CN103011895B - Air sand and preparation method thereof - Google Patents

Air sand and preparation method thereof Download PDF

Info

Publication number
CN103011895B
CN103011895B CN201210507438.XA CN201210507438A CN103011895B CN 103011895 B CN103011895 B CN 103011895B CN 201210507438 A CN201210507438 A CN 201210507438A CN 103011895 B CN103011895 B CN 103011895B
Authority
CN
China
Prior art keywords
sand
shell powder
polyvinyl alcohol
calcined shell
dioxide
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.)
Expired - Fee Related
Application number
CN201210507438.XA
Other languages
Chinese (zh)
Other versions
CN103011895A (en
Inventor
罗乐平
雷荣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LISHUI ZHUOYUE STATIONERY MANUFACTURING Co Ltd
Original Assignee
LISHUI ZHUOYUE STATIONERY MANUFACTURING Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by LISHUI ZHUOYUE STATIONERY MANUFACTURING Co Ltd filed Critical LISHUI ZHUOYUE STATIONERY MANUFACTURING Co Ltd
Priority to CN201210507438.XA priority Critical patent/CN103011895B/en
Publication of CN103011895A publication Critical patent/CN103011895A/en
Application granted granted Critical
Publication of CN103011895B publication Critical patent/CN103011895B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention provides air sand and a preparation method thereof. Air clay is prepared from the components of: silicon dioxide, calcined shell powder, polyethylene glycol, polyvinyl alcohol, foam powder k12, glycerol and propylene glycol. The preparation method comprises the following steps of: (1) adding the silicon dioxide which is used as a main body, the calcined shell powder which is used as a molecular structure connecting carrier, and the polyethylene glycol, the polyvinyl alcohol and the foam powder k12 which are used as reaction elements into a heatable reaction kettle; (2) stirring when the reaction kettle rotates at a constant speed of 25rpm; (3) raising the temperature to ensure that the reaction elements fully react with the silicon dioxide and the calcined shell powder to achieve an effect of shaping micro-particles; (4) after the temperature is up to 120 DEG C, stopping heating and continuously mixing; (5) adding a propylene glycol solution with the concentration being about 70 percent, stirring, mixing, and adjusting the rotating speed of the reaction kettle to be 20 rpm; (6) lowering the temperature, adding the glycerol, and adjusting the rotating speed of the reaction kettle to be 40rpm; (7) rotating for 10 minutes to obtain the air sand. The method has the characteristics of reasonable technological process and high product yield.

Description

A kind of air sand and preparation method thereof
Technical field
The invention belongs to Material Field, be specifically related to a kind of air sand self with restraining and sterilizing bacteria function with its preparation method.
Background technology
Children like playing sand, and the time of having forgotten that at every turn all can play in sand ground, some kindergartens that have have also prepared the place of sand specially for child, and child likes playing sand and meets their cognitive levels.And, play the raising that sand contributes to strengthen child's perception, contribute to develop child's imagination, also contribute to help child's fine movement development, the composition that sand is the most general is silicon-dioxide, be generally quartzy form, because of its stable chemical nature and quality hard, proportion is high, the objectionable impuritiess such as easy breed bacteria, single molecular structure cannot ensure its plasticity-and security, at present the most high-grade is in the world Korea S's air sand, can utilize various moulding moulds freely to create, also the design works of can giving the rein to imagination, reuse, nontoxic, free posing, but there is equally certain defect, for example, Korea S's air sand has lost sand mobility and loose, trample rear formation knot tying, it just look like heavy knot after common river sand absorbs water, be difficult to the sand after the moving knot tying of shovel with children's strength, cost causes selling at exorbitant prices, average family purchasing power is restricted.
Summary of the invention
Technical problem to be solved by this invention is: the characteristic that has retained sand has thoroughly changed again sand molecular structure, make the original feature of the existing sand of product, there is again soft, light specific gravity, do not add water just can reach the moulding effect of sand carving, self-restraining and sterilizing bacteria composition safety performance is superior, meet father and mother's making excessive demands toy safety, can effectively utilize the husky instrument of various objects for appreciation to operate, the characteristic of true perception sand.
The invention provides a kind of air sand, its feature is being, made by silicon-dioxide, calcined shell powder, polyoxyethylene glycol, polyvinyl alcohol, sparklet k12, glycerine, 7 kinds of components of propylene glycol, the mass content of described each component is respectively silicon-dioxide: 60 ~ 70%, calcined shell powder: 15 ~ 20%, polyoxyethylene glycol: 5 ~ 8%, polyvinyl alcohol: 1.5 ~ 2.5%, sparklet k12:2.5 ~ 3.5%, glycerine: 3 ~ 5%, propylene glycol: 7 ~ 9%, and each component sum of air sand is 100%.
For the mass content mentioned above, further choosing preference is: air sand is made up of the component of following mass content: silicon-dioxide 70%, calcined shell powder 10%, polyoxyethylene glycol 2%, polyvinyl alcohol 2.5%, sparklet 2.5%, glycerine 5%, propylene glycol 8%, each component sum of air clay is 100%.
Air sand provided by the invention, its characteristic is: solve product appearance and common sand consistence, moulding function is better than sand, not knot tying, is subject to can shape after External Force Acting, tack-free, self have restraining and sterilizing bacteria function, chance water decomposition speed is fast, and mobility is the same with the beach sand that humidity is 15%.
Another object of the present invention provides the preparation method of air sand, and the method has the advantages that technological process is reasonable, product yield is high.
The present invention also provides a kind of preparation method of air sand ,the method comprises the steps: that (1) utilizes silicon-dioxide for main body, and calcined shell powder is molecular structure connection carrier, and polyoxyethylene glycol, polyvinyl alcohol, sparklet K12 are reactive element, join together in the reactor that can heat up; (2) reactor stirring at the uniform velocity down rotating speed 25/ minute; (3) heat up its reactive element is fully reacted with silicon-dioxide and calcined shell powder, play particulate fixed effect; (4) reach after 120 degree, close heating and continuous mixing; (5) add the propylene glycol solution of 70% left and right concentration, be uniformly mixed reactor adjustment of rotational speed to 20 rev/min; (6) reduce temperature and add glycerine, reactor adjustment of rotational speed to 40 rev/min; (7) continuing 10 minutes products completes.
The method has the advantages that technological process is reasonable, product yield is high.
specific implementation method
The invention provides a kind of air sand, made by silicon-dioxide, calcined shell powder, polyoxyethylene glycol, polyvinyl alcohol, sparklet k12, glycerine, 7 kinds of components of propylene glycol, the mass content of described each component is respectively silicon-dioxide: 70%, calcined shell powder: 10%, polyoxyethylene glycol: 5 ~ 8%, polyvinyl alcohol: 1.5 ~ 2.5%, sparklet k12:2.5 ~ 3.5%, glycerine: 3 ~ 5%, sorbyl alcohol: 7 ~ 9%, and each component sum of air sand is 100%.
For the superiority of each component, below content further explain:
One, silicon-dioxide claims again silica, chemical formula SiO 2.Occurring in nature has two kinds of crystalline silica and soft silicas.Crystalline silica is because of crystalline structure difference, is divided into three kinds of quartz, tridymite and cristobalites.Pure quartz is clear crystal, and the quartz of large and transparent prism-shaped is crystal.If the crystal that contains trace impurity, with different colours, has amethyst, yellow quartz, smoky quartz etc.Common sand is tiny quartz crystal, has yellow ground (more iron contamination) and white sand (impurity is few, purer).In silica crystals, 4 valence electrons and 4 Sauerstoffatoms of Siliciumatom form 4 covalent linkage, and Siliciumatom is positioned at the center of positive tetrahedron, and 4 Sauerstoffatoms are positioned on 4 drift angles of positive tetrahedron, and whole crystal is a huge molecule, SiO 2being that the simplest formula that represents composition does not represent single silicon dioxide molecules, is only the ratio that represents the atom number of silicon and oxygen in silica crystals.SiO 2the bond energy of middle Si-O key is very high, fusing point, boiling point higher (1723 DEG C of fusing points, 2230 DEG C of boiling points).The diatomite that nature exists is soft silica, is the low remains that wait waterplant diatom, is white solid or Powdered, porous, light weight, soft solid, and adsorptivity is strong;
Two. oyster shell whiting has absorption, decomposes the function such as effect and adjusting air humidity of (formaldehyde, benzene, TVOC, ammonia), eliminates odor function, antibacterial, bacteriostatic action, the oyster shell whiting film of firing has extremely strong antibacterial and germicidal action to intestinal bacteria, in addition Salmonellas, yellow glucose fungus is also had to remarkable effect.Not only there is high performance germ resistance, and there is " aquatic respiration " function of anticorrosion, to prevent flat lice function, antistatic performance, adjusting air humidity uniqueness.
Three, polyoxyethylene glycol (PEG) product can be used for medicament.The polyoxyethylene glycol that relative molecular weight is lower can be used as solvent, solubility promoter, o/w type emulsifying agent and stablizer, be used for making the outstanding agent of cement, emulsion, injection etc., also as water-soluble ointment base and suppository base, the viscosity that the wax-like polyoxyethylene glycol of solid that relative molecular weight is high is usually used in increasing low-molecular-weight liquid PEG with become solidity, and repay other drug outward; For not diffluent medicine in water, this product can be made the carrier of solid dispersion, disperse object to reach solid, PEG4000, PEG6000 are good coating materials, hydrophilic polishing material, film material and capsule material, softening agent, lubricant and Basic compose, for the preparation of tablet, pill, capsule, microcapsule etc.
Four, this product of PVAC polyvinylalcohol is a kind of anion surfactant, white or faint yellow (grain) shape solid.Belong to the Typical Representative of sulfuric acid ester tensio-active agent, nontoxic, be slightly soluble in alcohol, be insoluble to chloroform, ether, soluble in water, good with the multiple compatibleness of negatively charged ion, nonionic, there is good emulsifying, whipability, foaming, infiltration, decontamination and dispersing property, bubble is abundant, stable lasting, biological degradation is fast.Insensitive to alkali and hard water, long-term heating should not exceed 95 DEG C.Utilize its foaminess, can be by adding other additive to improve its stimulation degree, be that degreasing power reduces, washing good hand touch, is the main component of liquid detergent.
Five, sparklet k12 is widely used in toothpaste, soap, shampoo, washing powder, bubble bath lotion, hand cleaner and makeup as whipping agent.Industry and other industry can be used as the washing composition, metal ore dressing flotation agent, electroplating additive, rubber pange agent, mortar king whipping agent, mixed earth air entrapment agent, pesticide wettable processing, water-latex type tackiness agent, coating lubricant of emulsifying agent, fire-fighting medium whipping agent, textile auxiliary agent, Wool detergent, silk hairs fine work fabric etc.
Six. the chemistry glycerine glycerol by name of glycerine, pleasantly sweet, be water white transparency viscous liquid, there is good water-absorbent, be commonly used to do the interpolation raw material of makeup.Glycerine is the most general wetting Agent for Printing Inks, and price is also very cheap, and nearly all skin care products has its existence.Glycerine can be drawn airborne moisture content to skin moisture-keeping, also the moisture content in skin can be pinned, and does not allow it run off.
Seven. propylene glycol is the stable water-absorbent liquid of colourless thickness, and almost tasteless odorless, inflammable, low toxicity.With water, ethanol and multiple immiscible organic solvent.187.3 DEG C of boiling points.Fusing point-60 DEG C.Relative density 1.0381 (20/20 DEG C).Refractive index n D (20 DEG C) 1.4326.Surface tension (20 DEG C) 38mN/m.Viscosity (20 DEG C) 60.5mPas.Specific heat capacity (20 DEG C) 2.49kJ/ (kg DEG C).Vaporization heat (101.3kPa) 711kJ/kg.The combustion heat (25 DEG C) 1824.0kJ/mol.99 DEG C of flash-points (opening cup).415.5 DEG C of spontaneous ignition temperatures.352 DEG C of critical temperatures.Emergent pressure 6.1MPa.End-use propylene glycol can be used as the raw material of unsaturated polyester resin, the raw material of tensio-active agent, emulsifying agent and emulsion splitter.Can be used as mould inhibitor, sanitas, frostproofer and tobacco humectant.
According to the characteristic of above-mentioned each component, the present invention draws each ratio of component by experiment, and the right constituent mass content ratio further illustrating in practical application is given an example by lower:
Embodiment 1
A kind of air sand ,made by silicon-dioxide, calcined shell powder, polyoxyethylene glycol, polyvinyl alcohol, sparklet k12, glycerine, 7 kinds of components of sorbyl alcohol, the mass content of each component is respectively silicon-dioxide: 60%, calcined shell powder: 15%, polyoxyethylene glycol: 5 ~ 8%, polyvinyl alcohol: 1.5 ~ 2.5%, sparklet k12:2.5 ~ 3.5%, glycerine: 3 ~ 5%, propylene glycol: 7 ~ 9%, each component sum of air sand is 100%, because polyoxyethylene glycol, polyvinyl alcohol, sparklet k12, glycerine and sorbyl alcohol are as additive, its numerical value is got in scope.
Embodiment 2
A kind of air sand ,made by silicon-dioxide, calcined shell powder, polyoxyethylene glycol, polyvinyl alcohol, sparklet k12, glycerine, 7 kinds of components of propylene glycol, the mass content of each component is respectively silicon-dioxide: 66%, calcined shell powder: 15%, polyoxyethylene glycol: 5 ~ 8%, polyvinyl alcohol: 1.5 ~ 2.5%, sparklet k12:2.5 ~ 3.5%, glycerine: 3 ~ 5%, propylene glycol: 7 ~ 9%, each component sum of air sand is 100%, because polyoxyethylene glycol, polyvinyl alcohol, sparklet k12, glycerine and sorbyl alcohol are as additive, its numerical value is got in scope.
Embodiment 3
A kind of air sand ,made by silicon-dioxide, calcined shell powder, polyoxyethylene glycol, polyvinyl alcohol, sparklet k12, glycerine, 7 kinds of components of propylene glycol, the mass content of each component is respectively silicon-dioxide: 60%, calcined shell powder: 20%, polyoxyethylene glycol: 5 ~ 8%, polyvinyl alcohol: 1.5 ~ 2.5%, sparklet k12:2.5 ~ 3.5%, glycerine: 3 ~ 5%, propylene glycol: 7 ~ 9%, each component sum of air sand is 100%, because polyoxyethylene glycol, polyvinyl alcohol, sparklet k12, glycerine and sorbyl alcohol are as additive, its numerical value is got in scope.
With reference to flexibility, feel and the flowing property of the finished product, in original span, show that best numerical value samples:
Embodiment 4
A kind of air sand ,made by silicon-dioxide, calcined shell powder, polyoxyethylene glycol, polyvinyl alcohol, sparklet k12, glycerine, 7 kinds of components of propylene glycol, the mass content of each component is respectively silicon-dioxide: 66%, calcined shell powder: 15%, polyoxyethylene glycol: 5 ~ 8%, polyvinyl alcohol: 1.5 ~ 2.5%, sparklet k12:2.5 ~ 3.5%, glycerine: 3 ~ 5%, propylene glycol: 7 ~ 9%, each component sum of air sand is 100%, because polyoxyethylene glycol, polyvinyl alcohol, sparklet k12, glycerine and sorbyl alcohol are as additive, its numerical value is got in scope.
If need further to limit for the numerical value of the additive in embodiment 4, can adopt following numerical value:
Embodiment 5
A kind of air sand ,made by silicon-dioxide, calcined shell powder, polyoxyethylene glycol, polyvinyl alcohol, sparklet k12, glycerine, 7 kinds of components of propylene glycol, the mass content of each component is respectively silicon-dioxide: 66%, calcined shell powder: 15%, polyoxyethylene glycol: 5 ~ 8%, polyvinyl alcohol: 1.5 ~ 2.5%, sparklet k12:2.5 ~ 3.5%, glycerine: 3 ~ 5%, propylene glycol: 7 ~ 9%, and each component sum of air sand is 100%.
Air sand provided by the invention, its characteristic is: the characteristic that has retained sand has thoroughly changed again sand molecular structure, make the original feature of the existing sand of product, there is again soft, light specific gravity, do not add water just can reach the moulding effect of sand carving, self-restraining and sterilizing bacteria composition safety performance is superior, meet father and mother's making excessive demands toy safety, can effectively utilize the husky instrument of various objects for appreciation to operate, the characteristic of true perception sand.
The present invention also provides a kind of preparation method of air sand ,the method comprises the steps: that (1) utilizes silicon-dioxide for main body, and calcined shell powder is molecular structure connection carrier, and polyoxyethylene glycol, polyvinyl alcohol, sparklet K12 are reactive element, join together in the reactor that can heat up; (2) reactor stirring at the uniform velocity down rotating speed 25/ minute; (3) heat up its reactive element is fully reacted with silicon-dioxide and calcined shell powder, play particulate fixed effect; (4) reach after 120 degree, close heating and continuous mixing; (5) add the Sorbitol Solution USP of 70% left and right concentration, be uniformly mixed reactor adjustment of rotational speed to 25 rev/min; (6) reduce temperature and add glycerine, reactor adjustment of rotational speed to 40 rev/min; (7) continuing 10 minutes products completes.
This preparation process has fully been decomposed the chemical action of reactive element, utilizes chemical temperatures control and physical motion rotating speed to reach stable material structure, has reached expectation object.
The relative prior art of product of the present invention:
Comparative: solve product appearance and common sand consistence, moulding function is better than air sand, not knot tying, be subject to can shape after External Force Acting, tack-free, self there is restraining and sterilizing bacteria function, chance water decomposition speed is fast, mobility is the same at 15% beach sand with humidity, is the popular product of environmental protection of real meaning.
Security: adopt the material compatibility of occurring in nature ecosystem synthetic completely; children's torso is injured to composition without any stimulation; particularly select the general skin care such as glycerine, the Bei Fen element of makeup; after contact, skin is played to protection and moisten effect, also can not cause consequence even children eat and fall into eyes because of carelessness by mistake.
The feature of environmental protection: this product all material is all taken from nature, molecular structure disperses, after child plays and abandons, as long as heavy rain is just dissolved in nature completely, unharmful substance is residual, to soil without any pollution destructiveness.
Product detects: this product has been passed through toy for children inspection center, Shanghai safety performance and detected, and EN71 detects, and SGS detects, and bacteriostasis property detects, and indices is all better than national standard.

Claims (1)

1. the preparation method of an air sand, this air sand is made up of the component of following mass content: silicon-dioxide 70%, calcined shell powder 10%, polyoxyethylene glycol 2%, polyvinyl alcohol 2.5%, K12 sparklet 2.5%, glycerine 5%, propylene glycol 8%, each component sum of air sand is 100%, and its preparation method comprises the steps:
(1) utilize silicon-dioxide for main body, calcined shell powder is molecular structure connection carrier, and polyoxyethylene glycol, polyvinyl alcohol, sparklet K12 are reactive element, joins together in the reactor that can heat up; (2) reactor stirring at the uniform velocity down 15 revs/min of rotating speeds; (3) heat up its reactive element is fully reacted with silicon-dioxide and calcined shell powder, play particulate fixed effect; (4) reach after 120 degree, close heating and continuous mixing; (5) add the propylene glycol solution of 70% concentration, be uniformly mixed reactor adjustment of rotational speed to 25 rev/min; (6) reduce temperature and add glycerine, reactor adjustment of rotational speed to 40 rev/min; (7) continuing 10 minutes products completes; (8) after work in-process take the dish out of the pot, temperature must drop to envrionment temperature, then enters high speed reactor and mixes that stirring expanded after 10 minutes pours out, and completes all process steps.
CN201210507438.XA 2012-12-03 2012-12-03 Air sand and preparation method thereof Expired - Fee Related CN103011895B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210507438.XA CN103011895B (en) 2012-12-03 2012-12-03 Air sand and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210507438.XA CN103011895B (en) 2012-12-03 2012-12-03 Air sand and preparation method thereof

Publications (2)

Publication Number Publication Date
CN103011895A CN103011895A (en) 2013-04-03
CN103011895B true CN103011895B (en) 2014-07-09

Family

ID=47961063

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210507438.XA Expired - Fee Related CN103011895B (en) 2012-12-03 2012-12-03 Air sand and preparation method thereof

Country Status (1)

Country Link
CN (1) CN103011895B (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103771770B (en) * 2013-12-01 2016-09-07 肖霄 A kind of moulding sand
WO2016011593A1 (en) * 2014-07-22 2016-01-28 陈信雄 Toy simulation sand and preparation method therefor
WO2016011595A1 (en) * 2014-07-22 2016-01-28 陈信雄 Toy sand for children and preparation method therefor
CN106007476B (en) * 2016-05-19 2018-05-15 衢州贝蒙文教用品制造有限公司 antibacterial air sand composition and preparation method thereof
CN106861196B (en) * 2017-04-01 2019-04-26 青岛乐谷休闲游乐设备有限公司 A kind of preparation method of recreation ground shell sand

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215185A (en) * 2007-12-27 2008-07-09 佛山石湾鹰牌陶瓷有限公司 Method for producing ceramic brick decorated with aperture
CN102101792A (en) * 2009-12-18 2011-06-22 黄家洞 Production process of light foam ceramic bricks
CN102656618A (en) * 2010-08-19 2012-09-05 马卡砂株式会社 Non-hardening clay composite and method for manufacturing same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101215185A (en) * 2007-12-27 2008-07-09 佛山石湾鹰牌陶瓷有限公司 Method for producing ceramic brick decorated with aperture
CN102101792A (en) * 2009-12-18 2011-06-22 黄家洞 Production process of light foam ceramic bricks
CN102656618A (en) * 2010-08-19 2012-09-05 马卡砂株式会社 Non-hardening clay composite and method for manufacturing same

Also Published As

Publication number Publication date
CN103011895A (en) 2013-04-03

Similar Documents

Publication Publication Date Title
CN103011895B (en) Air sand and preparation method thereof
TWI325853B (en) Glassy antibacterial agent and antibacterial product
JPH08104605A (en) Antibacterial agent
CN106007478B (en) Ultralight clay composition and preparation method thereof
CA2126339C (en) Play material composition
CN103284938B (en) A kind of infant wet tissue annex solution and processing technology thereof and infant wet tissue
WO1993016132A1 (en) Play material based on cross-link sodium alginate
CN107151462A (en) It is a kind of long-acting except aldehyde, antibacterial, mould proof house ornamentation spray and its manufacture method
CN108948615A (en) A kind of nontoxic crystal mud of intelligence development DIY and preparation method thereof
CN109289211A (en) A kind of production method of antibacterial educational toy
CN103011686B (en) Air clay and preparation method thereof
CN101869084A (en) Preparation method for magnetic pearl nucleus
CN106146960A (en) A kind of preparation method of vapor-permeable type antibacterial sponge
CN107236318A (en) A kind of degradable bamboo is nanocomposite moulded
CN104161044A (en) Preparation method and application of organic/inorganic compound antibacterial agent
US3850864A (en) Compound to make products,per se and to cast other materials
CN100400272C (en) Manufacture method of linear low density polyethylene lawn-shape ground cushion
CN106085665B (en) A kind of functional polyurethane soap and preparation method thereof
CN111437615B (en) Preparation method of double-component instant safe bubble water concentration agent
JP2001026439A (en) Glass based antibacterial agent
KR101842109B1 (en) Shapable soap floating on water and the manufacturing method thereof
CN104327464A (en) APET film having fragrance
CN104671701B (en) A kind of toy sand using solvent-borne type rubber polymer to make and preparation method thereof
CN104877285A (en) Cotton mud preparation process
KR100361019B1 (en) Playdough for Kids and Preparation Thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20140709

Termination date: 20141203

EXPY Termination of patent right or utility model