CN102533304A - Compound oil sand oil extracting agent - Google Patents
Compound oil sand oil extracting agent Download PDFInfo
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- CN102533304A CN102533304A CN2010106094818A CN201010609481A CN102533304A CN 102533304 A CN102533304 A CN 102533304A CN 2010106094818 A CN2010106094818 A CN 2010106094818A CN 201010609481 A CN201010609481 A CN 201010609481A CN 102533304 A CN102533304 A CN 102533304A
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- CN
- China
- Prior art keywords
- oil
- sand
- sodium
- compound
- agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003027 oil sand Substances 0.000 title claims abstract description 33
- 150000001875 compounds Chemical class 0.000 title claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 title abstract description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims abstract description 11
- 239000000600 sorbitol Substances 0.000 claims abstract description 11
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 claims abstract description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 6
- 239000011734 sodium Substances 0.000 claims abstract description 6
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 6
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 6
- 229910000162 sodium phosphate Inorganic materials 0.000 claims abstract description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 6
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 6
- -1 oleic acid ester Chemical class 0.000 claims description 9
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 5
- 235000019353 potassium silicate Nutrition 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 abstract description 9
- 238000005406 washing Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000000605 extraction Methods 0.000 abstract description 2
- 229940049964 oleate Drugs 0.000 abstract description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract 2
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 abstract 1
- 239000004115 Sodium Silicate Substances 0.000 abstract 1
- 229920002401 polyacrylamide Polymers 0.000 abstract 1
- 229940051841 polyoxyethylene ether Drugs 0.000 abstract 1
- 229920000056 polyoxyethylene ether Polymers 0.000 abstract 1
- 229920000915 polyvinyl chloride Polymers 0.000 abstract 1
- 239000004800 polyvinyl chloride Substances 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 239000011780 sodium chloride Substances 0.000 abstract 1
- 229910052911 sodium silicate Inorganic materials 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 239000010779 crude oil Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- 239000004576 sand Substances 0.000 description 5
- 239000010426 asphalt Substances 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000003518 caustics Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011295 pitch Substances 0.000 description 3
- 239000013543 active substance Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000011275 tar sand Substances 0.000 description 2
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000010729 system oil Substances 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002569 water oil cream Substances 0.000 description 1
Landscapes
- Lubricants (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to a compound oil sand oil extracting agent; the weight percentages of the components are as follows: 0.1-6% of sodium phosphate; 0.3-2.5% of sodium sulfonate; 0.1-5% of sodium silicate; 1-8% of sodium bicarbonate; 0.05-3.5% of sodium chloride; 0.05-1.5% of polyacrylamide; 0.05-0.85% of sorbitol oleate; 0.01-0.85% of polyvinyl chloride sorbitan; 0.1-0.75% of octyl phenol polyoxyethylene ether; the balance of water; the oil extraction agent has remarkable energy-saving and emission-reducing effects, and can reduce the oil-sand separation temperature by 5 ℃; the oil washing efficiency, the oil content of the residue, the oil recovery rate and the environmental protection index of the residue are all superior to those of the oil agent on the premise of the prior art, the separation efficiency is high, the cost is low, the separated aqueous reagent can be recycled, and the environment is not polluted.
Description
Technical field
The compound oil-sand that the present invention relates to use in a kind of oil-sand washing sepn process is carried finish, and this prescription also can be used for the clean of oil field oil-containing mud and other oil-containing solids waste.
Background technology
Oil-sand is a kind of mixture, is made up of sand, pitch, mineral substance, water and clay, and its internal component is quite complicated.It is a kind of sedimentogeneous rock that contains pitch or other heavy crudes, is mainly used in the extraction oil sands bitumen, to produce synthetic crude.China's oil-sand aboundresources, national oil-sand geological resource amount is 59.7 * 10
8T, can adopt stock number is 22.58 * 10
8T occupies the 5th in the world.As a developing power, China is swift and violent to the increase in demand of crude oil, and imported crude oil accounted for more than 1/3 of national consumption of petroleum total amount in 2005, and the huge breach of following China energy will rely on oil-sand and heavy oil to remedy to a great extent.Estimate that 10 years from now on global conventional crude output will reduce, and the abundant heavy crude resources such as tar sand of reserves have caused the attention of international community.Canada has exploited heavy oil and pitch in a large number and has progressively replaced traditional crude oil, and tar sand will be one of main source of following liquid fuel, be the important supplement of traditional crude oil.Therefore, press for research, the development and utilization work of carrying out the oil-sand reserved resources from strategic height.
The research of oil-sand mainly is to utilize oil-sand system oil, and its method can be divided into thermokalite WATER-WASHING METHOD, solvent-extraction process and pyrogenic silica substantially.Crude oil chemical constitution in the oil-sand is extremely complicated, is mainly condensed-nuclei aromatics and macromolecule hydrocarbon, colloid, asphalt content height.Because its viscosity is high, molecular weight is big, causes their flowabilities and mutual solubility poor, thereby very easily deposits, be adsorbed on institute's contact interface, therefore, the asphalt oil on the oil-sand is quite difficult with separating of silica sand.Domestic in recent years how tame unit furthers investigate the development and use of Inner Mongol water profit characteristic oil-sand; Obtaining certain achievement aspect the oil-sand separation; But glossy type oil-sand a little less than China's many places oil-sand belongs to; Thermokalite washing process effect with the dried up profit type of general branch oil-sand is not satisfactory, and the separating technology of developing the washing separating agent prescription of a kind of suitable China oil-sand characteristics and seeking a kind of the best is very necessary and has realistic meaning.Therefore, achievement of the present invention will have certain directive function for further research China oil-sand exploitation, separation.
The washing separating mechanism of oil-sand is similar to the caustic waterflooding and the surfactant flooding mechanism of tertiary oil production in oil field.For caustic waterflooding mainly is to form naphthenic soap class tensio-active agent through the naphthenic effect in alkaline matter and the crude oil; Thereby reduce the IT between water and the crude oil; Make oil-water emulsion; Change the wettability and the solubilized interfacial film of sandstone, reach the purpose that improves tar productivity through these effects.Can know that by caustic waterflooding and surfactant flooding mechanism oil-sand washing separating mechanism has following several kinds: 1. reduce oil water interfacial tension; 2. the wettability modification of oil/sand; 3. reducing viscosity by emulsifying effect; 4. destroy the stiffness films that solubilisation oils water termination place forms.
Oil-sand separates the existing relevant report of the research work carry finish, and is of " oilfield chemistry " 2005 the 4th phase p375-377, " the 9th the academic nd Annual Meeting collection of national chemical technology " p577-582 in 2005, patent of invention CN101260308, patent of invention CN1511919 etc.The finish of carrying in these reports all contains highly basic sodium hydroxide, not only inferior separating effect (generally about 80%, patent CN101260308 oil-collecting ratio is 94% to oil yield); And because the reaction of the acidic substance such as naphthenic acid in highly basic and the oil sands bitumen needs constantly to replenish alkali lye, alkaline consumption is bigger in the oil-sand sepn process; Required separation temperature higher (more than 90 ℃); Reclaim reagent recycling weak effect, basically can not second stage employ, bigger to environmental hazard.In addition, in above method (CN1511919), relate to the polymkeric substance operational version, its purpose is at underground flocculating settling clay and sand grains, and large usage quantity and will cause that polymkeric substance is underground to be accumulated forms environmental protection hidden danger.In the present invention, use (＜1.5%) polymkeric substance seldom, be stabilize oil moisture phase state, in the antiquated sand of discharging, do not contain organic composition, realize green emissions object.
Summary of the invention
The purpose of this invention is to provide a kind of compound oil-sand of alkaline that do not contain and carry finish and the lower prescription of polymer loading; The finish of carrying with its preparation carries out oil-sand washing separation, and not only separation efficiency is high, and cost is low; Water-based reagent reusable edible after the separation, environmentally safe.
Compound oil-sand of the present invention is put forward finish each component mass percent:
Sodium phosphate 0.1%～6%;
Sodium sulfonate 0.3%～2.5%;
Water glass 0.1%～5%;
Sodium hydrogencarbonate 1%～8%;
Sodium-chlor 0.05%～3.5%;
SEPIGEL 305 0.05%～1.5%;
Sorbitol Powder oleic acid ester 0.05%～0.85%;
SE sorbitol anhydride 0.01%～0.85%;
Octyl phenol Soxylat A 25-7 0.1%～0.75%;
Water surplus
According to the synergistic effect of tensio-active agent, the major advantage that the efficient oil-sand of this Compositional type is carried finish is:
(1) required reagent concentration is lower in the sepn process, generally below 4%.
(2) it is temperature required lower to carry oil, can realize down separating preferably at 85 ℃.
(3) separation efficiency is higher, and oil yield can be up to more than 95%.
(4) but the reagent recirculation utilization after separating has reduced second environmental pollution.
Embodiment
Embodiment 1
The compound oil-sand of the present invention is put forward finish each component mass percent and can be:
Sodium phosphate 1.0%;
Sodium sulfonate 0.8%;
Water glass 0.5%;
Sodium hydrogencarbonate 8.0%;
Sodium-chlor 0.4%;
SEPIGEL 305 0.1%;
Sorbitol Powder oleic acid ester 0.2%;
SE sorbitol anhydride 0.2%;
Octyl phenol Soxylat A 25-7 0.3%;
Water surplus
Embodiment 2
Sodium phosphate 0.1%;
Sodium sulfonate 0.3%%;
Water glass 0.1%%;
Sodium hydrogencarbonate 1%%;
Sodium-chlor 0.05%%;
SEPIGEL 305 0.05%%;
Sorbitol Powder oleic acid ester 0.05%%;
SE sorbitol anhydride 0.01%%;
Octyl phenol Soxylat A 25-7 0.1%%;
Water surplus
Embodiment 3
The compound oil-sand of the present invention is carried oil formula better quality per-cent:
Sodium phosphate 0.65%;
Sodium sulfonate 0.4%;
Water glass 0.3%;
Sodium hydrogencarbonate 5.0%;
Sodium-chlor 0.15%;
SEPIGEL 305 0.07%;
Sorbitol anhydride oleate 0.1%;
SE sorbitol anhydride 0.05%;
Octyl phenol Soxylat A 25-7 0.13%;
Water surplus.
Claims (1)
1. a compound oil-sand is carried finish, it is characterized in that:
The each component mass percent is:
Sodium phosphate 0.1%～6%;
Sodium sulfonate 0.3%～2.5%;
Water glass 0.1%～5%;
Sodium hydrogencarbonate 1%～8%;
Sodium-chlor 0.05%～3.5%;
SEPIGEL 305 0.05%～1.5%;
Sorbitol Powder oleic acid ester 0.05%～0.85%;
SE sorbitol anhydride 0.01%～0.85%;
Octyl phenol Soxylat A 25-7 0.1%～0.75%;
Water surplus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106094818A CN102533304B (en) | 2010-12-17 | 2010-12-17 | Compound oil sand oil extracting agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106094818A CN102533304B (en) | 2010-12-17 | 2010-12-17 | Compound oil sand oil extracting agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102533304A true CN102533304A (en) | 2012-07-04 |
| CN102533304B CN102533304B (en) | 2013-12-04 |
Family
ID=46341363
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010106094818A Active CN102533304B (en) | 2010-12-17 | 2010-12-17 | Compound oil sand oil extracting agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102533304B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849415A (en) * | 2014-03-07 | 2014-06-11 | 天津大学 | Extraction agent used for extracting asphalt from oil sand and application method thereof |
| CN104109551A (en) * | 2013-04-18 | 2014-10-22 | S.P.C.M.公司 | Improved Method Fro Recovering Bitument From Tar Sands |
| CN106010813A (en) * | 2016-05-26 | 2016-10-12 | 中国石油集团渤海钻探工程有限公司 | Oil sludge cleaning agent for fracturing flow-back fluid and preparation method of oil sludge cleaning agent |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4101172A (en) * | 1975-12-22 | 1978-07-18 | Rabbitts Leonard C | In-situ methods of extracting bitumen values from oil-sand deposits |
| CN1613975A (en) * | 2003-11-06 | 2005-05-11 | 王健 | Formula of composite diesel fuel emulsifier |
| US20080047876A1 (en) * | 2006-08-28 | 2008-02-28 | Keller Brian C | Compositions and methods for extracting hydrocarbons from oil sands |
| CN101260308A (en) * | 2008-04-14 | 2008-09-10 | 辽宁石油化工大学 | Separating agent for extracting asphalt from oil-sand |
| CN101665685A (en) * | 2009-09-14 | 2010-03-10 | 天津师范大学 | Oil-displacing agent for enhancing crude oil recovery efficiency in tertiary recovery |
-
2010
- 2010-12-17 CN CN2010106094818A patent/CN102533304B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4101172A (en) * | 1975-12-22 | 1978-07-18 | Rabbitts Leonard C | In-situ methods of extracting bitumen values from oil-sand deposits |
| CN1613975A (en) * | 2003-11-06 | 2005-05-11 | 王健 | Formula of composite diesel fuel emulsifier |
| US20080047876A1 (en) * | 2006-08-28 | 2008-02-28 | Keller Brian C | Compositions and methods for extracting hydrocarbons from oil sands |
| CN101260308A (en) * | 2008-04-14 | 2008-09-10 | 辽宁石油化工大学 | Separating agent for extracting asphalt from oil-sand |
| CN101665685A (en) * | 2009-09-14 | 2010-03-10 | 天津师范大学 | Oil-displacing agent for enhancing crude oil recovery efficiency in tertiary recovery |
Non-Patent Citations (4)
| Title |
|---|
| 周雅萍: "化学驱油体系中各组分在油砂表面上静吸附特征研究", 《化学工程师》 * |
| 张刚: "油砂分离技术的研究现状及影响因素分析", 《内蒙古石油化工》 * |
| 徐冬梅: "微乳液在油砂洗油中的应用", 《精细石油化工进展》 * |
| 陈艳玲: "青海沥青砂油的提取试验研究", 《江汉石油学院学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104109551A (en) * | 2013-04-18 | 2014-10-22 | S.P.C.M.公司 | Improved Method Fro Recovering Bitument From Tar Sands |
| CN104109551B (en) * | 2013-04-18 | 2017-11-21 | S.P.C.M.股份公司 | For the improved method from tar sand recovery pitch |
| CN103849415A (en) * | 2014-03-07 | 2014-06-11 | 天津大学 | Extraction agent used for extracting asphalt from oil sand and application method thereof |
| CN106010813A (en) * | 2016-05-26 | 2016-10-12 | 中国石油集团渤海钻探工程有限公司 | Oil sludge cleaning agent for fracturing flow-back fluid and preparation method of oil sludge cleaning agent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102533304B (en) | 2013-12-04 |
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