CN108977187A - A kind of composite crude oil thinner and preparation method thereof - Google Patents
A kind of composite crude oil thinner and preparation method thereof Download PDFInfo
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- CN108977187A CN108977187A CN201810968784.5A CN201810968784A CN108977187A CN 108977187 A CN108977187 A CN 108977187A CN 201810968784 A CN201810968784 A CN 201810968784A CN 108977187 A CN108977187 A CN 108977187A
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
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- C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F17D—PIPE-LINE SYSTEMS; PIPE-LINES
- F17D1/00—Pipe-line systems
- F17D1/08—Pipe-line systems for liquids or viscous products
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Abstract
The invention discloses a kind of composite crude oil thinners and preparation method thereof, which is prepared from the following raw materials of the following mass: 100 parts of ethylene-vinyl acetate copolymer, 20-40 parts of fatty acid, 20-200 parts modified of phyllosilicate, 1-5 parts of p-methyl benzenesulfonic acid, 100.8-307.2 parts of methanol, 0.2-0.8 parts of sodium hydroxide.The viscosity of viscous crude can be effectively reduced when volume is minimum in composite crude oil thinner of the invention；The thinner is added in viscous crude, viscosity of thickened oil can be significantly reduced, makes viscous crude that there is excellent low temperature flow, crude oil production and pipeline transportation, wide market can be effectively applied to.Preparation method of the invention is simple, product structure is controllable and has good eurytopicity.
Description
Technical field
The invention belongs to the technical fields of petroleum industry chemicals, and in particular to a kind of composite crude oil thinner and its preparation
Method.
Technical background
Viscous crude has the physical property that specific gravity is high, viscosity is high, and hydrogen-carbon ratio is lower, and carbon residue content is high, and asphalitine, heavy metal,
Sulphur, the content of nitrogen are higher, the natural high viscous hypercoagulability of viscous crude can make its production, transport, in terms of it is more tired than conventional crude
It is much more difficult.
Viscous crude due to high viscosity, flow resistance it is big, be not easy to exploit.So needing in crude oil recovery process to thick
Oil carries out viscosity reduction, and traditional viscosity reducing process such as heating, viscosity reducing mixes dilute viscosity reduction, reducing viscosity by emulsifying etc. and has its unsurmountable limitation
Property.Currently, being considered as a kind of more promising viscosity reduction method using oil soluble crude oil thinner.Due to being dropped using crude oil
Stick reduction viscosity of thickened oil, improvement rheological characteristic of crude oil operation is easy, general dosage is smaller, cost is relatively low, to the processing nothing of crude oil
It influences, therefore the research and development of efficient heavy crude thinner is had a very important significance.
In recent years, an important directions of oil-soluble viscosity reducers for viscous crude oil development are that a large amount of polarity is introduced into molecular structure
Or the functional group with surface-active, enhance the active force of itself and colloid, asphalitine isopolarity macromolecular.Therefore, one is studied
The compound viscosity reducer for crude oil obtained of kind plurality of raw materials, has great importance.
Summary of the invention
In order to solve the above technical problems, the present invention provides the composite crude oil viscosity reductions with efficient viscosity reduction and pour point depression performance
Agent and preparation method thereof.
The technical scheme adopted by the invention is that:
A kind of composite crude oil thinner, the thinner are prepared from the following raw materials of the following mass: ethylene-vinyl acetate
00 part of copolymer 1,20-40 parts of fatty acid, 20-200 parts modified of phyllosilicate, 1-5 parts of p-methyl benzenesulfonic acid, methanol 100.8-
307.2 parts, 0.2-0.8 parts of sodium hydroxide.
The viscosity-reducing mechanism for the viscosity reducer for crude oil that the present invention obtains: ethylene-vinyl acetate copolymer alcohol in viscosity reduction agent molecule
The polar side chain that the ester group that remaining ester group is obtained with esterification belongs to different length is solved, the two synergistic effect provides strong pole
Property, highly polar group in addition is introduced in the layer structure of modified phyllosilicate, composite viscosity reducer molecule is by means of itself
Strong formation bonding ability penetrates between resin and asphalt sheet molecule, breaks resin and asphalt and stacks and formed
Aggregation, to form sheet molecule amorphous packings, loosely organized, order degree is substantially reduced, spatial extension is little
Structure makes asphalitine, colloid be formed by spacial framework and be destroyed, and makes to be wrapped in petroleum light components release therein
Out, to play the role of effective viscosity reduction.
Further, the content of ethylene segment is 30-60% in ethylene-vinyl acetate copolymer.
Further, fatty acid is carbon atom number in 6 or more, long chain fatty acids.
Further, modified phyllosilicate be through organic amine, organic ammonium salt, pyridiniujm, organic phosphine, organic phosphonium salt,
The phyllosilicate for the polymer modification that amido siloxanes, hydrosiloxane or nitrogenous, phosphorus, oxygen functional group roll into a ball.
Further, layered silicate is the planar aqueous phyllosilicate of serpentine-kaolinite race, smectite race
Planar aqueous phyllosilicate, the planar aqueous phyllosilicate of vermiculite race, pyribole race chain hydrosilicate, slope thread
Stone, tired de- at least one of stone and montmorillonite.
Further, the planar aqueous phyllosilicate of the serpentine-kaolinite race is lizardite, magnalium snake
Stone, gram greenalite, iron zoblizite, nickel lizardite, manganese zoblizite, cutting edge of a knife or a sword zoblizite, nickel serpentine, kaolinite, enlightening
Open at least one of stone, nacrite, galapectite and odenite；The planar aqueous phyllosilicate of smectite race is soap
At least one of stone, sauconite, stevensite, montmorillonite, beidellite, nontronite and chromium-rich nontronite；Vermiculite race plane
The aqueous phyllosilicate of shape is vermiculite；The pyribole race chain hydrosilicate is sepiolite, fine sodium sepiolite, nickel Hai Pao
At least one of stone, vivaolite and manganese vivaolite.
The preparation method of the composite crude oil thinner the following steps are included:
(1) methanol solution of ethylene-vinyl acetate copolymer and the methanol solution of sodium hydroxide are prepared respectively；
(2) methanol solution of ethylene-vinyl acetate copolymer is placed in flask, 75-85 DEG C of oil bath, is condensed back,
The methanol that the methanol solution of sodium hydroxide is added to ethylene-vinyl acetate copolymer under 200-300rpm mixing speed is molten
In liquid, persistently it is stirred to react；
(3) solution after reaction is poured slowly into deionized water and product is precipitated while stirring, after washing by soaking, 80-90
It is dried under the conditions of DEG C, obtains ethylene-vinylacetate-vinyl alcohol ternary copolymer；
(4) ethylene-vinylacetate-vinyl alcohol ternary copolymer, fatty acid and p-methyl benzenesulfonic acid are added in flask,
Toluene makees solvent, obtains esterification products solution after 100-120 DEG C of reaction 6-8h；
(5) modified phyllosilicate is added in esterification products solution, dehydrated alcohol is added after being stirred to react, filters,
After washing, drying, the composite crude oil thinner is obtained.
Ethylene-vinyl acetate copolymer alcoholysis is obtained ethylene-vinylacetate-vinyl alcohol ternary copolymerization by the present invention
Terpolymer is mixed in toluene solution with fatty acid and esterification occurs by object, then by esterification products and modified stratiform
Silicate solutions are mixed to get viscosity reducer for crude oil.The operating process for preparing viscosity reducer for crude oil using this method is simple, product structure
Controllably, there is good eurytopicity.
Wherein, in step (1), the mass concentration of the methanol solution of ethylene-vinyl acetate copolymer is 25-50%, hydrogen
The mass concentration of the methanol solution of sodium oxide molybdena is 10-20%.
Wherein, in step (2), the time being persistently stirred to react is 1-2h.
In step (3), the content of vinylacetate segment is 20- in ethylene-vinylacetate-vinyl alcohol ternary copolymer
40%.The polar vinylacetate segment for retaining certain content, for destroying the overlapping that resin and asphalt is formed in viscous crude
Packing structure important role.
Wherein, it in step (5), is dried in vacuo at 60-80 DEG C, obtains flaxen product.
The invention has the following beneficial effects: composite crude oil thinners of the invention when volume is minimum, can effectively drop
The viscosity of low viscous crude；The thinner is added in viscous crude, viscosity of thickened oil can be significantly reduced, makes viscous crude that there is excellent low temperature
Mobility can be effectively applied to crude oil production and pipeline transportation, wide market.Preparation method letter of the invention
Single, product structure is controllably and with good eurytopicity.
Specific embodiment
The invention will be further described combined with specific embodiments below.
In following embodiments, test apparatus used, reagent, raw material can directly be bought by commercial sources.
Embodiment 1
A kind of composite crude oil thinner is prepared from the following raw materials of the following mass: ethylene-vinyl acetate copolymer (second
50 parts of kaolinite, 3 parts of the p-methyl benzenesulfonic acid, methanol that alkene segment content is 50%) 100 parts, 30 parts of fatty acid, organic amine are modified
304.5 parts, 0.5 part of sodium hydroxide.
The preparation method of above-mentioned composite crude oil thinner the following steps are included:
(1) 100 parts of ethylene-vinyl acetate copolymers are dissolved in 300 parts of methanol, are configured to the second of mass concentration 25%
0.5 part of sodium hydroxide is dissolved in 4.5 parts of methanol, is configured to mass concentration by alkene-vinyl acetate co-polymer methanol solution
The methanol solution of 10% sodium hydroxide；
(2) methanol solution of ethylene-vinyl acetate copolymer is placed in three-necked flask, 80 DEG C of oil bath, is condensed back,
The methanol solution of sodium hydroxide is added in the methanol solution of ethylene-vinyl acetate copolymer under 200rpm mixing speed,
Persistently it is stirred to react 2h；
(3) solution after reaction is poured slowly into deionized water and product is precipitated while stirring, by product in deionized water
In repeatedly after washing by soaking, drying obtains ethylene-vinylacetate-vinyl alcohol ternary copolymer under the conditions of 80 DEG C of baking oven；Pass through
The additional amount of sodium hydroxide and the time of reaction are controlled, adjusting vinylacetate segment content in terpolymer is 30%；
(4) ethylene-vinylacetate-vinyl alcohol ternary copolymer and 30 parts of fatty acid are added in three-necked flask, 600
Part toluene makees solvent, and 3 parts of p-methyl benzenesulfonic acid make catalyst, and 110 DEG C of reaction 6h obtain esterification products solution；
(5) the modified kaolinite of 50 parts of organic amines is added in esterification products solution, is stirred to react 30min, is added anhydrous
Ethyl alcohol, filtering, is washed with low-concentration alkali liquor, removes remaining catalyst in reaction process, then be washed with deionized, and 80 DEG C true
Sky is dry, obtains flaxen product, as composite crude oil thinner.
Embodiment 2
A kind of composite crude oil thinner is prepared from the following raw materials of the following mass: ethylene-vinyl acetate copolymer (second
Alkene segment content is 30%) 100 parts, 20 parts of fatty acid, 0 part organophosphine modified of montmorillonite 2,1 part of p-methyl benzenesulfonic acid, methanol
100.8 parts, 0.2 part of sodium hydroxide.
The preparation method of above-mentioned composite crude oil thinner the following steps are included:
(1) 100 parts of ethylene-vinyl acetate copolymers are dissolved in 100 parts of methanol, are configured to the second of mass concentration 50%
0.2 part of sodium hydroxide is dissolved in 0.8 part of methanol, is configured to mass concentration by alkene-vinyl acetate co-polymer methanol solution
The methanol solution of 20% sodium hydroxide；
(2) methanol solution of ethylene-vinyl acetate copolymer is placed in three-necked flask, 75 DEG C of oil bath, is condensed back,
The methanol solution of sodium hydroxide is added in the methanol solution of ethylene-vinyl acetate copolymer under 250rpm mixing speed,
Persistently it is stirred to react 1.5h；
(3) solution after reaction is poured slowly into deionized water and product is precipitated while stirring, by product in deionized water
In repeatedly after washing by soaking, drying obtains ethylene-vinylacetate-vinyl alcohol ternary copolymer under the conditions of 85 DEG C of baking oven；Pass through
The additional amount of sodium hydroxide and the time of reaction are controlled, adjusting vinylacetate segment content in terpolymer is 20%；
(4) ethylene-vinylacetate-vinyl alcohol ternary copolymer and 20 parts of fatty acid are added in three-necked flask, 600
Part toluene makees solvent, and 1 part of p-methyl benzenesulfonic acid makees catalyst, and 100 DEG C of reaction 8h obtain esterification products solution；
(5) 20 parts of organophosphine modified montmorillonites are added in esterification products solution, are stirred to react 30min, are added anhydrous
Ethyl alcohol, filtering, is washed with low-concentration alkali liquor, removes remaining catalyst in reaction process, then be washed with deionized, and 60 DEG C true
Sky is dry, obtains flaxen product, as composite crude oil thinner.
Embodiment 3
A kind of composite crude oil thinner is prepared from the following raw materials of the following mass: ethylene-vinyl acetate copolymer (second
Alkene segment content is 60%) 100 parts, 40 parts of fatty acid, amido siloxanes are modified 200 parts of nontronite, 5 parts of p-methyl benzenesulfonic acid,
307.2 parts of methanol, 0.8 part of sodium hydroxide.
The preparation method of above-mentioned composite crude oil thinner the following steps are included:
(1) 100 parts of ethylene-vinyl acetate copolymers are dissolved in 300 parts of methanol, are configured to the second of mass concentration 25%
0.8 part of sodium hydroxide is dissolved in 7.2 parts of methanol, is configured to mass concentration by alkene-vinyl acetate co-polymer methanol solution
The methanol solution of 10% sodium hydroxide；
(2) methanol solution of ethylene-vinyl acetate copolymer is placed in three-necked flask, 85 DEG C of oil bath, is condensed back,
The methanol solution of sodium hydroxide is added in the methanol solution of ethylene-vinyl acetate copolymer under 300rpm mixing speed,
Persistently it is stirred to react 1h；
(3) solution after reaction is poured slowly into deionized water and product is precipitated while stirring, by product in deionized water
In repeatedly after washing by soaking, drying obtains ethylene-vinylacetate-vinyl alcohol ternary copolymer under the conditions of 90 DEG C of baking oven；Pass through
The additional amount of sodium hydroxide and the time of reaction are controlled, adjusting vinylacetate segment content in terpolymer is 40%；
(4) ethylene-vinylacetate-vinyl alcohol ternary copolymer is added to three-necked flask together with 40 parts of fatty acid
In, 600 parts of toluene make solvent, and 5 parts of p-methyl benzenesulfonic acid make catalyst, and 120 DEG C of reaction 6h obtain esterification products solution；
(5) the modified nontronite of 200 parts of amido siloxanes is added in esterification products solution, is stirred to react 30min, is added
Dehydrated alcohol, filtering, is washed with low-concentration alkali liquor, removes remaining catalyst in reaction process, then be washed with deionized, 60
DEG C vacuum drying, obtain flaxen product, as composite crude oil thinner.
Embodiment 4
A kind of composite crude oil thinner is prepared from the following raw materials of the following mass: ethylene-vinyl acetate copolymer (second
100 parts of montmorillonite, 4 parts of the p-methyl benzenesulfonic acid, methanol that alkene segment content is 40%) 100 parts, 30 parts of fatty acid, organic amine are modified
303.2 parts, 0.5 part of sodium hydroxide.
The preparation method of above-mentioned composite crude oil thinner the following steps are included:
(1) 100 parts of ethylene-vinyl acetate copolymers are dissolved in 300 parts of methanol, are configured to the second of mass concentration 25%
0.4 part of sodium hydroxide is dissolved in 3.2 parts of methanol, is configured to mass concentration by alkene-vinyl acetate co-polymer methanol solution
The methanol solution of 10% sodium hydroxide；
(2) methanol solution of ethylene-vinyl acetate copolymer is placed in three-necked flask, 80 DEG C of oil bath, is condensed back,
The methanol solution of sodium hydroxide is added to the methanol solution of ethylene-vinyl acetate copolymer under 200rpm mixing speed
In, persistently it is stirred to react 1h；
(3) solution after reaction is poured slowly into deionized water and product is precipitated while stirring, by product in deionized water
In repeatedly after washing by soaking, drying obtains ethylene-vinylacetate-vinyl alcohol ternary copolymer under the conditions of 85 DEG C of baking oven；Pass through
The additional amount of sodium hydroxide and the time of reaction are controlled, adjusting vinylacetate segment content in terpolymer is 30%；
(4) ethylene-vinylacetate-vinyl alcohol ternary copolymer is added to three-necked flask together with 30 parts of fatty acid
In, 600 parts of toluene make solvent, and 4 parts of p-methyl benzenesulfonic acid make catalyst, 110 DEG C of reaction 6h；
(5) the modified montmorillonite of 100 parts of organic amines is added in esterification products solution, is stirred to react 30min, is added anhydrous
Ethyl alcohol, filtering, is washed with low-concentration alkali liquor, removes remaining catalyst in reaction process, then be washed with deionized, and 70 DEG C true
Sky is dry, obtains flaxen product, as composite crude oil thinner.
The viscosity reducer for crude oil 80ppm that Example 1-4 is obtained is added in viscous crude, in 60 DEG C, the mechanical stirring of 200rpm
Effect is lower to handle 30min, keeps thinner evenly dispersed in viscous crude, apparent viscous at 25 DEG C with rheometer test treatment with PPD
Degree.
Comparative example 1
Non- treatment with PPD is handled into 30min under 60 DEG C, the mechanical agitation of 200rpm, is existed with rheometer test crude oil
Apparent viscosity at 25 DEG C.
Comparative example 2
Ethylene-vinyl acetate copolymer (EVA) thinner 80ppm is taken to be added in viscous crude, in 60 DEG C, the machinery of 200rpm
30min is handled under stirring action, keeps thinner evenly dispersed in viscous crude, with table of the rheometer test treatment with PPD at 25 DEG C
See viscosity.
Comparative example 3
The montmorillonite Composite thinner 80ppm for taking acetate ethylene copolymer and organic amine to be modified is added in viscous crude, 60
DEG C, handle 30min under the mechanical agitation of 200rpm, keep thinner evenly dispersed in viscous crude, with rheometer test plus agent
Apparent viscosity of the crude oil at 25 DEG C.
Apparent viscosity of the crude oil of 1-4 of the embodiment of the present invention and comparative example 1-3 under the conditions of 25 DEG C is as shown in table 1.
As shown in Table 1, viscosity reducer for crude oil of the invention has excellent viscosity reduction, pour point depression performance and viscosity reduction, depression effeCt bright
It is aobvious to be better than traditional thinner.
Table 1
Composite crude oil thinner provided by the present invention and preparation method thereof is described in detail above.It answers herein
With a specific example illustrates the principle and implementation of the invention, the explanation of above example is only intended to help to manage
Solve method and its core concept of the invention.It should be pointed out that for those skilled in the art, not departing from
, can be with several improvements and modifications are made to the present invention under the premise of the principle of the invention, these improvement and modification also fall into this hair
In bright scope of protection of the claims.
Claims (10)
1. a kind of composite crude oil thinner, which is characterized in that the thinner is prepared from the following raw materials of the following mass: ethylene-
100 parts of vinyl acetate co-polymer, 20-40 parts of fatty acid, 20-200 parts modified of phyllosilicate, 1-5 parts of p-methyl benzenesulfonic acid,
100.8-307.2 parts of methanol, 0.2-0.8 parts of sodium hydroxide.
2. composite crude oil thinner according to claim 1, which is characterized in that second in ethylene-vinyl acetate copolymer
The content of alkene segment is 30-60%.
3. composite crude oil thinner according to claim 1, which is characterized in that modified phyllosilicate is through organic
Amine, organic ammonium salt, pyridiniujm, organic phosphine, organic phosphonium salt, amido siloxanes, hydrosiloxane or nitrogenous, phosphorus, oxygen functional group
The phyllosilicate of the polymer modification of group.
4. composite crude oil thinner according to claim 3, which is characterized in that phyllosilicate is serpentine-kaolinite
The planar aqueous phyllosilicate of race, the planar aqueous phyllosilicate of smectite race, the planar aqueous laminar silicic acid of vermiculite race
Salt, pyribole race chain hydrosilicate, palygorskite, tired de- at least one of stone and montmorillonite.
5. composite crude oil thinner according to claim 4, which is characterized in that the serpentine-kaolinite race is planar
Aqueous phyllosilicate is lizardite, magnalium serpentine, gram greenalite, iron zoblizite, nickel lizardite, manganese aluminium snake
At least one of stone, cutting edge of a knife or a sword zoblizite, nickel serpentine, kaolinite, dickite, nacrite, galapectite and odenite；The illiteracy
The planar aqueous phyllosilicate of saponite race is saponite, sauconite, stevensite, montmorillonite, beidellite, nontronite and chromium-rich green de-
At least one of stone；The planar aqueous phyllosilicate of vermiculite race is vermiculite；The aqueous silicic acid of pyribole race chain
Salt is at least one of sepiolite, fine sodium sepiolite, nickel sepiolite, vivaolite and manganese vivaolite.
6. a kind of method for preparing the described in any item composite crude oil thinners of claim 1-5, which is characterized in that this method packet
Include following steps:
(1) methanol solution of ethylene-vinyl acetate copolymer and the methanol solution of sodium hydroxide are prepared respectively；
(2) methanol solution of ethylene-vinyl acetate copolymer is placed in flask, 75-85 DEG C of oil bath, is condensed back,
The methanol solution of sodium hydroxide is added to the methanol solution of ethylene-vinyl acetate copolymer under 200-300rpm mixing speed
In, persistently it is stirred to react；
(3) solution after reaction is poured slowly into deionized water and product is precipitated while stirring, after washing by soaking, 80-90 DEG C of item
It is dried under part, obtains ethylene-vinylacetate-vinyl alcohol ternary copolymer；
(4) ethylene-vinylacetate-vinyl alcohol ternary copolymer, fatty acid and p-methyl benzenesulfonic acid are added in flask, toluene
Make solvent, obtains esterification products solution after 100-120 DEG C of reaction 6-8h；
(5) modified phyllosilicate is added in esterification products solution, dehydrated alcohol is added after being stirred to react, filters, washing,
After drying, the composite crude oil thinner is obtained.
7. the preparation method of composite crude oil thinner according to claim 6, which is characterized in that in step (1), ethylene-
The mass concentration of the methanol solution of vinyl acetate co-polymer is 25-50%, and the mass concentration of the methanol solution of sodium hydroxide is
10-20%.
8. the preparation method of composite crude oil thinner according to claim 6, which is characterized in that in step (2), persistently stir
The time for mixing reaction is 1-2h.
9. the preparation method of composite crude oil thinner according to claim 6, which is characterized in that in step (3), ethylene-
The content of vinylacetate segment is 20-40% in vinylacetate-vinylalcohol terpolymer.
10. the preparation method of composite crude oil thinner according to claim 6, which is characterized in that in step (5), 60-80
It is dried in vacuo at DEG C, obtains flaxen product.
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| CN109897620A (en) * | 2019-03-27 | 2019-06-18 | 广州市天河区车陂亚贝思烘焙店 | A kind of efficient cryogenic pour point depressant for crude oil |
| CN112342005A (en) * | 2021-01-05 | 2021-02-09 | 山东奥士德石油技术有限公司 | Environment-friendly efficient thick oil viscosity reducer |
| CN113402724A (en) * | 2021-06-11 | 2021-09-17 | 东北石油大学 | Preparation method of nano composite pour point depressant |
| CN114989373A (en) * | 2022-05-11 | 2022-09-02 | 滨州学院 | Copolymer pour point depressant based on halloysite nanotube and preparation method thereof |
| CN116240006A (en) * | 2021-12-07 | 2023-06-09 | 天津大港油田滨港集团博弘石油化工有限公司 | Modified nano thick oil viscosity reducer and preparation method thereof |
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| CN109897620A (en) * | 2019-03-27 | 2019-06-18 | 广州市天河区车陂亚贝思烘焙店 | A kind of efficient cryogenic pour point depressant for crude oil |
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| CN116240006A (en) * | 2021-12-07 | 2023-06-09 | 天津大港油田滨港集团博弘石油化工有限公司 | Modified nano thick oil viscosity reducer and preparation method thereof |
| CN114989373A (en) * | 2022-05-11 | 2022-09-02 | 滨州学院 | Copolymer pour point depressant based on halloysite nanotube and preparation method thereof |
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