CN101391767A - Method for preparing active carbon by using waste walnut outer peel - Google Patents

Method for preparing active carbon by using waste walnut outer peel Download PDF

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Publication number
CN101391767A
CN101391767A CNA2008101218643A CN200810121864A CN101391767A CN 101391767 A CN101391767 A CN 101391767A CN A2008101218643 A CNA2008101218643 A CN A2008101218643A CN 200810121864 A CN200810121864 A CN 200810121864A CN 101391767 A CN101391767 A CN 101391767A
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China
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active carbon
epicarp
outer peel
powder
pecan
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CNA2008101218643A
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CN101391767B (en
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宣贵达
钱建畅
张永钰
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Zhejiang University City College ZUCC
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Zhejiang University City College ZUCC
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Abstract

The invention provides a method for preparing active carbon by using abandoned pecan epicarp, which can not only change waste into valuable, but also can solve the problems of substantial accumulation and decay of the abandoned pecan epicarp, speaking in a more deep-seated meaning. The invention solves the problem mainly by the following proposals: A) the pecan epicarp is naturally dried and grinded in a grinder, and the powder thereof passes through 20 mesh sieve; B) the zinc chloride solution with the concentration of 30 to 60 percent is evenly mixed with the pecan epicarp powder and then impregnated, with the mass ratio of the zinc chloride solution and the pecan epicarp powder of 2 to 5:1 and the impregnation time of 24 to 36 hours; C) the mixture which is obtained from the step B) carries out continuous microwave activation with the microwave power of 500 to 1000W and the impregnation time of 10 to 25 minutes; D) when the product which is obtained from the step C) is cooled, firstly the product is cleaned with diluted hydrochloric acid and later washed with deionized water with the temperature of 60 to 80 DEG C till the pH value is 6 to 7, then the product is filtered, dried under the 80 to 100 DEG C condition, and finally passes through 200 mesh sieve after being grinded, and then the product is obtained.

Description

A kind of waste walnut outer peel that utilizes prepares process of active carbon
Technical field
The present invention relates to a kind of preparation method of active carbon, especially relate to a kind of waste walnut outer peel that utilizes and prepare process of active carbon.
Background technology
Semen Caryae Cathayensis mainly is distributed in counties such as the Ningguo, Shexian County, Jixi, Jingde in Linan, Chunan, Ji'an, Tonglu and the Anhui Province in Zhejiang.Zhejiang Province is about 25.05 ten thousand mu of cultivated area in recent years, and 6300 tons of gross outputs account for 85% of national Semen Caryae Cathayensis gross output, and main product are at Lin'an County.But the behind of high yield is being carried serious environmental secretly and is being destroyed, and the outsourcing of Semen Caryae Cathayensis fruit has pericarp, and its processing back waste exocarp, shell are arbitrarily abandoned by the peasant, cause the severe contamination in several rivers.Utilize processing waste, createing more valuable material is the optimal path that addresses this problem.The raw material of early stage preparation gac mainly is a wood material, seeks the exploration of cheap raw material and comes into one's own and prepare gac in recent years, makes raw material range augmentation.Remove traditional high-quality timber, wood sawdust, charcoal, coconut husk charcoal, palm nuclear charcoal, also have agriculture and forestry by-product and some foodstuffs industry waste to comprise culled wood, bamboo, bark, wind-falls blowdown, boll hull, coffee berry stalk, oil palm shell, bagasse, furfural dregs etc., wherein Exocarpium cocois (Cocos nucifera L) optimum in addition.Hickory nut epicarp is the high-quality resource that a kind of potential prepares gac as a kind of agriculture and forestry by-product in fact, but does not enter people's sight.
Traditional method for preparation of active carbon has gas activation method, chemical activation method, chemicals logos both at home and abroad.The gas activation method is after the raw material charing, with water vapour, carbonic acid gas, air, stack gas etc., carries out the activatory method under 800~900 ℃.But there are following problems in this method: the gac yield is lower, quality is unstable, specific surface area is lower, activation temperature is high, facility investment is big etc., does not have advantage so industrialness is promoted; Chemical activation method is that pharmaceutical chemicals is added in the raw material, heats in rare gas element then, carries out a kind of method of charing and activatory simultaneously.This method is bigger to the corrodibility of equipment, and residue is more, and maximum problem is to have caused environmental pollution, also is not suitable for promoting; The chemicals logos is to add a certain amount of pharmaceutical chemicals (being additive) to carry out the chemical activation dip treating (in the inner transmission road that forms of carbon material in the gac raw material, help the gas activation agent enter carry out etching in the hole), a kind of method of carrying out charing afterwards.The advantage of this method is and can makes the rational gac of pore size distribution by control impregnating ratio and dipping time that specific surface area is big, and the yield height.
Nowadays, microwave method prepares gac has become one of research focus of Chinese scholars in recent years.It has fast, efficient, resource recycling rate height, can not cause remarkable advantages such as secondary pollution, cost be low.Domestic and international many investigators attempt with the microwave preparation gac and have obtained encouraging success, and with the microwave heating of organic moulding waste material, charing activates and makes high grade activated carbon as Kasai, Takakazu etc.Peng Jinhui etc. are raw material with broad bean stalk, rice straw, black type bark mimosa extract waste material, melon seed cases, wheat straw, corn cob, Testa Viciae fabae, bagasse, Cortex Myricae Rubrae waste material, cigarette stalk, pine sawdust etc., the microwave preparation gac.Fan Xian etc. adopt microwave radiation ring, coconut husk, cotton stalk, utilize phosphoric acid, water vapour etc. to make high grade activated carbon for activator.Employing microwave radiation cigarette stalk methods such as Zhang Libo have made the different gac of performance.This shows that it is practicable adopting microwave method to prepare the hickory nut epicarp gac.Utilize the chemicals logos to adopt microwave activation simultaneously, can be more effectively with the high performance gac of hickory nut epicarp preparation becoming.
The patent of Chinese invention patent 200710069706 " the super active carbon based preparation method of a kind of coal doping pecan shell ", the patent No. is the patent " pecan shell becomes charcoal method and charcoal processing device " of CN200610049742.9, it all only is raw material with the pecan shell, its exocarp still goes out of use as a kind of processing after product, does not cause people's generally attention.Though patent CN200510133752.6 has openly reported " charcoal produced by shell of mountain walnut and working method thereof ", also be confined to hickory nut epicarp is processed into charcoal, no matter in economic worth, or all be not so good as to be processed into gac on the use value.
Summary of the invention
Technical problem to be solved by this invention provides a kind of waste walnut outer peel that utilizes and prepares process of active carbon, can not only turn waste into wealth, improve the economic worth of Semen Caryae Cathayensis crop, increase peasant's income, and from a deeper sense, also can solve waste walnut outer peel bulk deposition, septic problem.
Technical problem of the present invention mainly solves by following scheme:
A kind of waste walnut outer peel that utilizes of the present invention prepares process of active carbon, it is characterized in that may further comprise the steps successively:
A) with the hickory nut epicarp natural air drying, pulverize in pulverizer, powder is crossed 20 mesh sieves; B) be to flood behind 30~60% liquor zinci chloridi and the above-mentioned hickory nut epicarp powder uniform mixing concentration, the mass ratio of liquor zinci chloridi and hickory nut epicarp powder is 2~5:1, and dipping time is: 24~36 hours;
C) with step B) mixture that makes carries out the microwave continuous activation, microwave power: 500~1000W, irradiation time: 10-25 minutes;
D) treat step C) after the products therefrom cooling, use earlier the dilute hydrochloric acid pickling, again with temperature be 60~80 ℃ deionized water to be washed till pH value be 6~7, filter products therefrom, under 80~100 ℃ of conditions, dry, after pulverizing 200 mesh sieves, promptly get product.
As preferably, described chlorination zinc concentration is 40%.Because zinc oxide concentration is big more, also big more to the corrosion of equipment, and increase concentration and the adsorptive power of product is improved do not have much influences, consider zinc chloride condition the best of 40% concentration from multi-angles such as economy, environmental protection.
As preferably, the optimum quality ratio of described liquor zinci chloridi and hickory nut epicarp powder is 5:1.
As preferably, step B wherein) dipping time in is 24 hours.
As preferably, step C wherein) microwave power is 700W in.Microwave power is high more, and energy consumption is also big more, can not embody the advantage of microwave method.
As preferably, step C wherein) microwave irradiation time is 20 minutes in.
As preferably, step D wherein) drying time is 1 hour in.
The present invention compared with prior art has following beneficial effect: adopts present widely used microwave method, compares with traditional method, and low consumption, efficient, yield is high and of fine quality.The present invention can be processed into gac with hickory nut epicarp, adopt physico-chemical processes in conjunction with microwave activation, prepared product, iodine number absorption, methylene blue decolorizing ability are all above national standard, and yield is higher than the gac that traditional method makes far away, and cost is also lower.Hickory nut epicarp as the production waste of Semen Caryae Cathayensis, is turned waste into wealth it, not only can improve the economic worth of Semen Caryae Cathayensis crop, increase peasant's income, meet national agriculture, rural areas and farmers policy, and solved the rotten pollution problem of waste heap, have very big value of exploiting and utilizing.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1:
A kind of waste walnut outer peel that utilizes of this example prepares process of active carbon, the steps include:
Behind a, the hickory nut epicarp natural air drying, pulverize, cross 20 mesh sieves with pulverizer;
B, configuration zinc oxide concentration are 40%, will flood behind liquor zinci chloridi and the above-mentioned hickory nut epicarp powder uniform mixing, and the mass ratio of liquor zinci chloridi and hickory nut epicarp powder is 5:1, and soaking storage period is 24 hours;
C, said mixture is carried out the microwave continuous activation, microwave power: 560W, irradiation time: 20 minutes;
D, activation products obtained therefrom are the dilute hydrochloric acid of 1:9 with concentrated hydrochloric acid and distilled water proportioning, and pickling is that to be washed till pH be 6-7 for 60-80 ℃ deionized water with temperature again, filter products therefrom, dry in 80 ℃ baking oven, drying time 1 hour obtains product after 200 mesh sieves.
The iodine number of the hickory nut epicarp gac of preparing is adsorbed as 718.7mg/g, and the methylene blue adsorptive value is 156.6mg/g, and yield is 44.5%.
Embodiment 2:
A kind of waste walnut outer peel that utilizes of this example prepares process of active carbon, the steps include:
Behind a, the hickory nut epicarp natural air drying, pulverize, cross 20 mesh sieves with pulverizer;
B, configuration zinc oxide concentration are 50%, will flood behind liquor zinci chloridi and the above-mentioned hickory nut epicarp powder uniform mixing, and the mass ratio of liquor zinci chloridi and hickory nut epicarp powder is 5:1, and soaking storage period is 24 hours;
C, said mixture is carried out the microwave continuous activation, microwave power is 700W, continuous activation 16 minutes;
D, products obtained therefrom are the dilute hydrochloric acid of 1:9 with concentrated hydrochloric acid and distilled water proportioning, and pickling is that to be washed till pH be 6-7 for 60-80 ℃ deionized water with temperature again, filter products therefrom, dry in 100 ℃ baking oven, drying time 1 hour obtains product after 200 mesh sieves.
The iodine number of the hickory nut epicarp gac of preparing is adsorbed as 735.4mg/g, and the methylene blue adsorptive value is 144.2mg/g, and yield is 45.8%.
Embodiment 3:
A kind of waste walnut outer peel that utilizes of this example prepares process of active carbon, the steps include:
Behind a, the hickory nut epicarp natural air drying, pulverize, cross 20 mesh sieves with pulverizer,
B, configuration zinc oxide concentration are 50%, will flood behind liquor zinci chloridi and the above-mentioned hickory nut epicarp powder uniform mixing, and the mass ratio of liquor zinci chloridi and hickory nut epicarp powder is 5:1, and soaking storage period is 24 hours;
C, said mixture is carried out the microwave continuous activation, microwave power is 480W, continuous activation 20 minutes;
D, products obtained therefrom are the dilute hydrochloric acid of 1:9 with concentrated hydrochloric acid and distilled water proportioning, pickling, and being washed till pH at the deionized water that with temperature is 60-80 ℃ is 6-7, filter products therefrom, dry in 100 ℃ baking oven, drying time 1 hour obtains product after 200 mesh sieves.
The iodine number of the hickory nut epicarp gac of preparing is adsorbed as 619.6mg/g, and the methylene blue adsorptive value is 110.4mg/g, and yield is 47.2%.
Embodiment 4:
A kind of waste walnut outer peel that utilizes of this example prepares process of active carbon, the steps include:
Behind a, the hickory nut epicarp natural air drying, pulverize, cross 20 mesh sieves with pulverizer,
B, configuration zinc oxide concentration are 50%, will flood behind liquor zinci chloridi and the above-mentioned hickory nut epicarp powder uniform mixing, and the mass ratio of liquor zinci chloridi and hickory nut epicarp powder is 5:1, and soaking storage period is 24 hours;
C, said mixture is carried out the microwave continuous activation, microwave power is 700W, continuous activation 18 minutes;
D, products obtained therefrom are the dilute hydrochloric acid of 1:9 with concentrated hydrochloric acid and distilled water proportioning, pickling, and being washed till pH at the deionized water that with temperature is 60-80 ℃ is 6-7, filter products therefrom, dry in 100 ℃ baking oven, drying time 1 hour obtains product after 200 mesh sieves.
The iodine number of the hickory nut epicarp gac of preparing is adsorbed as 689.7mg/g, and the methylene blue adsorptive value is 108.2mg/g, and yield is 44.9%.

Claims (6)

1, a kind of waste walnut outer peel that utilizes prepares process of active carbon, it is characterized in that may further comprise the steps successively:
A) with the hickory nut epicarp natural air drying, pulverize in pulverizer, powder is crossed 20 mesh sieves;
B) be to flood behind 30~60% liquor zinci chloridi and the above-mentioned hickory nut epicarp powder uniform mixing concentration, the mass ratio of liquor zinci chloridi and hickory nut epicarp powder is 2~5:1, and dipping time is: 24~36 hours;
C) with step B) mixture that makes carries out the microwave continuous activation, microwave power: 500~1000W, irradiation time: 10-25 minutes;
D) treat step C) after the products therefrom cooling, use earlier the dilute hydrochloric acid pickling, again with temperature be 60~80 ℃ deionized water to be washed till pH value be 6~7, filter products therefrom, under 80~100 ℃ of conditions, dry, after pulverizing 200 mesh sieves, promptly get product.
2, a kind ofly according to claim 1 utilize waste walnut outer peel to prepare process of active carbon, it is characterized in that: the optimum concn of described zinc chloride is 40%.
3, a kind ofly as claimed in claim 1 or 2 utilize waste walnut outer peel to prepare process of active carbon, it is characterized in that: the optimum quality ratio of described liquor zinci chloridi and hickory nut epicarp powder is 5:1.
4, a kind ofly as claimed in claim 1 or 2 utilize waste walnut outer peel to prepare process of active carbon, it is characterized in that: step B wherein) in best dipping time be 24 hours.
5, a kind ofly as claimed in claim 1 or 2 utilize waste walnut outer peel to prepare process of active carbon, it is characterized in that: step C wherein) in best microwave power be 700W.
6, a kind ofly as claimed in claim 1 or 2 utilize waste walnut outer peel to prepare process of active carbon, it is characterized in that: step C wherein) in best microwave irradiation time be 20 minutes.
7, a kind ofly as claimed in claim 1 or 2 utilize waste walnut outer peel to prepare process of active carbon, it is characterized in that: step D wherein) in best drying time be 1 hour.
CN 200810121864 2008-11-03 2008-11-03 Method for preparing active carbon by using waste walnut outer peel Expired - Fee Related CN101391767B (en)

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101559989B (en) * 2009-05-15 2011-04-20 黄樟焱 Method for preparing powdered water treatment material used together with microporous ceramics
CN102951639A (en) * 2012-10-31 2013-03-06 中国计量学院 Method for preparing high specific surface area active carbon by using carya cathayensis peels
CN103816868A (en) * 2014-03-03 2014-05-28 石河子大学 Mesoporous sugar beet pulp activated carbon and microwave-assisted preparation method thereof
CN103833013A (en) * 2012-11-23 2014-06-04 海洋王照明科技股份有限公司 Graphene and preparation method thereof
CN103848473A (en) * 2014-03-13 2014-06-11 北京工业大学 Method for removing methylene blue dye in wastewater through walnut shell biomass charcoal adsorbent
CN103864168A (en) * 2014-03-13 2014-06-18 北京工业大学 Method for removing rhodamine B dye from wastewater by walnut shell biomass charcoal adsorbent
CN104495843A (en) * 2015-01-26 2015-04-08 姚雯楸 Method for making activated carbon by using wild peach pit shells
CN104925806A (en) * 2014-03-20 2015-09-23 吕凤楼 Preparation method of walnut activated carbon
CN105731453A (en) * 2016-01-25 2016-07-06 石河子大学 Preparation method for apricot shell activated carbon and apricot activated carbon
CN106040186A (en) * 2016-06-12 2016-10-26 浙江农林大学 Method for synthesizing porous adsorption materials from traditional Chinese medicine residues
CN106552612A (en) * 2015-09-29 2017-04-05 云南民族大学 A kind of microwave improves the method that activity of bamboo charcoal increases absorption property
CN107200326A (en) * 2017-06-26 2017-09-26 四川建筑职业技术学院 A kind of method that utilization walnut shell prepares scavenging material
CN107445161A (en) * 2017-09-25 2017-12-08 常州西夏墅东方工具有限公司 A kind of preparation method of melon seed cases hydrothermal activity charcoal
CN107473217A (en) * 2017-09-22 2017-12-15 广州聚禅现代农业研究院有限公司 A kind of preparation method and application of sunflower seed shell activated carbon
CN112938968A (en) * 2021-03-02 2021-06-11 安徽金轩科技有限公司 Method for producing activated carbon by using furfural residues

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101559989B (en) * 2009-05-15 2011-04-20 黄樟焱 Method for preparing powdered water treatment material used together with microporous ceramics
CN102951639A (en) * 2012-10-31 2013-03-06 中国计量学院 Method for preparing high specific surface area active carbon by using carya cathayensis peels
CN103833013A (en) * 2012-11-23 2014-06-04 海洋王照明科技股份有限公司 Graphene and preparation method thereof
CN103816868A (en) * 2014-03-03 2014-05-28 石河子大学 Mesoporous sugar beet pulp activated carbon and microwave-assisted preparation method thereof
CN103848473A (en) * 2014-03-13 2014-06-11 北京工业大学 Method for removing methylene blue dye in wastewater through walnut shell biomass charcoal adsorbent
CN103864168A (en) * 2014-03-13 2014-06-18 北京工业大学 Method for removing rhodamine B dye from wastewater by walnut shell biomass charcoal adsorbent
CN103864168B (en) * 2014-03-13 2015-10-28 北京工业大学 The method of rhdamine B in waste water removed by a kind of nut-shell biomass charcoal sorbent material
CN103848473B (en) * 2014-03-13 2015-09-02 北京工业大学 The method of methylene blue in waste dyestuff removed by a kind of nut-shell biomass charcoal sorbent material
CN104925806A (en) * 2014-03-20 2015-09-23 吕凤楼 Preparation method of walnut activated carbon
CN104495843A (en) * 2015-01-26 2015-04-08 姚雯楸 Method for making activated carbon by using wild peach pit shells
CN106552612A (en) * 2015-09-29 2017-04-05 云南民族大学 A kind of microwave improves the method that activity of bamboo charcoal increases absorption property
CN105731453A (en) * 2016-01-25 2016-07-06 石河子大学 Preparation method for apricot shell activated carbon and apricot activated carbon
CN106040186A (en) * 2016-06-12 2016-10-26 浙江农林大学 Method for synthesizing porous adsorption materials from traditional Chinese medicine residues
CN106040186B (en) * 2016-06-12 2018-07-06 浙江农林大学 A kind of method of Chinese medicine dreg synthesis porous adsorbing material
CN107200326A (en) * 2017-06-26 2017-09-26 四川建筑职业技术学院 A kind of method that utilization walnut shell prepares scavenging material
CN107200326B (en) * 2017-06-26 2019-10-25 四川建筑职业技术学院 A method of scavenging material is prepared using walnut shell
CN107473217A (en) * 2017-09-22 2017-12-15 广州聚禅现代农业研究院有限公司 A kind of preparation method and application of sunflower seed shell activated carbon
CN107445161A (en) * 2017-09-25 2017-12-08 常州西夏墅东方工具有限公司 A kind of preparation method of melon seed cases hydrothermal activity charcoal
CN112938968A (en) * 2021-03-02 2021-06-11 安徽金轩科技有限公司 Method for producing activated carbon by using furfural residues

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