CN106244313A - A kind of water substitution Oleum Camelliae method for producing - Google Patents
A kind of water substitution Oleum Camelliae method for producing Download PDFInfo
- Publication number
- CN106244313A CN106244313A CN201610686012.3A CN201610686012A CN106244313A CN 106244313 A CN106244313 A CN 106244313A CN 201610686012 A CN201610686012 A CN 201610686012A CN 106244313 A CN106244313 A CN 106244313A
- Authority
- CN
- China
- Prior art keywords
- water
- oleum camelliae
- producing
- extraction
- layer
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of water substitution Oleum Camelliae method for producing, camellia oleosa seed is shelled, be dried, pulverize after mix with water, pH to 4 4.5 is adjusted with glacial acetic acid, add sodium chloride, mechanical shaking extraction, separates upper strata oil reservoir, is extracted with ethyl acetate water layer and emulsion layer, merging oil reservoir and ethyl acetate layer, vacuum drying obtains product.Compare existing Oleum Camelliae extraction technique, camellia oleosa seed oil extracting rate >=87% in the present invention, clear oil-collecting ratio >=92%, organic solvent-free residual in Oleum Camelliae, remain without tea saponin；Technique is simple to operation simultaneously, is suitable for industrialized production.
Description
Technical field
The present invention relates to Oleum Camelliae manufacture field, be specifically related to a kind of water substitution Oleum Camelliae method for producing.
Background technology
Oleum Camelliae obtains from Theaceae tea oil tree seed, has another name called Oleum Camelliae, Camellia oil, is the distinctive woody oil of China
Fat.China's oil tea aboundresources, camellia oleifera lam area accounts for more than 80% that woody edible oil charge level is long-pending, is distributed widely in south 17
The knob of individual province, especially with Guangxi, Hunan, Jiangxi, the ground such as Yunnan be most.
Containing several functions composition in Oleum Camelliae, for maintaining the function of cardiovascular system, improve body immunity, reduce
Cholesterol, prevents and treats hypertension have obvious effect.Additionally, traditional medicine is thought, Oleum Camelliae has clearing away heat and eliminating dampness, parasite killing to detoxify
Effect, can clearing stomach intestine moistening, eruptive disease stomachache, acute ascarid obstructive intestinal obstruction etc. can be controlled.
The extraction of Oleum Camelliae has milling process, organic solvent extraction, water substitution and aqueous enzymatic method etc..At present, commercial production is commonly used
Method be mainly milling process, organic solvent extraction.Milling process technique is simple, but press apparatus maintenance changes the amount of labour greatly,
Extraction efficiency is relatively low；Organic solvent extraction efficiency is the highest, and production cost is relatively low, but organic reagent exists potential safety and asks
Topic；It is simple that water substitution produces equipment, processing ease, and cost is relatively low, but its oil yield is low, and the acid value of lipids proposed is high, uses water
Measure bigger；And in aqueous enzymatic method, high active enzyme difficulty obtains, remain in and Oleum Camelliae easily causes content of microorganisms exceed standard.
Document " technique that water substitution extracts Oleum Camelliae from Semen Camelliae " (Transactions of the Chinese Society of Agricultural Engineering, the 9th phase of volume 24,2008 years 9
Month, Guo Yubao etc.) disclose a kind of method that water substitution extracts Oleum Camelliae from tea seed, optimum condition is, dries with decortication
Camellia oleosa seed is raw material, is 75 DEG C in temperature, and extraction time is 150min, and ratio of water to material is 4.5:1 (mL/g) and the condition of pH value 9.0
Lower extraction, Oleum Camelliae extraction rate is up to 80.28%.Extraction ratio is higher than general water substitution, but tea certain in residual in Oleum Camelliae
Saponin, remains more Oleum Camelliae in the screenings obtained, comprehensive utilization ratio is the highest.
Summary of the invention
It is an object of the invention to provide a kind of water substitution Oleum Camelliae method for producing, the traditional Oleum Camelliae production technology of transformation, excellent
Change water substitution Oleum Camelliae technique, improve the purity of Oleum Camelliae, improve the comprehensive utilization ratio of raw material, reduce cost, shorten the production cycle.
The present invention is achieved by the following technical programs:
A kind of water substitution Oleum Camelliae method for producing, comprises the following steps:
1) get the raw materials ready
Choose the camellia oleosa seed dried, shelling, pulverize stand-by；
2) pH and extraction are adjusted
Add water, sodium chloride, adjust pH with glacial acetic acid, mechanical shaking extraction, layering；
3) extraction
Be extracted with ethyl acetate step 2) in water layer and emulsion layer, extract 2-3 time, collect ethyl acetate layer；Water layer and breast
After change layer dries 12h at 55 DEG C, obtain the screenings of drying, weigh, survey residual oil content；
4) purification is with dry
Combining step 2) oil reservoir and step 3) ethyl acetate layer, wash 1-2 time, vacuum drying.
Preferably, step 1) in, pulverizing requirement is: be ground into the camellia oleosa seed powder of 100-130 mesh.
Preferably, step 2) in, pH regulator to 4-4.5.
Preferably, step 3) in, mechanical shaking extraction condition is: temperature 40-50 DEG C, rotating speed 100r/min, and the time is that 2-3 is little
Time.
Preferably, step 3) in, ethyl acetate single extraction consumption is 1-2 times of camellia oleosa seed weight.
Preferably, step 4) in, vacuum drying condition is: temperature 50-60 DEG C, vacuum 0.06-0.08Mpa, time
1.5-3h。
Preferably, step 1)-3) in, camellia oleosa seed, water, the consumption of sodium chloride, according to weight ratio, camellia oleosa seed: water: sodium chloride=1:
4-5:0.2-0.5。
The foundation of the present invention:
1) rational method of cell disruption
The camellia oleosa seed that decortication is dried is ground into the camellia oleosa seed powder of certain mesh number, contributes to the broken of cell wall in camellia oleosa seed
Split；By adding glacial acetic acid, regulation system pH value, change the charge characteristics of protein, increase the permeability of cell wall, reduce born of the same parents
The interaction of interior product, makes Oleum Camelliae easily discharge, and adds certain density sodium chloride solution, makes intraor extracellular form infiltration
Pressure, can accelerate rupturing of cell wall.
2) rational extractive technique
During Oleum Camelliae processing for many years, it has been found that in water-glacial acetic acid system, fatty acid is at pH=4-
When 4.5, dissolubility is relatively big, is suitable for using mechanical shaking extraction to extract Oleum Camelliae.
3) difference of dissolubility is utilized
Tea saponin is soluble in aqueous methanol, aquiferous ethanol, n-butyl alcohol and glacial acetic acid, acetic anhydride and pyridine, adds when extracting
Enter glacial acetic acid, tea saponin can be made more to distribute tea saponin in water layer, oil reservoir and distribute less, and add sodium chloride so that water
Density increase, beneficially extracting and demixing and abolish emulsion layer；In upper strata and emulsion layer, add ethyl acetate extract, can be complete
Entirely extract and do not extract clean Oleum Camelliae, make tea saponin stay in water layer；Finally use water backwash again, glacial acetic acid can be got rid of.
4) computing formula
The invention has the beneficial effects as follows, by the destruction emulsion layer of sodium chloride, in acid condition, at glacial acetic acid-water body
System carries out mechanical shaking extraction, can fully extract the Oleum Camelliae in camellia oleosa seed；By processing water layer and emulsion layer by ethyl acetate,
The residual oil content in screenings can be reduced；By water backwash, remove the tea saponin in Oleum Camelliae；And the organic solvent in Oleum Camelliae, Jing Guozhen
Empty dried, noresidue；Therefore the raising oil extracting rate of energy camellia oleosa seed of the present invention, edible vegetable oil rate, comprehensive utilization ratio is high, without tea saponin in Oleum Camelliae
Residual, organic solvent-free remains, and safety is high；Production technology is simple to operation simultaneously, low cost, is suitable for industrialized production.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is further described, but claimed scope is not limited to
In described.
Embodiment 1
1) get the raw materials ready
Choose the camellia oleosa seed 10Kg drying (moisture Control is below 10%), shelling, camellia oleosa seed is pulverized, crosses 100 purposes
Sieve, obtains camellia oleosa seed powder, stand-by；
2) pH and extraction are adjusted
In an oscillator add step 1) in camellia oleosa seed powder, water 50kg, sodium chloride 2.0Kg, with glacial acetic acid adjust pH extremely
4.0, agitator rotating speed be 100r/min, temperature be 40-50 DEG C under conditions of extract 2 hours, stratification, separate upper strata oil
Layer；
3) extraction
By step 2) in after water layer and emulsion layer separate, be extracted with ethyl acetate, layering, coextraction 2 times, use every time
20Kg, collects ethyl acetate layer；After water layer and emulsion layer dry 12h at 55 DEG C, obtain the screenings of drying, weigh, survey residual oil content；
4) purification is with dry
Combining step 2) oil reservoir and step 3) ethyl acetate layer, to wash 1 time, be 50-60 DEG C in temperature, vacuum is
It is dried 1.5 hours under conditions of 0.06-0.08Mpa, obtains Oleum Camelliae.Embodiment 2
1) get the raw materials ready
Choose the camellia oleosa seed 10Kg drying (moisture Control is below 10%), shelling, camellia oleosa seed is pulverized, crosses 130 purposes
Sieve, obtains camellia oleosa seed powder, stand-by；
2) pH and extraction are adjusted
In an oscillator add step 1) in camellia oleosa seed powder, water 40kg, sodium chloride 3.5Kg, with glacial acetic acid adjust pH extremely
4.5, agitator rotating speed be 100r/min, temperature be 40-50 DEG C under conditions of extract 3 hours, stratification, separate upper strata oil
Layer；
3) extraction
By step 2) in after water layer and emulsion layer separate, be extracted with ethyl acetate, layering, coextraction 3 times, use every time
20Kg, collects ethyl acetate layer；After water layer and emulsion layer dry 12h at 55 DEG C, obtain the screenings of drying, weigh, survey residual oil content；
4) purification is with dry
Combining step 2) oil reservoir and step 3) ethyl acetate layer, to wash 2 times, be 50-60 DEG C in temperature, vacuum is
It is dried 3 hours under conditions of 0.06-0.08Mpa, obtains Oleum Camelliae.
Embodiment 3
1) get the raw materials ready
Choose the camellia oleosa seed 10Kg drying (moisture Control is below 10%), shelling, camellia oleosa seed is pulverized, crosses 120 purposes
Sieve, obtains camellia oleosa seed powder, stand-by；
2) pH and extraction are adjusted
In an oscillator add step 1) in camellia oleosa seed powder, water 45kg, sodium chloride 6Kg, with glacial acetic acid adjust pH to 4.3,
Agitator rotating speed be 100r/min, temperature be 40-50 DEG C under conditions of extract 2.5 hours, stratification, separate upper strata oil
Layer；
3) extraction
By step 2) in after water layer and emulsion layer separate, be extracted with ethyl acetate, layering, coextraction 2 times, use every time
20Kg, collects ethyl acetate layer；After water layer and emulsion layer dry 12h at 55 DEG C, obtain the screenings of drying, weigh, survey residual oil content；
4) purification is with dry
Combining step 2) oil reservoir and step 3) ethyl acetate layer, to wash 1 time, be 50-60 DEG C in temperature, vacuum is
It is dried 2.5 hours under conditions of 0.06-0.08Mpa, obtains Oleum Camelliae.
Contrast test 1: employing document " technique that water substitution extracts Oleum Camelliae from Semen Camelliae " (Transactions of the Chinese Society of Agricultural Engineering, the 24th
Rolled up for the 9th phase, in JIUYUE, 2008, Guo Yubao etc.) in optimum test method carry out the processing of Oleum Camelliae, embodiment and contrast
Test 1 gained Oleum Camelliae, carry out detection and analyze, testing result and yield situation, as shown in the table:
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Documents |
| Transparency | Clear | Clear | Clear | Clear |
| Solvent residual amount (ppm) | Do not detect | Do not detect | Do not detect | Do not detect |
| Tea saponin (%) | Do not detect | Do not detect | Do not detect | 1.07 |
| Oleum Camelliae extraction rate | 89.25% | 88.13% | 87.50% | 80.28% |
| Clear oil-collecting ratio | 94.20% | 93.16% | 92.86% | 90.19% |
Claims (6)
1. a water substitution Oleum Camelliae method for producing, it is characterised in that: described production method, comprise the following steps:
1) get the raw materials ready
Choose the camellia oleosa seed dried, shelling, pulverize stand-by；
2) pH and extraction are adjusted
Add water, sodium chloride, adjust pH with glacial acetic acid, mechanical shaking extraction, layering；
3) extraction
Be extracted with ethyl acetate step 2) in water layer and emulsion layer, extract 2-3 time collect ethyl acetate layer；Water layer and emulsion layer exist
After drying 12h at 55 DEG C, obtain the screenings of drying, weigh, survey residual oil content；
4) purification is with dry
Combining step 2) oil reservoir and step 3) ethyl acetate layer, wash 1-2 time, vacuum drying.
A kind of water substitution Oleum Camelliae method for producing, it is characterised in that: described step 2) in, pH
Regulate to 4-4.5.
A kind of water substitution Oleum Camelliae method for producing, it is characterised in that: described step 2) in, shake
Swinging extraction conditions is: temperature 40-50 DEG C, and rotating speed is 100r/min, and the time is 2-3 hour.
A kind of water substitution Oleum Camelliae method for producing, it is characterised in that: described step 3) in, second
Acetoacetic ester single extraction consumption is 1-2 times of camellia oleosa seed weight.
A kind of water substitution Oleum Camelliae method for producing, it is characterised in that: described step 4) in, very
Empty dry condition is: temperature 50-60 DEG C, vacuum 0.06-0.08Mpa, time 1.5-3h.
A kind of water substitution Oleum Camelliae method for producing, it is characterised in that: described step 1)-3) in,
Camellia oleosa seed, water, the consumption of sodium chloride, according to weight ratio, camellia oleosa seed: water: sodium chloride=1:4-5:0.2-0.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610686012.3A CN106244313A (en) | 2016-08-18 | 2016-08-18 | A kind of water substitution Oleum Camelliae method for producing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610686012.3A CN106244313A (en) | 2016-08-18 | 2016-08-18 | A kind of water substitution Oleum Camelliae method for producing |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106244313A true CN106244313A (en) | 2016-12-21 |
Family
ID=57591860
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610686012.3A Pending CN106244313A (en) | 2016-08-18 | 2016-08-18 | A kind of water substitution Oleum Camelliae method for producing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106244313A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109923196A (en) * | 2017-03-08 | 2019-06-21 | 快速工业与商业公司 | By the palm-kernel oil extraction system of hydrodynamic processes |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034758A (en) * | 1987-10-29 | 1989-08-16 | 福州市抗菌素厂 | Emulsion-breaking process by extracting with antibiotic dissolved medium |
| CN1196384A (en) * | 1998-05-19 | 1998-10-21 | 张咪 | High production method for producing oil with water extraction process |
| CN102250678A (en) * | 2011-05-23 | 2011-11-23 | 井冈山茶油有限公司 | Method for extracting camellia oil by using microwave assisted aqueous extraction method |
| CN102585992A (en) * | 2012-01-16 | 2012-07-18 | 浙江师范大学 | Method for extracting tea oil from tea oilseeds by water substitution |
| CN103205310A (en) * | 2013-05-08 | 2013-07-17 | 长沙理工大学 | Method for sequentially extracting tea saponin and tea seed oil from oil-tea camellia seeds |
| CN103396879A (en) * | 2013-08-12 | 2013-11-20 | 长沙昊瑞生物科技有限公司 | Demulsification method in production processes for extracting tea-seed oil extraction with participation of water phase |
| CN105331437A (en) * | 2015-11-25 | 2016-02-17 | 华南理工大学 | Low-viscosity tea-seed oil, preparation method thereof and application thereof |
| CN105670788A (en) * | 2016-01-13 | 2016-06-15 | 北京中浩丹食品股份有限公司 | Method for preparing traditional ground sesame seed oil by high-yield high-quality water extraction process |
-
2016
- 2016-08-18 CN CN201610686012.3A patent/CN106244313A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034758A (en) * | 1987-10-29 | 1989-08-16 | 福州市抗菌素厂 | Emulsion-breaking process by extracting with antibiotic dissolved medium |
| CN1196384A (en) * | 1998-05-19 | 1998-10-21 | 张咪 | High production method for producing oil with water extraction process |
| CN102250678A (en) * | 2011-05-23 | 2011-11-23 | 井冈山茶油有限公司 | Method for extracting camellia oil by using microwave assisted aqueous extraction method |
| CN102585992A (en) * | 2012-01-16 | 2012-07-18 | 浙江师范大学 | Method for extracting tea oil from tea oilseeds by water substitution |
| CN103205310A (en) * | 2013-05-08 | 2013-07-17 | 长沙理工大学 | Method for sequentially extracting tea saponin and tea seed oil from oil-tea camellia seeds |
| CN103396879A (en) * | 2013-08-12 | 2013-11-20 | 长沙昊瑞生物科技有限公司 | Demulsification method in production processes for extracting tea-seed oil extraction with participation of water phase |
| CN105331437A (en) * | 2015-11-25 | 2016-02-17 | 华南理工大学 | Low-viscosity tea-seed oil, preparation method thereof and application thereof |
| CN105670788A (en) * | 2016-01-13 | 2016-06-15 | 北京中浩丹食品股份有限公司 | Method for preparing traditional ground sesame seed oil by high-yield high-quality water extraction process |
Non-Patent Citations (3)
| Title |
|---|
| 李武客等主编: "《基础化学实验教程（第二版）》", 31 August 2014, 华中师范大学出版社 * |
| 罗明生等主编: "《药剂辅料大全（第2版）》", 31 January 2006, 四川科学技术出版社 * |
| 詹益兴主编: "《现代化工小商品制法大全 第3集》", 31 August 1999, 湖南大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109923196A (en) * | 2017-03-08 | 2019-06-21 | 快速工业与商业公司 | By the palm-kernel oil extraction system of hydrodynamic processes |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103113483B (en) | Method for extracting various active ingredients from dendrobium officinale | |
| CN101085958B (en) | Tartary buckwheat oxidation resistance health care wine | |
| CN101928639A (en) | Natural tea essence prepared by using tea and preparation method thereof | |
| CN105963328B (en) | A method of continuously extracting Chinese torreya flavones and essential oil from Chinese torreya aril | |
| CN103980242B (en) | The method of Moringa flavones is extracted from leaf of Moringa | |
| CN101239995B (en) | Method for preparing flax lignins | |
| CN104710391A (en) | Method for extracting luteolin and beta-sitosterol from peanut shells | |
| CN103333768B (en) | Black fungus-radix puerariae fruit wine and preparation method thereof | |
| CN102388987B (en) | Ultrasound-assisted tea oil extraction method | |
| CN104688801A (en) | Production technology for extracting eucommia flavonoid from eucommia ulmoides leaves by combining compound enzyme with ultrasound | |
| CN104593441A (en) | Method for simultaneously extracting volatile oil, polysaccharides and amino acids from tricholoma matsutake | |
| CN102942637B (en) | Method for increasing extraction rate of wide cactus polysaccharide | |
| CN107118253A (en) | The preparation method of Tea Saponin | |
| CN103356740B (en) | Preparation method of baicalein and scutellaria baicalensis flavone total-aglycone extractives | |
| CN104982597B (en) | A kind of multi-functional composite instant tea and its preparation method and application | |
| CN106244313A (en) | A kind of water substitution Oleum Camelliae method for producing | |
| CN102206538B (en) | Method for extracting grease and flavone from soy sauce residues | |
| CN106190524A (en) | A kind of production method of aqueous enzymatic extraction Oleum Camelliae | |
| CN104726197A (en) | Method for extracting tobacco seed oil from aromatic tobacco waste tobacco seed | |
| CN109364110B (en) | Method for extracting flavone from embelia nasuta shell and application thereof | |
| CN104666383B (en) | A kind of technique of microwave radiation exaraction Dysosma versipellis flavone compound | |
| CN105153320B (en) | The extracting method of one Polysaccharides From Laminaria Japonica | |
| CN102241656A (en) | Preparation method of tricin | |
| CN104074086A (en) | Method for extracting cellulose from sow thistle | |
| CN103908513A (en) | Method for extracting total saponins of xanthoceras sorbifolia shell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161221 |
|
| RJ01 | Rejection of invention patent application after publication |