is in the wrong to significantly reduce gel point, apparent viscosity and the structure of waxy crude oil
Clothes value, so as to improve the low-temperature rheology characteristics of waxy crude oil.
Embodiment
Technical scheme is described further with route with reference to embodiments, but following examples are only this
The limited citing of invention, the limitation to present invention is not constituted.
Embodiment 1：The preparation of polymethylsilsesquioxane (PMSQ) microballoon：At 25 DEG C, 250ml deionized waters are added
Into the round-bottomed flask equipped with magnetic stirring apparatus, it is 900r/min to control stir speed (S.S.), with 1ml/min drop speed be added dropwise with go from
Sub- water quality ratio is 1:10 MTMS, it is 4 to control pH value of solution, persistently stirs and reacts after 4h, and ammoniacal liquor is added dropwise
Temperature is adjusted to polycondensation reaction temperature by regulation system pH value simultaneously to polycondensation reaction pH=8, continues to react 4h.After reacting
Solution washed 3-4 times by centrifugation-absolute ethyl alcohol after be placed in 10 hours of vacuum oven, obtained white powder is i.e.
For polymethylsilsesquioxane microballoon (granularity concentrates on 0.5 μm).Wherein, control stir speed (S.S.), polycondensation reaction pH, polycondensation are coordinated
Reaction temperature, can control the size distribution (0.5 μm~10 μm) of the polymethylsilsesquioxane microballoon of synthesis；By converting silicon
The species in source can synthesize the oligomeric silsesquioxane microballoon with different organic groups.
Embodiment 2：The preparation of polystyrene (PS) microballoon：250ml absolute ethyl alcohols and 20g polyvinylpyrrolidones are added
Into four-hole boiling flask, stirring is formed after homogeneous system, is passed through excessive nitrogen, and start to be slowly added dropwise 50g dissolved with 0.5g azos two
The styrene of isobutyronitrile.After monomer dropping is finished, nitrogen atmosphere and certain mixing speed are kept, 24h is reacted at 70 DEG C, makes
Settled with centrifuge, discard supernatant liquor, washed with ethanol three times.Product after washing is dried in vacuo at 60 DEG C
24h, produces polystyrene microsphere (granularity concentrates on 0.5 μm).The preparation of other particle diameter microballoons can be by adjusting stir speed (S.S.)
Complete.
Embodiment 3：The preparation of polymethyl-benzene e pioic acid methyl ester (PMMA) microballoon：150mL deionized waters are taken in there-necked flask, and
Lauryl sodium sulfate 0.0011g is added, leads to N2Protection.Stir after 5min (300r/min), 10.0g formaldehyde is added into system
Methyl acrylate continues to whisk.After 10min, system is placed in 75 DEG C of water-baths and heated, after system temperature rises to 75 DEG C, continued
Stir 30min.Then initiator potassium persulfate 0.1g is rapidly added into system.Entirely react in N2Protection is lower to be carried out, after 5h
Reaction is completed.Settled, washed with ethanol three times using centrifuge.Product after washing is dried in vacuo 24h at 60 DEG C,
Produce polymethyl-benzene e pioic acid methyl ester microballoon (granularity concentrates on 0.75 μm).The preparation of other particle diameter microballoons can pass through regulation 12
The consumption of sodium alkyl sulfate and water is completed.
Embodiment 4：Using domestic typical waxy crude oil Qinghai crude oil as research object, the basic physical properties such as table of Qinghai crude oil
Shown in 1.By the average grain diameter prepared by embodiment 1 be respectively 0.2 μm, 0.5 μm, 2 μm, 5 μm, 10 μm of PMSQ microballoons with
200ppm's adds dosage to be added in the crude oil of Qinghai, and uniform stirring is made plus PMSQ particle oil samples for 20~40 minutes at 60 DEG C.
Measured in oscillation mode using AR-G2 coaxial cylinders rotational rheometer and add the viscoplasticity of particle oil sample in temperature-fall period with temperature
Situation of change, when its storage modulus be equal to loss modulus when temperature spot be defined as plus particle oil sample gel point.Meanwhile, do
Blank sample experiment is contrasted, as a result as shown in table 2.
Table 1
Table 2
Embodiment 5：Average grain diameter prepared by embodiment 1 is added into dosage addition for 2 μm of PMSQ microballoons with 200ppm
To Qinghai crude oil, uniform stirring is made plus PMSQ particle oil samples for 20~40 minutes at 60 DEG C.Similarly, by prepared by embodiment 1
Average grain diameter be 2 μm PMSQ microballoons and PESQ microballoons with 1:1、1:3、1:5 mass ratio, 200ppm's plus dosage addition
Into Qinghai crude oil, uniform stirring is made plus PMSQ and PESQ particle oil samples for 20~40 minutes at 60 DEG C.It is coaxial using AR-G2
Cylinder rotational rheometer measures the viscoplasticity variation with temperature situation for adding particle oil sample in temperature-fall period, note in oscillation mode
Record plus the gel point of particle oil sample.Meanwhile, do blank sample experiment and contrasted, as a result as shown in table 3.
Table 3
Embodiment 6：By the average grain diameter prepared by embodiment 1 for 2 μm PMSQ microballoons respectively with 10ppm, 20ppm,
50ppm, 100ppm, 200ppm, 400ppm plus dosage is added in the crude oil of Qinghai, uniform stirring 20~40 minutes at 60 DEG C
It is made plus PMSQ particle oil samples.Measured in oscillation mode in temperature-fall period using AR-G2 coaxial cylinders rotational rheometer plus
The gel point of the viscoplasticity variation with temperature situation of grain oil sample, record plus particle oil sample.Meanwhile, do blank sample experiment progress pair
Than as a result as shown in table 4.
Table 4
Embodiment 7：It is respectively 0.2 μm, 0.5 μm, 2 μm, 5 μm, 10 μm of PMSQ by the average grain diameter prepared by embodiment 1
Microballoon is added to Qinghai crude oil with 200ppm's plus dosage, and uniform stirring is made plus PMSQ particles oil for 20~40 minutes at 60 DEG C
Sample.Using AR-G2 coaxial cylinders rotational rheometers, 15 DEG C of measurement temperature is down to from 60 DEG C with 0.5 DEG C/min cooling rate, it is permanent
Shear rate 10s is increased continuously after warm 30min-1To 200s-1, test plus apparent viscosity of the particle oil sample under measurement temperature.And
Blank sample is done to be contrasted.Its result is as shown in table 5.
Table 5
Embodiment 8：By the average grain diameter prepared by embodiment 1 for 2 μm PMSQ microballoons respectively with 50ppm, 200ppm and
400ppm's adds dosage to be added to Qinghai crude oil, and uniform stirring is made plus PMSQ particle oil samples for 20~40 minutes at 60 DEG C.Together
Manage by the average grain diameter prepared by embodiment 1 be 2 μm PMSQ microballoons and PESQ microballoons with 1:1 mass ratio, respectively with
50ppm, 200ppm and 400ppm plus dosage is added to Qinghai crude oil, and uniform stirring is made and added for 20~40 minutes at 60 DEG C
PMSQ and PESQ particle oil samples.Using AR-G2 coaxial cylinders rotational rheometers, dropped with 0.5 DEG C/min cooling rate from 60 DEG C
To 15 DEG C of measurement temperature, shear rate 10s is increased continuously after constant temperature 30min-1To 200s-1, two kinds of test plus particle oil sample are being surveyed
Apparent viscosity under amount temperature, and do blank sample and contrasted, its result is as shown in table 6.
Table 6
Embodiment 9：Prepare same as Example 5 plus PMSQ particles oil sample and add PMSQ and PESQ particle oil samples.Use
AR-G2 coaxial cylinders rotational rheometers, 15 DEG C of measurement temperature, constant temperature 30min are down to from 60 DEG C with 0.5 DEG C/min cooling rate
After increase continuously shear rate 0s-1To 1s-1, test plus the strain of particle oil sample and the variation relation of stress, the stress measured is maximum
It is worth as the structure yields value for adding particle oil sample under the conditions of this.And do blank sample and contrasted.Its result is as shown in table 7.
Table 7
Embodiment 10：By the average grain diameter prepared by embodiment 2 for 0.5 μm PS microballoons with 10ppm, 20ppm, 50ppm,
100ppm, 200ppm, 400ppm plus dosage is added in the crude oil of Qinghai, and uniform stirring is made and added for 20~40 minutes at 60 DEG C
PS particle oil samples.Measured in oscillation mode using AR-G2 coaxial cylinders rotational rheometer and add particle oil sample in temperature-fall period
Viscoplasticity variation with temperature situation, and record the gel point for adding particle oil sample.Meanwhile, do blank sample experiment and contrasted.Knot
Fruit is as shown in table 8.
Table 8
Embodiment 11：By the average grain diameter prepared by embodiment 3 for 0.75 μm PMMA microsphere with 10ppm, 20ppm,
50ppm, 100ppm, 200ppm, 400ppm plus dosage is added in the crude oil of Qinghai, uniform stirring 20~40 minutes at 60 DEG C
It is made plus PMMA particle oil samples.Measured in oscillation mode in temperature-fall period using AR-G2 coaxial cylinders rotational rheometer plus
The viscoplasticity variation with temperature situation of grain oil sample, and record the gel point for adding particle oil sample.Meanwhile, do blank sample experiment progress
Contrast, as a result as shown in table 9.
Table 9
Embodiment 12：It is 0.5 μm of PMSQ microballoons, flat prepared by embodiment 2 by the average grain diameter prepared by embodiment 1
Equal particle diameter for 0.5 μm PS microballoons, as the average grain diameter prepared by embodiment 2 and embodiment 3 be respectively 0.5 μm of PS microballoons
1 is pressed with PMMA microsphere:Hybrid particles made from 1 mass ratio are added in the crude oil of Qinghai with 200ppm's plus dosage, 60
Three kinds plus particle oil sample is made in 20~40 minutes in uniform stirring at DEG C.Using AR-G2 coaxial cylinders rotational rheometers, with 0.5 DEG C/
Min cooling rate increases continuously shear rate 10s after 15 DEG C of measurement temperature, constant temperature 30min are down to from 60 DEG C-1To 200s-1,
Above-mentioned three kinds plus apparent viscosity of the particle oil sample under measurement temperature are tested, and is contrasted with blank sample, its result such as table 10
It is shown.
Table 10
Can be seen that the addition oil-dispersing property microballoon into waxy crude oil from above-mentioned result of the test can be effectively reduced the content of wax
Gel point, apparent viscosity and the structure yields value of crude oil, and effect and grain type, particle size distribution interval and granule density
It is closely related.
Embodiments above, is that the goal in research to the present invention, technology path, effect of optimization are further illustrated, and
The other embodiment of the present invention is not limited, and within the spirit and principles of the invention, any modification, the optimization made are set
Meter, equivalent substitution etc., all should be within protection scope of the present invention.
Claims (6)
1. a kind of waxy crude oil rheological characteristic ameliorative way, excellent using its by adding oil-dispersing property microballoon into waxy crude oil
Oil-dispersing property with rule microcosmic spherical morphology, in waxy crude oil temperature-fall period, pass through the effect of steric restriction, suppress wax
The formation and development of brilliant three-dimensional net structure, and then significantly reduce gel point, apparent viscosity and the structure yields value of waxy crude oil,
So as to improve the low-temperature rheology characteristics of waxy crude oil, it is characterized in that comprising the following steps：By oil-dispersing property microballoon with 10mg/kg~
400mg/kg concentration is added in waxy crude oil, and 20~40 points of uniform stirring when more than waxy crude oil wax precipitation point temperature
Clock, then crude oil non-newtonian fluid temperature range is cooled to 0.5 DEG C/min rate of temperature fall, measure waxy crude oil gel point,
Apparent viscosity and structure yields value；Described oil-dispersing property microballoon is selected from organosilicon microballoon or crosslinking polymer microballoon；Oil
The size distribution for dissipating property microballoon is 0.2 μm~10 μm.
2. waxy crude oil rheological characteristic ameliorative way according to claim 1, it is characterized in that described organosilicon microballoon is selected from
One kind or its combination in polymethyl siloxane, PES-4, polyvinyl siloxane or phenyl silicone microballoon etc..
3. waxy crude oil rheological characteristic ameliorative way according to claim 1, it is characterized in that described crosslinking polymer is micro-
Ball selected from polystyrene, polystyrene-to one kind in benzene diene copolymers, polymethacrylates microballoon etc. or its combination.
4. waxy crude oil rheological characteristic ameliorative way according to claim 1, it is characterized in that described oil-dispersing property microballoon is also
It may be selected from based on organosilicon microsphere particle or crosslinking polymer microsphere particle after physical absorption or chemically grafting and modifying
One kind or its combination in microballoon.
5. waxy crude oil rheological characteristic ameliorative way according to claim 1, it is characterized in that the granularity of oil-dispersing property microballoon point
Cloth is 0.5 μm~2 μm.
6. waxy crude oil rheological characteristic ameliorative way according to claim 1, contains it is characterized in that oil-dispersing property microballoon is added to
Concentration in wax crude oil is 10mg/kg~400mg/kg.
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Cited By (1)
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| CN113651928A (en) * | 2021-08-16 | 2021-11-16 | 宁波锋成先进能源材料研究院有限公司 | Oil-soluble thick oil viscosity reducer and preparation method and application thereof |
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