AU2021105814A4 - Application of Microwave/Subcritical Combined Key Technology for High-Efficiency Low-Temperature Extraction of Cyperus Esculentus Oil - Google Patents
Application of Microwave/Subcritical Combined Key Technology for High-Efficiency Low-Temperature Extraction of Cyperus Esculentus Oil Download PDFInfo
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- AU2021105814A4 AU2021105814A4 AU2021105814A AU2021105814A AU2021105814A4 AU 2021105814 A4 AU2021105814 A4 AU 2021105814A4 AU 2021105814 A AU2021105814 A AU 2021105814A AU 2021105814 A AU2021105814 A AU 2021105814A AU 2021105814 A4 AU2021105814 A4 AU 2021105814A4
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- cyperus esculentus
- extraction
- oil
- microwave
- minutes
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- 238000000605 extraction Methods 0.000 title claims abstract description 52
- 235000005853 Cyperus esculentus Nutrition 0.000 title claims abstract description 40
- 238000005516 engineering process Methods 0.000 title description 6
- 241000103725 Cyperus esculentus var. esculentus Species 0.000 title 1
- 244000285774 Cyperus esculentus Species 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000005096 rolling process Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 210000001161 mammalian embryo Anatomy 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 46
- 238000000926 separation method Methods 0.000 claims description 23
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical group CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 5
- 238000004807 desolvation Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 2
- 238000005336 cracking Methods 0.000 claims 1
- 239000010779 crude oil Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000000053 physical method Methods 0.000 abstract description 2
- 239000002932 luster Substances 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 235000019198 oils Nutrition 0.000 description 43
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 6
- 235000016709 nutrition Nutrition 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 3
- 241000234653 Cyperus Species 0.000 description 3
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- 239000005642 Oleic acid Substances 0.000 description 3
- 235000021314 Palmitic acid Nutrition 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 3
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- 235000020778 linoleic acid Nutrition 0.000 description 3
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 3
- 229960004488 linolenic acid Drugs 0.000 description 3
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 3
- 230000035764 nutrition Effects 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 3
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 3
- 235000015112 vegetable and seed oil Nutrition 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000008157 edible vegetable oil Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000008158 vegetable oil Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241000234646 Cyperaceae Species 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 240000000950 Hippophae rhamnoides Species 0.000 description 1
- 235000003145 Hippophae rhamnoides Nutrition 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 241000219925 Oenothera Species 0.000 description 1
- 235000004496 Oenothera biennis Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000003283 Pachira macrocarpa Nutrition 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 240000001890 Ribes hudsonianum Species 0.000 description 1
- 235000016954 Ribes hudsonianum Nutrition 0.000 description 1
- 235000001466 Ribes nigrum Nutrition 0.000 description 1
- 240000001085 Trapa natans Species 0.000 description 1
- 235000014364 Trapa natans Nutrition 0.000 description 1
- 229930003270 Vitamin B Natural products 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 235000001497 healthy food Nutrition 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 235000009165 saligot Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 235000019156 vitamin B Nutrition 0.000 description 1
- 239000011720 vitamin B Substances 0.000 description 1
- 239000010497 wheat germ oil Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention specifically relates to a technical method for subcritical extraction of Cyperus
esculentus oil. The extraction process includes the following contents: taking Cyperus
esculentus with uniform, full and mature color as raw materials, drying, and microwave
pretreatment; Peeling, crushing and rolling embryo by physical method; Packaging and sealing
the processed Cyperus esculentus powder cake, and placing it into an extraction tank. The
extraction is carried out under the set conditions. The obtained Cyperus esculentus oil is
transparent and uniform, has bright yellow luster and smell unique to Cyperus esculentus, and
has high purity and good quality. The preparation method of the invention has the advantages
of simple process, convenient operation, accurate and reliable process condition parameters,
economy, environmental protection and high efficiency, and is easy to realize industrial
expanded production. The content of the invention is of great significance for preparing
Cyperus esculentus oil with high efficiency and high quality and realizing the industrialized
production of new resource of functional oil.
Description
Application of Microwave/Subcritical Combined Key Technology for High
Efficiency Low-Temperature Extraction of Cyperus Esculentus Oil
The invention belongs to the technical field of extraction and processing of vegetable oil,
and particularly relates to a subcritical extraction method of Cyperus esculentus oil.
According to the invention, a GC-MS analysis method is adopted to analyze the
unsaturated fatty acid composition of the sub-critical extracted Cyperus esculentus oil,
and the optimal extraction process conditions of Cyperus esculentus oil are determined to
accord to the composition ratio of the unsaturated fatty acid and the oil yield.
Cyperus esculentus L. var. Sativus Baeck, also known as Cyperus esculentus, Tiger Nut,
Iron Water Chestnut and Sea Chestnut, they are representative variety of Cyperaceae. It is
widely cultivated in parts of Africa, Asia and parts of Europe.
As a kind of functional, nutritional, multi-purpose and beneficial natural varieties in the
new oil crop family with the most development prospect in recent years, Cyperus
esculentus is rich in protein, polyunsaturated fatty acids and trace elements (kalium,
calcium, magnesium, zinc, vitamin B, E, etc.). The oil content of Cyperus esculentus is as
high as 38%, and the content of unsaturated fatty acid is as high as 73%. It is of great
strategic significance to study and develop Cyperus esculentus oil as characteristic oil to
ensure the development of characteristic oil industry and meet the market demand, which
is in line with the development trend of high quality, specialization and nutrition of oil
industry, and caters to consumers' demand for higher food safety and healthy food. This
kind of oil resource has the characteristics of high quality, high yield, comprehensive utilization value and high economic value, and has huge market development space at home and abroad.
The subcritical technology for oil production is a process of extracting with subcritical
fluid (n-butane, propane and other solvents) at low temperature, which can ensure the
higher oil production rate, keep the effective components of the oil sample unchanged
and ensure the quality of oil products. In addition, the used solvents can be recycled. At
present, subcritical technology is widely used in oil preparation because of its advantages
of safety, high efficiency, energy saving, environmental protection, and effective
protection of oil quality. It has been applied to oil production from peanut oil, soybean
oil, rapeseed oil and other bulk oil crops in industry, and achieved considerable economic
benefits. There are also studies on the preparation of special vegetable oils such as rice,
wheat germ oil, blackcurrant, evening primrose seed oil and sea buckthorn oil. However,
the research and application of the subcritical preparation technology of Cyperus
esculentus are still few.
With the development of society, people's understanding of nutrition and health is
gradually deepened, and they are increasingly the nutrition and health function of food.
At the same time, seeking and developing new edible oil resources can not only relieve
the pressure of global oil demand, but also meet the needs of different groups of people
for functional nutritional oils. Therefore, the invention aims to improve oil production
efficiency, develop new edible oil, meet the needs of global economic development, and
meet the needs of customers.
The purpose of the present invention aims to provide extraction method for preparing
Cyperus esculentus oil by combining microwave with subcritical technology.
The microwave/subcritical combined method for efficiently extracting Cyperus
esculentus oil comprises the following extraction processes:
(1) Selecting Cyperus esculentus with uniform color, full particles and maturity as raw
material, treating with conventional drying method, pretreating at 70 °C with microwave
for 15 minutes, 420 W, peeling, crushing and rolling embryo by pure physical method;
(2) Subcritical extraction: bag and seal the crushed Cyperus esculentus powder, and put it
into extraction tank. The extraction was carried out under the conditions of extractant n
butane, extraction tank temperature 405 °C and extraction pressure 0.41 Mpa, and the
extraction times were 4 times, 40 min each time, and the mixed oil samples were put into
the separation tank in turn.;
C) Desolvation: put the mixture of Cyperus esculentus oil and n-butane into the
separation tank, desolventize for 30 minutes with compressor, followed by 30 minutes
with the combination of vacuum pump and compressor. Then, open the valve at the
bottom of the separation tank to collect the crude Cyperus esculentus oil.
Fig. 1 is a diagram of peeled Cyperus esculentus
Fig. 2 is a diagram of Cyperus esculentus oil
The present invention will be described in detail by examples. In addition, the technical
scheme of the present invention is not limited to the following listed embodiments. Some changes and adjustments made by those skilled in the art within the scope of the claims are also within the scope of the present invention.
Example 1: 4.3 kg of crushed and milled Cyperus esculentus powder was weighed,
bagged and sealed, and then placed in the extraction tank. Evacuate the extraction tank to
-0.08 MPa, open the inlet channel until the solvent reaches 2/3 of the extraction tank (raw
materials can be immersed); Adjust the extraction temperature upto 40±5°C through hot
water valve, extraction pressure at 0.41 MPa, and extract for 40 minutes. After extraction
is completed, open the connection valve between the extraction tank and separation tank,
and release the mixed oil sample into the separation tank; Close the connection valve,
open the desolventizing channel of the separation tank and desolventize for 30 minutes
with compressor, followed by 30 minutes with the combination of vacume pump and
compressor; Close the desolventizing channel, open the vent valve of the separation tank
to break the vacuum inside the separation tank, and then open the valve at the bottom of
the separation tank to discharge the Cyperus esculentus oil when the operation is
completed. Repeat the extraction steps for three more times to realize the high-efficiency
extraction of Cyperus esculentus oil.
Product performance indicators: 902.5 g of oil was obtained with the yield of 20.98%,
palmitic acid 14.00%, stearic acid 3.30%, oleic acid 72.00%, linoleic acid 9.6% and
linolenic acid 0.4%. This product is yellow and transparent, with few impurities, good
quality and high purity, and has a unique flavor of Cyperus esculentus.
Example 2: 4.3 kg of crushed and milled Cyperus esculentus powder was weighed,
bagged and sealed, and then placed in the extraction tank. Evacuate the extraction tank to
-0.08 MPa, open the inlet channel until the solvent reaches 2/3 of the extraction tank (raw materials can be immersed); Adjust the extraction temperature upto 40±5°C through hot water valve ,extraction pressure to 0.41 MP, and extract for 40 minutes. After extraction is completed, open the connecion valve between the extraction tank and the separation tank, and release the mixed oil sample into the separation tank; Close the connection valve, open the desolventizing channel of the separation tank and desolventizing for 30 minutes with compressor, followed by 30 minutes with the combination of vacume pump and compressor; Close the desolventizing channel, open the vent valve of the separation tank to break the vacuum inside the separation tank, and then open the valve at the bottom of the separation tank to discharge the Cyperus esculentus oil when the operation is completed. Repeat the extraction steps for three more times to realize the high efficiency extraction of Cyperus esculentus oil.
Product performance indicators: 905.0 g of oil was obtained with the yield is 21.05%,
palmitic acid 13.70%, stearic acid 3.30%, oleic acid 71.10%, linoleic acid 10.40% and
linolenic acid 0.30%. This product is yellow and transparent, with few impurities, good
quality and high purity, and has a unique flavor of Cyperus esculentus.
Example 3: 4.3 kg of crushed and milled Cyperus esculentus powder was weighed,
bagged and sealed, and then placed in the extraction tank. Evacuate the extraction tank to
-0.08 MPa, open the inlet channel until the solvent reaches 2/3 of the extraction tank (raw
materials can be immersed); Adjust the extraction temperature upto 40±5C through hot
water valve ,extraction pressure to 0.41 MP, and extract for 40 minutes. After extraction
is completed, open the connecion valve between the extraction tank and the separation
tank, and release the mixed oil sample into the separation tank; Close the connection valve, open the desolventizing channel of the separation tank and desolventizing for 30 minutes with compressor, followed by 30 minutes with the combination of vacume pump and compressor; Close the desolventizing channel, open the vent valve of the separation tank to break the vacuum inside the separation tank, and then open the valve at the bottom of the separation tank to discharge the Cyperus esculentus oil when the operation is completed. Repeat the extraction steps for three more times to realize the high efficiency extraction of Cyperus esculentus oil.
Product performance indicators: 903.4g of oil was obtained with the yield is 21.01%,
palmitic acid 14.20%, stearic acid 3.20%, oleic acid 69.8%, linoleic acid 10.90% and
linolenic acid is 0.40%. This product is yellow and transparent, with few impurities, good
quality and high purity, and has a unique flavor of Cyperus esculentus.
Claims (5)
1. A subcritical extraction method of Cyperus esculentus oil, which is characterized by
comprising the following steps:
A) Pretreatment of raw materials: Cyperus esculentus with uniform color, full particles
and maturity is selected as the raw material, and after being treated by conventional
drying method, microwave pretreatment, peeling, crushing and embryo rolling are
performed.
B) Subcritical extraction: bag the crushed Cyperus esculentus powder, seal and put into
the extraction tank. The extractant is n-butane, the temperature of extraction tank is
+5°C and the extraction pressure is 0.41 MPa;
C) Desolvation: put the oil mixture of Cyperus esculentus oil and n-butane into the
separation tank from the extraction tank, and perform desolvation with compressor and
then with vacuum pump-compressor. After desolventizing, open the valve at the bottom
of the separation tank and discharge the Cyperus esculentus crude oil.
2. The method according to claim 1, characterized in step a) is 40 meshes, and the
judgment standard of the rolling degree is the cracking of Cyperus esculentus.
3. The method according to claim 1, characterized in step a) is performed at microwave
temperature of 70°C, microwave time of 15 minutes and microwave power of 420 W.
4. The method according to claim 1, characterized in step b) is that the extraction times is
4 and the time for each extraction is 40 minutes.
5. The method according to claim 1, characterized in step c) is that the desolvation time is
minutes with compressor, and then 30 minutes with the combination of vacuum pump
and compressor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2021105814A AU2021105814A4 (en) | 2021-08-18 | 2021-08-18 | Application of Microwave/Subcritical Combined Key Technology for High-Efficiency Low-Temperature Extraction of Cyperus Esculentus Oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU2021105814A AU2021105814A4 (en) | 2021-08-18 | 2021-08-18 | Application of Microwave/Subcritical Combined Key Technology for High-Efficiency Low-Temperature Extraction of Cyperus Esculentus Oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| AU2021105814A4 true AU2021105814A4 (en) | 2021-10-21 |
Family
ID=78176966
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AU2021105814A Ceased AU2021105814A4 (en) | 2021-08-18 | 2021-08-18 | Application of Microwave/Subcritical Combined Key Technology for High-Efficiency Low-Temperature Extraction of Cyperus Esculentus Oil |
Country Status (1)
| Country | Link |
|---|---|
| AU (1) | AU2021105814A4 (en) |
-
2021
- 2021-08-18 AU AU2021105814A patent/AU2021105814A4/en not_active Ceased
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| FGI | Letters patent sealed or granted (innovation patent) | ||
| DA3 | Amendments made section 104 |
Free format text: THE NATURE OF THE AMENDMENT IS: AMEND THE NAME OF THE INVENTOR TO READ CAI, XIAOSHUANG; MIAO, WENBO; LIU, HUAMIN; WANG, XUEDE; QI, KUN; ZHU, XINLIANG; SUN, XIANHONG; HU, PENG; ZHANG, JINGRU; WU, HONGFEI AND FU, CHAOQIANG |
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| MK22 | Patent ceased section 143a(d), or expired - non payment of renewal fee or expiry |