CN103467245A - Method for complexing and removing water contained in ethanol and water mixed solution by utilizing eutectic solvent - Google Patents
Method for complexing and removing water contained in ethanol and water mixed solution by utilizing eutectic solvent Download PDFInfo
- Publication number
- CN103467245A CN103467245A CN2013104366084A CN201310436608A CN103467245A CN 103467245 A CN103467245 A CN 103467245A CN 2013104366084 A CN2013104366084 A CN 2013104366084A CN 201310436608 A CN201310436608 A CN 201310436608A CN 103467245 A CN103467245 A CN 103467245A
- Authority
- CN
- China
- Prior art keywords
- complexing
- eutectic solvent
- mixed solution
- water mixed
- ethanol water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention belongs to the technical field of chemical engineering, and particularly relates to a method for complexing and removing water contained in an ethanol and water mixed solution by utilizing an eutectic solvent. The method is used for preparing anhydrous ethanol. The method disclosed by the invention can be used for complexing the water contained in the ethanol and water mixed solution by utilizing the eutectic solvent and then removing the water contained in the ethanol and water mixed solution through distillation, is especially suitable for preparing the anhydrous ethanol by removing the water contained in the 95% ethanol and water mixed solution and prevents the high energy consumption of an extractive distillation method and an azeotropic distillation method. According to the invention, the eutectic solvent which plays a complexing agent role can be recycled after being removed in water through evaporation. The method disclosed by the invention has the advantages of easiness for process operation, low cost, no wastewater discharge, mildness in complexing condition, operation at low temperature and normal pressure and high production safety and is suitable for small-scale device production and also suitable for large-scale device production.
Description
Technical field
The present invention relates to a kind of method of utilizing the eutectic solvent complexing to remove moisture in the ethanol water mixed solution.
Background technology
Dehydrated alcohol is a kind of important industrial chemicals.Be widely used in the industries such as medicine, agricultural chemicals, paint, food, makeup, rubber, electronic industry.In addition, add properties-correcting agent in dehydrated alcohol and can form denatured fuel ethanol.Denatured fuel ethanol is in harmonious proportion with certain proportion and gasoline, forms vehicle-use alcohol gasoline, can be used as the environment-friendly fuel of automobile.In recent years, along with the Continued of energy prices, save the behave of petroleum resources and listed the national science and technology Outline Development Plan in.Automobile-used dehydrated alcohol project is actively promoted in some provinces.
The purity that ethanol can reach is the important quality index of dehydrated alcohol.Most commercially available dehydrated alcohols generally can only reach 99.5% purity, need the dehydrated alcohol higher by purity in many organic synthesis, often need oneself preparation.Usually industrial 95.5% ethanol can not directly be produced dehydrated alcohol by distillation method, because of the water formation constant boiling mixture of 95.5% ethanol and 4.5%.Remove water, the general the first step is to add calcium oxide (unslaked lime) boiling reflux, makes water and unslaked lime effect in ethanol generate calcium hydroxide, and then dehydrated alcohol is steamed.Obtain like this dehydrated alcohol, purity is the highest by approximately 99.5%.At present, the production method of dehydrated alcohol also has azeotropic distillation, extraction fractional distillation, molecular sieve adsorbing and dewatering method, calcium oxide evaporation, pervaporation method, vacuum dehydration method and biomass absorbent method etc.Wherein all exist certain deficiency, as high as energy consumption.And the higher dehydrated alcohol of purity will be processed with MAGNESIUM METAL or sodium Metal 99.5.Thereby, from Energy Angle, exploitation energy consumption dehydrated alcohol lower, that product purity is higher is significant.
Summary of the invention
The present invention is the technical problems such as the higher and product purity of moisture energy consumption used in the ethanol water mixed solution is lower that remove that overcome that the prior art extraction fractional distillation exists, and a kind of method of utilizing the eutectic solvent complexing to remove moisture in the ethanol water mixed solution is provided.
The moisture that the technology of the present invention is applicable to remove in 95% ethanol water mixed solution is produced dehydrated alcohol, avoided the high energy consumption of extraction fractional distillation and azeotropic distillation, the eutectic solvent that plays the complexing agent effect can be recycled after moisture is removed in evaporation, novel process has significantly reduced production cost, and product quality indicator can reach the requirement of dehydrated alcohol high-quality product.
The present invention is achieved by the following technical solutions:
A kind of method of utilizing the eutectic solvent complexing to remove moisture in the ethanol water mixed solution, it comprises the following steps:
A. ethanol content is less than or equal to 95% ethanol water mixed solution and sends into the complexing still kettle, the eutectic solvent that can form complex compound with water in proportion afterwards joins the complexing still kettle under agitation condition, complexing still kettle temperature is 20 ℃～40 ℃, pressure is 0.1～0.2MPa, and in described eutectic solvent and described ethanol water mixed solution, the mass ratio of moisture is 15～20:1;
Described eutectic solvent is the eutectic solvent that quaternary ammonium salt and hydrogen bond donor form, described quaternary ammonium salt is a kind of in Dodecyl trimethyl ammonium chloride, choline chloride 60, beet alkali hydrochlorate, palmityl trimethyl ammonium chloride, tri-n-octyl methyl ammonium chloride, chitosan quaternary ammonium salt and tetrabutylammonium chloride or it is composite, and described hydrogen bond donor is a kind of in urea, glycerine, ethylene glycol, formic acid, acetic acid and methane amide or it is composite;
B. in described step a, the complex liquid that moisture in described ethanol water mixed solution and eutectic solvent form is after distillation finishes, be driven into the complex liquid storage tank, be sent to afterwards follow-up decompression dehydration operation and remove the moisture in complex liquid in evaporating kettle, obtain the eutectic solvent of regeneration for complexing next time.
The above-mentioned eutectic solvent complexing that utilizes removes the method for moisture in the ethanol water mixed solution, and it is further comprising the steps of:
C squeezes into evaporating kettle by the complex liquid in complex liquid storage tank in step b with pump, before entering evaporating kettle, heater via heats, in temperature, be to remove moisture under 70 ℃～90 ℃, the vacuum tightness condition that is 0.5MPa～0.8MPa, the moisture that flow out on evaporating kettle still top enters the complex liquid of evaporating kettle for preheating;
D. the dewatered eutectic solvent stayed in evaporating kettle being sent to the complexing still kettle recycles.
Preferably, in described steps d, Heating temperature is 75 ℃～85 ℃, and the best is 80 ℃.
Preferably, the service temperature in the complexing still kettle of described step a is 30 ℃, pressure 0.1MPa.
Preferably, in described ethanol water mixed solution, the water-content scope is 85%～95%.
The unusual effect that the present invention compared with prior art has is:
1. the present invention utilizes the method for eutectic solvent complexing to remove the moisture in the ethanol water mixed solution, the ethanol water mixed solution contacts with the eutectic solvent added from complexing still kettle top, the complexing of moisture in realization and ethanol water mixed solution, adopt afterwards the method for simple distillation dehydrated alcohol can be separated, purity of alcohol reaches 99.5%～99.9%, and add-on, complexing condition and the distillation condition of adjusting eutectic solvent can be controlled the specification of product dehydrated alcohol.Technological operation of the present invention is simple, cost is low, and non-wastewater discharge both had been applicable to small-scale device and also has been applicable to large-scale device production.Complexing mild condition of the present invention, the low-temperature atmosphere-pressure operation, production security is high.
2. the present invention utilizes eutectic solvent high as the complexing agent dewatering efficiency, and in complexing kettle, mixed once gets final product the almost whole moisture in complexing ethanol water mixed solution, and in product, water-content is extremely low.
3. the present invention's, preparation low as the eutectic solvent cost of complexing agent easily and can be recycled, belongs to biodegradable environmentally friendly machine.
4. the process characteristic that the complexing that the present invention adopts and distillation combine is that Complexation Efficiency is high, and dehydration thoroughly.Simultaneously, eutectic solvent also has removal effect to a small amount of metallic impurity in the ethanol water mixed solution, has significantly alleviated energy expenditure and production cost, obtains high-quality dehydrated alcohol.
In a word, the present invention adopts eutectic solvent, and a kind of ionic liquid analogue, produce dehydrated alcohol as complexing agent in conjunction with simple distillation.With existing extraction fractional distillation, compare, energy consumption further descends.Thinking of the present invention is to give full play to the good characteristic of eutectic solvent moisture absorption, removes the moisture in the ethanol water mixed solution.Through exploratory development, we find the eutectic solvent method can with the ethanol water mixed solution in moisture complexing well, adopt afterwards the method for distillation dehydrated alcohol can be separated, purity of alcohol reaches 99.5%～99.9%.After dehydration by evaporation, eutectic solvent can be recycled.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
95% commercially available ethanol water mixed solution is joined in complexing still kettle 1, add eutectic solvent, continue to stir 1 hour.Standing 20 minutes.In the complexing still kettle, the complexing phase temperature is 25 ℃, and the complexing staged pressure is 0.1MPa, and in described eutectic solvent and described ethanol water mixed solution, the mass ratio of moisture is 16.5:1; Eutectic solvent used is made from choline chloride 60 and urea, and choline chloride 60 and weight of urea are than being 1:2.3 cubic metres of described complexing still kettle volumes, aspect ratio is 2:1.
In the complexing still kettle, the distillation phase temperature is 80 ℃, the distillation staged pressure is 0.1MPa, the complex liquid that moisture after distillation finishes in the ethanol water mixed solution and eutectic solvent form is driven into evaporating kettle with pump, under the vacuum tightness of 80 ℃ and 0.7MPa, decompression dehydration obtains the eutectic solvent of regeneration, recycles.
The dehydrated alcohol yield that complexing still kettle still top steams reaches 97% of theoretical amount, after testing, ethanol mass fraction in the product that distillation obtains > 99.6%, the mass fraction of water is less than 0.4%, and evaporation residue is less than 0.001%, reaches the standard of dehydrated alcohol.
Embodiment 2
95% commercially available ethanol water mixed solution is joined in the complexing still kettle, add eutectic solvent, continue to stir 2 hours.Standing 10 minutes.In the complexing still kettle, the complexing phase temperature is 35 ℃, and the complexing staged pressure is 0.1MPa, and in described eutectic solvent and described ethanol water mixed solution, the mass ratio of moisture is 25:1; Described eutectic solvent is that choline chloride 60 and glycerol mixture form, and its weight ratio is 1:3.3 cubic metres of described complexing still kettle volumes, aspect ratio is 2:1.
The distillation phase temperature is 80 ℃, the distillation staged pressure is 0.1MPa, moisture after distillation finishes in the ethanol water mixed solution is driven into evaporating kettle with the complex liquid that eutectic solvent forms with pump, and under the vacuum tightness of 80 ℃ and 0.7MPa, decompression dehydration obtains the eutectic solvent of regenerating, and recycles.
The dehydrated alcohol yield that complexing still kettle still top steams reaches 98% of theoretical amount, after testing, ethanol mass fraction in the product that distillation obtains > 99.8%, the mass fraction of water is less than 0.2%, and evaporation residue is less than 0.001%, reaches the standard of dehydrated alcohol.
Embodiment 3
95% commercially available ethanol water mixed solution is joined in the complexing still kettle, add eutectic solvent, continue to stir 0.5 hour.Standing 15 minutes.In the complexing still kettle, the complexing phase temperature is 40 ℃, and the complexing staged pressure is 0.1MPa, and in described eutectic solvent and described ethanol water mixed solution, the mass ratio of moisture is 20:1; Described eutectic solvent is that choline chloride 60 and urea admixture form, and its weight ratio is 1:2.3 cubic metres of described complexing still kettle volumes, aspect ratio is 2:1.
The distillation phase temperature is 80 ℃, the distillation staged pressure is 0.1MPa, moisture after distillation finishes in the ethanol water mixed solution is driven into evaporating kettle with the complex liquid that eutectic solvent forms with pump, and under the vacuum tightness of 80 ℃ and 0.7MPa, decompression dehydration obtains the eutectic solvent of regenerating, and recycles.
The dehydrated alcohol yield that complexing still kettle still top steams reaches 95% of theoretical amount, after testing, ethanol mass fraction in the product that distillation obtains > 99.7%, the mass fraction of water is less than 0.3%, and evaporation residue is less than 0.001%, reaches the standard of dehydrated alcohol.
Embodiment 4
95% commercially available ethanol water mixed solution is joined in the complexing still kettle, add eutectic solvent, continue to stir 0.5 hour.Standing 10 minutes.In the complexing still kettle, the complexing phase temperature is 20 ℃, and the complexing staged pressure is 0.1MPa, and in described eutectic solvent and described ethanol water mixed solution, the mass ratio of moisture is 15:1; Described eutectic solvent is choline chloride 60 and ethylene glycol, and its weight ratio is 1:4.3 cubic metres of described complexing still kettle volumes, aspect ratio is 2:1.
The distillation phase temperature is 80 ℃, the distillation staged pressure is 0.1MPa, moisture after distillation finishes in the ethanol water mixed solution is driven into evaporating kettle with the complex liquid that eutectic solvent forms with pump, and under the vacuum tightness of 80 ℃ and 0.7MPa, decompression dehydration obtains the eutectic solvent of regenerating, and recycles.
The dehydrated alcohol yield that complexing still kettle still top steams reaches 99% of theoretical amount, after testing, ethanol mass fraction in the product that distillation obtains > 99.5%, the mass fraction of water is less than 0.5%, and evaporation residue is less than 0.001%, reaches the standard of dehydrated alcohol.
Claims (6)
1. a method of utilizing the eutectic solvent complexing to remove moisture in the ethanol water mixed solution, is characterized in that, it comprises the following steps:
A. ethanol content is less than or equal to 95% ethanol water mixed solution and sends into the complexing still kettle, the eutectic solvent that can form complex compound with water in proportion afterwards joins the complexing still kettle under agitation condition, complexing still kettle temperature is 20 ℃～40 ℃, pressure is 0.1～0.2MPa, and in described eutectic solvent and described ethanol water mixed solution, the mass ratio of moisture is 15～20:1;
Described eutectic solvent is the eutectic solvent that quaternary ammonium salt and hydrogen bond donor form, described quaternary ammonium salt is a kind of in Dodecyl trimethyl ammonium chloride, choline chloride 60, beet alkali hydrochlorate, palmityl trimethyl ammonium chloride, tri-n-octyl methyl ammonium chloride, chitosan quaternary ammonium salt and tetrabutylammonium chloride or it is composite, and described hydrogen bond donor is a kind of in urea, glycerine, ethylene glycol, formic acid, acetic acid and methane amide or it is composite;
B. in described step a, the complex liquid that moisture in described ethanol water mixed solution and eutectic solvent form is after distillation finishes, be driven into the complex liquid storage tank, be sent to afterwards follow-up decompression dehydration operation and remove the moisture in complex liquid in evaporating kettle, obtain the eutectic solvent of regeneration for complexing next time.
2. the method for utilizing the eutectic solvent complexing to remove moisture in the ethanol water mixed solution as claimed in claim 1, is characterized in that, it is further comprising the steps of:
C squeezes into evaporating kettle by the complex liquid in complex liquid storage tank in step b with pump, before entering evaporating kettle, heater via heats, in temperature, be to remove moisture under 70 ℃～90 ℃, the vacuum tightness condition that is 0.5MPa～0.8MPa, the moisture that flow out on evaporating kettle still top enters the complex liquid of evaporating kettle for preheating;
D. the dewatered eutectic solvent stayed in evaporating kettle being sent to the complexing still kettle recycles.
3. the method for utilizing the eutectic solvent complexing to remove moisture in the ethanol water mixed solution as claimed in claim 2, is characterized in that, in described steps d, Heating temperature is 75 ℃～85 ℃.
4. the method for utilizing the eutectic solvent complexing to remove moisture in the ethanol water mixed solution as claimed in claim 3, is characterized in that, in described steps d, Heating temperature is 80 ℃.
5. the method for utilizing the eutectic solvent complexing to remove moisture in the ethanol water mixed solution as claimed in claim 1, is characterized in that, the service temperature in the complexing still kettle of described step a is 30 ℃, pressure 0.1MPa.
6. the method for utilizing the eutectic solvent complexing to remove moisture in the ethanol water mixed solution as claimed in claim 1, is characterized in that, in described ethanol water mixed solution, the water-content scope is 85%～95%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310436608.4A CN103467245B (en) | 2013-09-23 | 2013-09-23 | Method for complexing and removing water contained in ethanol and water mixed solution by utilizing eutectic solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310436608.4A CN103467245B (en) | 2013-09-23 | 2013-09-23 | Method for complexing and removing water contained in ethanol and water mixed solution by utilizing eutectic solvent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103467245A true CN103467245A (en) | 2013-12-25 |
| CN103467245B CN103467245B (en) | 2015-07-01 |
Family
ID=49792327
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310436608.4A Active CN103467245B (en) | 2013-09-23 | 2013-09-23 | Method for complexing and removing water contained in ethanol and water mixed solution by utilizing eutectic solvent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103467245B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829426A (en) * | 2015-05-21 | 2015-08-12 | 济南大学 | Continuous isopropyl ether-isopropyl alcohol azeotrope extraction and rectification technology based on choline chloride/urea low-co-melting solvent |
| CN105248416A (en) * | 2015-10-30 | 2016-01-20 | 陕西省石油化工研究设计院 | Application of low-melting-point insoluble substance to green pesticide solvent and low-melting-point insoluble substance |
| CN107760739A (en) * | 2017-09-30 | 2018-03-06 | 江南大学 | A kind of new dihydrogen bond eutectic solvent and the method for combining sodium carbonate pretreated water rice straw |
| CN107970187A (en) * | 2017-12-07 | 2018-05-01 | 珀莱雅化妆品股份有限公司 | A kind of preparation method of antiallergic plant composition |
| CN108553937A (en) * | 2018-05-15 | 2018-09-21 | 广州科帆生物科技有限公司 | natural eutectic solvent and its application in plant extract |
| CN109704919A (en) * | 2018-12-28 | 2019-05-03 | 浙江工业大学 | Water-methanol based on choline chloride eutectic solvent-alcohol mixture extraction and rectification separation method |
| CN109701361A (en) * | 2019-01-28 | 2019-05-03 | 辽宁科技大学 | For absorbing SO2And NO2Polyalcohol-choline eutectic solvent and preparation method |
| CN110540508A (en) * | 2019-08-30 | 2019-12-06 | 齐鲁工业大学 | Eutectic solvent and application thereof in extracting lignin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070193952A1 (en) * | 2003-07-21 | 2007-08-23 | Basf Aktiengesellschaft | Method For Extracting Impurities Using Ionic Liquids |
| CN103313771A (en) * | 2010-12-30 | 2013-09-18 | 费伊肯私人有限公司 | Dehydration process that employs ionic liquid |
-
2013
- 2013-09-23 CN CN201310436608.4A patent/CN103467245B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070193952A1 (en) * | 2003-07-21 | 2007-08-23 | Basf Aktiengesellschaft | Method For Extracting Impurities Using Ionic Liquids |
| CN103313771A (en) * | 2010-12-30 | 2013-09-18 | 费伊肯私人有限公司 | Dehydration process that employs ionic liquid |
Non-Patent Citations (1)
| Title |
|---|
| 赵辉等: "络合萃取蒸馏法制备无水乙醇的工业生产技术", 《西南民族学院学报自然科学版》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829426A (en) * | 2015-05-21 | 2015-08-12 | 济南大学 | Continuous isopropyl ether-isopropyl alcohol azeotrope extraction and rectification technology based on choline chloride/urea low-co-melting solvent |
| CN105248416A (en) * | 2015-10-30 | 2016-01-20 | 陕西省石油化工研究设计院 | Application of low-melting-point insoluble substance to green pesticide solvent and low-melting-point insoluble substance |
| CN107760739A (en) * | 2017-09-30 | 2018-03-06 | 江南大学 | A kind of new dihydrogen bond eutectic solvent and the method for combining sodium carbonate pretreated water rice straw |
| CN107970187A (en) * | 2017-12-07 | 2018-05-01 | 珀莱雅化妆品股份有限公司 | A kind of preparation method of antiallergic plant composition |
| CN108553937A (en) * | 2018-05-15 | 2018-09-21 | 广州科帆生物科技有限公司 | natural eutectic solvent and its application in plant extract |
| CN108553937B (en) * | 2018-05-15 | 2020-12-25 | 广州科帆生物科技有限公司 | Natural eutectic solvent and application thereof in plant extraction |
| CN109704919A (en) * | 2018-12-28 | 2019-05-03 | 浙江工业大学 | Water-methanol based on choline chloride eutectic solvent-alcohol mixture extraction and rectification separation method |
| CN109701361A (en) * | 2019-01-28 | 2019-05-03 | 辽宁科技大学 | For absorbing SO2And NO2Polyalcohol-choline eutectic solvent and preparation method |
| CN110540508A (en) * | 2019-08-30 | 2019-12-06 | 齐鲁工业大学 | Eutectic solvent and application thereof in extracting lignin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103467245B (en) | 2015-07-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103467245B (en) | Method for complexing and removing water contained in ethanol and water mixed solution by utilizing eutectic solvent | |
| CN103012335B (en) | Method for co-producing furfural and 5-hydroxymethylfurfural by using lignocellulose-containing biomass | |
| CN105368574B (en) | Method for reducing acid value of liquid organic mixture | |
| CN103360255B (en) | Method for preparation of ethyl levulinate from furfural residues | |
| KR20200108845A (en) | Manufacturing method and application of highly active lignin and by-product furfural | |
| CN101429288A (en) | Method for treating process liquid generated in production process of polyphenylene sulfide | |
| CN104045518A (en) | Preparation method of 2-methyl-3-butyne-2-ol | |
| CN110590718A (en) | Production method for extracting furfural from corncobs | |
| CN105111079A (en) | Method and device for separating acetic acid sec-butyl ester and sec-butyl alcohol | |
| CN104292193A (en) | Method for grading biomass, preparing furfural and preparing levulinic acid through two steps | |
| CN105498801A (en) | Preparation method of sulfated carbonized corn cob catalyst and method for preparing furfural from xylose in presence of catalyst | |
| CN102584751B (en) | Process and reaction system for preparing furfuraldehyde by reaction rectification method | |
| CN101948400B (en) | Preparation method of methyl anthranilate | |
| CN101863738B (en) | Method for preparing neopentyl glycol | |
| CN103626633A (en) | Method for promoting solid catalyst to depolymerize cellulose | |
| CN102134191A (en) | Process method for producing ethyl acetate by catalytic rectification | |
| CN104086363A (en) | Energy-saving process for recycling n-butyl acetate and butyl alcohol from waste acid water | |
| CN103739486A (en) | Production method for ethyl acetate crude product | |
| CN104774636A (en) | Preparation method of biological oil | |
| CN104844542A (en) | Method for preparing gamma-valerolactone by levulinic acid ester without solvents | |
| CN104140357B (en) | Take acetic acid as the method for raw material production ethanol | |
| CN102659088A (en) | Water-phase synthesis method of sodium azide | |
| CN103508985A (en) | Method for producing furfural and/or 5-hydroxymethylfurfural by using red alga biomass as raw material | |
| CN102627551B (en) | Method for isomerizing rosin resin acid promoted by solid super acid | |
| CN114108350A (en) | Method for quickly separating main components of wood biomass by using eutectic solvent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent of invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Feng Danhua Inventor after: Song Liying Inventor before: Feng Danhua Inventor before: Song Liying Inventor before: Other inventor requests not to publish the name |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: FENG DANHUA SONG LIYING OTHER INVENTORS HAVE WAIVED THE RIGHT TO BE MENTIONED TO: FENG DANHUA SONG LIYING |
|
| C53 | Correction of patent of invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Feng Danhua Inventor after: Song Liying Inventor after: Other inventor requests not to publish the name Inventor before: Song Liying Inventor before: Other inventor requests not to publish the name |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: SONG LIYING OTHER INVENTORS HAVE WAIVED THE RIGHT TO BE MENTIONED TO: FENGDANHUA SONG LIYING OTHER INVENTORS HAVE WAIVED THE RIGHT TO BE MENTIONED |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C53 | Correction of patent of invention or patent application | ||
| CI01 | Publication of corrected invention patent application |
Correction item: First inventor Correct: Feng Shubo False: The inventor has waived the right to be mentioned Number: 26 Volume: 31 |
|
| CI02 | Correction of invention patent application |
Correction item: First inventor Correct: Feng Shubo False: The inventor has waived the right to be mentioned Number: 26 Page: The title page Volume: 31 |
|
| ERR | Gazette correction |
Free format text: CORRECT: THE FIRST INVENTOR; FROM: REQUEST TO WITHHOLD NAME TO: FENG SHUBO |