CN1876686A - Method for producing xanthans using film-separated concentrated ferment liquor - Google Patents
Method for producing xanthans using film-separated concentrated ferment liquor Download PDFInfo
- Publication number
- CN1876686A CN1876686A CN 200610036390 CN200610036390A CN1876686A CN 1876686 A CN1876686 A CN 1876686A CN 200610036390 CN200610036390 CN 200610036390 CN 200610036390 A CN200610036390 A CN 200610036390A CN 1876686 A CN1876686 A CN 1876686A
- Authority
- CN
- China
- Prior art keywords
- xanthan gum
- film
- filtration
- concentration
- desalination
- 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
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention relates the method of producing xanthan gum with film separating concentration fermentation liquor. The invention has the advantages of little raw material, high productivity and high purify. The method comprises the following steps: pumping xanthan gum fermentation liquor into microstrain film assembly, filtering, desalting, and thickening, getting xanthan gum desalinization concentration liquid; adding alcohol, settling xanthan gum; filter-pressing it, getting xanthan gum whose moisture content is below 23-30% and filtering medium, distilling filtering medium, and reclaiming alcohol, drying, disintegrating, and getting xanthan gum.
Description
Technical field
The present invention relates to a kind of xanthan gum, particularly relate to the method that a kind of membrane sepn concentrates xanthan gum fermentation broth production xanthan gum.
Background technology
Xanthan gum is a kind of microbial polysaccharide, also claims yellow unit cell polysaccharide, also claims xanthan gum.Xanthan gum is a kind of novel fermentation product of getting up of newly-developed in the world, and English name is Xanthan Gum, and trade(brand)name has Kelzan (technical grade, the U.S.), Keltrol (food grade, the U.S.), Xc-Polymer (oil with) etc.Xanthan gum is to be main raw material with starch, through microbial fermentation and a series of biological process, and a kind of biopolymer that finally obtains.Its main component is glucose, seminose and glucuronic acid etc.Molecular weight reaches millions of.Complete xanthan gum molecule is that the Mierocrystalline cellulose of many side chains is arranged is the linear structure of skeleton, because side chain contains acidic-group, so xanthan gum presents polyanion in the aqueous solution.In the aqueous solution, the electrically charged side chain of xanthan gum molecule oppositely twines cellulosic backbone, forms similar bar-shaped rigid structure, is the primary structure of xanthan gum molecule; Xanthan gum is intermolecular maintains the formation double stranded helix by the hydrogen chain, is the secondary structure of xanthan gum molecule; Xanthan gum molecule double stranded helix structure is arranged in neat helix poly zoarium by non-covalent chain combination, is three grades of three-dimensional arrangements of xanthan gum molecule.
Xanthan gum is a kind of anionic high molecular polymer, and is soluble in water, forms hydrophilic sol.Because its macromole singularity and colloid property, therefore have good emulsifying, tackifying, pseudo-plasticity, thixotropy, particle suspension, resistance to acids and bases, high thermal resistance, anti-salt calcium and high biological safety, can be used for emulsifying agent, stablizer, thickening material, treating compound and film binder, be widely used in food and non-food product industry.It is reported, it uses nearly more than 20 industry of coverage rate, tens of kinds of products, mainly contain food, oil, Di Kuang, medicine, light textile, pottery, lass lining, printing and dyeing, spices, makeup, tackiness agent, papermaking, building, gravity concentration, hydrometallurgy, agricultural chemicals, fire-fighting, explosive, paint, wash dye, photograph, video-tape and ink etc.And, make technological process, range of product and the quality generation change in various degree of these industries, bring great social benefit and economic benefit.
On Technology, the xanthan gum production technique of China and developed country's basically identical divide fermentation and back to extract two workshop sections, but the aggregate level gap are bigger.It shows: 1. strain excellent is cultivated and screening, and especially high temperature resistant good quality and high output bacterial strain aspect does not have big breakthrough as yet.2. the production equipment scale that adopted of domestic production producer is less than normal, and technical equipment is relatively poor (to adopt totally enclosed factory building, pipeline, valve as the manufacturer that has abroad, even even service platform is the stainless steel making, and it is then more advanced to detect control device); 3. individual other consumption indicators is higher etc.
The production of xanthan gum is to be main raw material with carbohydrate (as corn, starch etc.), through Xanthomonas campestris (Xanthomonas campestris) biological fermentation engineering cultivation, extraction using alcohol, drying, pulverizing and get.At present, the xanthan gum production process route is identical substantially both at home and abroad, and just there are outside the gap other basically identicals in China at aspects such as scale, fermentation technique, equipment, type of solvent and consumption, energy consumptions compared with developed countries.Production generally is divided into fermentation and extracts two workshop sections, and operational path is seen Figure of description 2.
There is two large problems in traditional technology:
1. the mixing of fermentation media, oxygen supply and heat transfer etc. are very difficult, and energy consumption is big;
2. carry out solid-liquid separation with alcohol, the ethanol consumption is big and the rate of recovery is low.
Problem at the aforesaid method existence, the present invention has developed the method that a kind of membrane sepn concentrates xanthan gum fermentation broth production xanthan gum, consumption of ethanol is from 2.5 times of 0.9 times of reducing to the fermented liquid original volume of fermentating liquid volume when making the production xanthan gum, save more than 60%, greatly reduce raw materials consumption, saved raw materials cost.
Publication number is the engineering method that the application for a patent for invention of CN1394878 discloses a kind of xanthan gum separation and Extraction, and material interpolation, mixing, precipitation, separation and pH value regulate process are balancedly carried out in airtight mechanical means continuously.
Publication number is the back extraction process that the application for a patent for invention of CN1046758 discloses a kind of xanthan gum fermentation broth, in xanthan gum fermentation broth, add complexing agent and xanthan gum complexing, complexing Hou is filtered, filter cake scrub solution elution, right Hou refilters, dried stamping, use mixing amine salt or pure amine salt to be complexing agent, under normal temperature to 80 ℃ stirring, carried out complexing 10-60 minute, 6-40 times low-carbon alcohol of filtration Hou usefulness xanthan gum or ketone under agitation elution 30-200 minute, control pH value is filtered the Hou filter cake at 60 ± 5 ℃ of following drying 2-6 of vacuum hours in the 7-13 scope.
Summary of the invention
The objective of the invention is to big and not desalination of product at its alcoholic acid consumption of the ethanol sedimentation operation in the existing xanthan gum production process, ash is higher, problems such as purity is lower, provide a kind of starting material material consume less, yield is high, product purity is high, and the membrane sepn that is suitable for suitability for industrialized production concentrates the method for xanthan gum fermentation broth production xanthan gum.
The objective of the invention is to realize by the following method:
1) micro-filtration desalination and concentration: xanthan gum fermentation broth pumped into from basin filters desalination and concentration in the micro-filtration membrane module, xanthan gum desalination and concentration liquid;
2) ethanol sedimentation: will add ethanol through the xanthan gum desalination and concentration liquid of micro-filtration desalination and concentration gained, the precipitation xanthan gum;
3) press filtration: will must contain the xanthan gum (solid content 70%～77%) and the filtered liquid that wet less than 23%～30% through the xanthan gum precipitation press filtration of ethanol sedimentation, filtered liquid reclaims ethanol through distillation;
4) drying-granulating: press filtration gained xanthan gum is dry and pulverize granulation and get xanthan gum.
In step 1), described micro-filtration desalination and concentration is to be that the micro-filtrate membrane filtration desalination and concentration of 0.1～0.4 μ m is to 30%～50% of original volume with the fermented liquid of xanthan gum with the aperture, used membrane module is plate type membrane component or tubular membrane component, mould material is polysulfone membrane, poly (ether sulfone) film, polyvinylidene fluoride film or cellulose membrane, working conditions is: room temperature to 65 ℃, entrance pressure 5.0～43.5bar, go out to press 1～40.5bar, pressure difference is 3～4bar; Or used mould material is ceramic membrane, and working conditions is: room temperature to 85 ℃, and entrance pressure 4.0～43.5bar goes out to press 1～40.5bar, and pressure difference is 3bar.
In step 2) in, described ethanol sedimentation is the xanthan gum concentrated solution metering with little concentrating and desalinating gained, extraordinarily goes into 85%～100% ethanolic soln by 1.0～2.5 of concentrated solution volume.
In step 3), described press filtration is to adopt the pressure filter filtering and concentrating to solid content 20%～25% xanthan gum through ethanol sedimentation, use the special-purpose filtering equipment press filtration of xanthan gum to solid content 70%～77% again, get xanthan gum wet feed and filtrate, filtrate is reclaimed ethanol through distillation.
In step 4), described drying-granulating is that the xanthan gum wet feed is pulverized after drying to solid content more than 90%, adopt pulverizer that the xanthan gum siccative is pulverized the back then and cross 80 to 100 mesh sieves, ash less than 5%, the high-quality xanthan gum finished product of anti-100 ℃ of high-temperature behaviors.
Use micro-filtration concentrating and separating method of the present invention, can realize following purpose:
1) can effectively the xanthan gum fermentation filtering solution be concentrated into 25%～40% of original volume, use 85%～90% ethanol sedimentation xanthan gum again, thereby make 2.5 times 0.9 times of reducing to fermented liquid original volume of consumption of ethanol from fermentating liquid volume, save more than 60%, greatly reduce raw materials consumption, saved raw material.
2) when concentrating xanthan gum solution, can also remove inorganic salt in the solution, reduce the ash of xanthan gum, improve the purity and the product performance of xanthan gum.
Embodiment
Embodiment 1
1) micro-filtration separates desalination and concentration: the xanthan gum fermentation broth metering of the gained that will ferment and in interchanger, heat with hot water after, directly pump into and filter desalination in the micro-filtration membrane module, be concentrated into 40% of original volume, get the desalination and concentration liquid of xanthan gum, the used membrane module of micro-filtration is the plate type membrane component of ultra-flo.Mould material is selected four kinds of 605,610,615,7020 poly (ether sulfone) films etc. respectively for use, compares experiment, measures its membrane flux and cycles of concentration.The aperture of microfiltration membrane is 0.1～0.4 μ m, and working conditions is: 25～40 ℃, entrance pressure 5.5bar goes out to press 1.5bar, and pressure difference is 4bar.The flux maximum of 7020 polyether sulfone micro-filtration membranes of 0.2 μ m after measured, cycles of concentration is the highest, average out to 25LMH, thus determine that micro-filtration adopts 7020 polyether sulfone micro-filtration membranes of 0.2 μ m.
2) ethanol sedimentation:, add 85%～90% the ethanolic soln of 750L (xanthan gum concentrated solution 1.5 times), and the precipitation xanthan gum is sticking to solution under constantly stirring with the xanthan gum concentrated solution of micro-filtration concentrating and desalinating gained metering 500L.
3) press filtration: will separate concentrating 9～10 times with Special Equipment through the xanthan gum solution of ethanol sedimentation to solid content 20%～25%, use the special-purpose filtering equipment press filtration of xanthan gum to solid content 70%～77% again, get xanthan gum wet feed and filtrate, filtrate is reclaimed ethanol through distillation.
4) drying-granulating: the xanthan gum wet feed is pulverized after drying to solid content more than 90%, adopts micronizer mill that the xanthan gum siccative is pulverized the back then and cross 80～100 mesh sieves, ash less than 5%, the high-quality xanthan gum finished product of anti-100 ℃ of high-temperature behaviors.
Being analyzed as follows of testing data:
1. ultra-flo is selected film test: by contrasting the service data of 605,610,615,7020 films, determine to select for use 7020 polyethersulfones, 0.2 μ m microfiltration membrane, because the maximum average out to 25LMH of its flux because cleaning needs to adopt hypochlorous acid, therefore also need select the film of scale resistance for use simultaneously.
2. cycles of concentration: with 3 batches of flat sheet membrane, having two batches, all to have reached concentrated solution/fermented liquid per-cent be 59% and 65%, and 1 batch is concentrated to 67% in addition; It is attainable fully that therefore conservative click-through is crossed membrane concentration to 60%.
3. flux: 3 batches of flat sheet membrane are at 25～30 degree operation average flux 20LMH.Film cleans restorability: flat sheet membrane can be recovered after cleaning by hypochlorous acid, because protein content is few in the feed liquid, so cleans and restoratively should be able to accomplish from theoretical analysis.
4. the benefit of membrane concentration: fermented liquid stoste need add 2.5 times of fermentating liquid volume 85% alcohol according to test just can reach the heavy purpose of wine, the fermented liquid process is concentrated to 60% concentrated solution, only need just can reach the heavy purpose of wine with 0.9 times 85% alcohol of fermented liquid original volume.The effect of therefore saving alcohol is obvious.
Embodiment 2
1) micro-filtration desalination and concentration: the xanthan gum fermentation broth of the gained that will ferment with the aperture be 0.2 μ m ceramic micro filter membrane filtration desalination and concentration to 35% of original volume, the desalination and concentration liquid of xanthan gum; Working conditions is: 40 ℃, entrance pressure 4.0bar goes out to press 1bar, and pressure difference is 3bar.
2) ethanol sedimentation:, add 85%～90% the ethanolic soln of 1000L (xanthan gum concentrated solution 2 times), and the precipitation xanthan gum is sticking to solution under constantly stirring with the xanthan gum concentrated solution of little concentrating and desalinating gained metering 500L.
3) press filtration: will separate concentrating 10 times through the xanthan gum solution of ethanol sedimentation with Special Equipment, and to solid content 25%, use the special-purpose filtering equipment press filtration of xanthan gum to solid content 76% again, and get xanthan gum wet feed and filtrate, filtrate is reclaimed ethanol through distillation.
4) drying-granulating: the xanthan gum wet feed is pulverized after drying to solid content more than 90%, adopts micronizer mill that the xanthan gum siccative is pulverized the back then and cross 80～100 mesh sieves, ash less than 5%, the high-quality xanthan gum finished product of anti-100 ℃ of high-temperature behaviors.
Embodiment 3
Similar to Example 1, its difference be with the xanthan gum fermentation broth metering of fermentation gained and in interchanger with after the hot water heating, directly pump into and filter desalination in the micro-filtration membrane module, be concentrated into 30% of original volume, get the desalination and concentration liquid of xanthan gum, the used membrane module of micro-filtration is the plate type membrane component of ultra-flo.Mould material is selected polysulfone membrane respectively for use, and the aperture of microfiltration membrane is 0.1 μ m, and working conditions is: 40～60 ℃, entrance pressure 11bar goes out to press 8bar.With the xanthan gum concentrated solution of micro-filtration concentrating and desalinating gained metering 500L, add the ethanolic soln of 500L (xanthan gum concentrated solution 1 times), and the precipitation xanthan gum is sticking to solution under constantly stirring.
Embodiment 4
Similar to Example 1, its difference be with the xanthan gum fermentation broth metering of fermentation gained and in interchanger with after the hot water heating, directly pump into and filter desalination in the micro-filtration membrane module, be concentrated into 50% of original volume, get the desalination and concentration liquid of xanthan gum, the used membrane module of micro-filtration is the tubular membrane component of ultra-flo.Mould material is selected polyvinylidene fluoride film respectively for use, and the aperture of microfiltration membrane is 0.4 μ m, and working conditions is: 55～65 ℃, entrance pressure 43bar goes out to press 40bar.With the xanthan gum concentrated solution of micro-filtration concentrating and desalinating gained metering 500L, add the ethanolic soln of 1250L (xanthan gum concentrated solution 2.5 times), and the precipitation xanthan gum is sticking to solution under constantly stirring.
Embodiment 5
Similar to Example 2, its difference is in the micro-filtration desalination and concentration, with the xanthan gum fermentation broth of fermentation gained with the aperture be 0.3 μ m ceramic micro filter membrane filtration desalination and concentration to 50% of original volume, desalination and concentration liquid that must xanthan gum; Working conditions is: 60～85 ℃, entrance pressure 43bar goes out to press 40bar, and pressure difference is 3bar.
Claims (7)
1. the method for a producing xanthans using film-separated concentrated ferment liquor is characterized in that the steps include:
1) micro-filtration desalination and concentration: xanthan gum fermentation broth pumped into from basin filters desalination and concentration in the micro-filtration membrane module, xanthan gum desalination and concentration liquid;
2) ethanol sedimentation: will add ethanol through the xanthan gum desalination and concentration liquid of micro-filtration desalination and concentration gained, the precipitation xanthan gum;
3) press filtration: will be through the press filtration of the xanthan gum of ethanol sedimentation precipitation, must contain wetly less than 23%～30% or the xanthan gum and the filtered liquid of solid content 70%～77%, filtered liquid reclaims ethanol through distillation;
4) drying-granulating: press filtration gained xanthan gum is dry and pulverize granulation and get xanthan gum.
2. the method for a kind of producing xanthans using film-separated concentrated ferment liquor as claimed in claim 1, it is characterized in that in step 1) described micro-filtration desalination and concentration is to be that the micro-filtrate membrane filtration desalination and concentration of 0.1～0.4 μ m is to 30%～50% of original volume with the fermented liquid of xanthan gum with the aperture.
3. the method for a kind of producing xanthans using film-separated concentrated ferment liquor as claimed in claim 1, it is characterized in that in step 1), described membrane module is plate type membrane component or tubular membrane component, mould material is polysulfone membrane, poly (ether sulfone) film, polyvinylidene fluoride film or cellulose membrane, working conditions is: room temperature to 65 ℃, entrance pressure 5.0～43.5bar, go out to press 1～40.5bar, pressure difference is 3～4bar.
4. the method for a kind of producing xanthans using film-separated concentrated ferment liquor as claimed in claim 1 is characterized in that in step 1), and mould material is a ceramic membrane, working conditions is: room temperature to 85 ℃, entrance pressure 4.0～43.5bar goes out to press 1～40.5bar, and pressure difference is 3bar.
5. the method for a kind of producing xanthans using film-separated concentrated ferment liquor as claimed in claim 1, it is characterized in that in step 2) in, described ethanol sedimentation is the xanthan gum concentrated solution metering with little concentrating and desalinating gained, extraordinarily goes into 85%～100% ethanolic soln by 1.0～2.5 of concentrated solution volume.
6. the method for a kind of producing xanthans using film-separated concentrated ferment liquor as claimed in claim 1, it is characterized in that in step 3), described press filtration is to adopt the pressure filter filtering and concentrating to solid content 20%～25% xanthan gum through ethanol sedimentation, use the special-purpose filtering equipment press filtration of xanthan gum to solid content 70%～77% again, get xanthan gum wet feed and filtrate, filtrate is reclaimed ethanol through distillation.
7. the method for a kind of producing xanthans using film-separated concentrated ferment liquor as claimed in claim 1, it is characterized in that in step 4), described drying-granulating is that the xanthan gum wet feed is pulverized after drying to solid content more than 90%, adopt pulverizer that the xanthan gum siccative is pulverized the back then and cross 80～100 mesh sieves, ash less than 5% xanthan gum finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610036390 CN1876686A (en) | 2006-07-10 | 2006-07-10 | Method for producing xanthans using film-separated concentrated ferment liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610036390 CN1876686A (en) | 2006-07-10 | 2006-07-10 | Method for producing xanthans using film-separated concentrated ferment liquor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1876686A true CN1876686A (en) | 2006-12-13 |
Family
ID=37509263
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610036390 Pending CN1876686A (en) | 2006-07-10 | 2006-07-10 | Method for producing xanthans using film-separated concentrated ferment liquor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1876686A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260354A (en) * | 2010-05-28 | 2011-11-30 | 淄博中轩生化有限公司 | Preprocessing method for increasing viscosity of xanthan gum product |
| CN103664518A (en) * | 2012-08-31 | 2014-03-26 | 郸城财鑫糖业有限责任公司 | Method for recycling waste alcohol in gellan gum production process |
| CN103897074A (en) * | 2014-03-12 | 2014-07-02 | 山东省食品发酵工业研究设计院 | Method for separating and purifying curdlan by use of membrane process |
| CN101642680B (en) * | 2009-08-14 | 2015-06-10 | 湖南豫园生物科技有限公司 | Concentration technology for zymogen liquid |
| CN110093389A (en) * | 2019-03-25 | 2019-08-06 | 卢松 | The fermentation method for producing of instant xanthan gum |
-
2006
- 2006-07-10 CN CN 200610036390 patent/CN1876686A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101642680B (en) * | 2009-08-14 | 2015-06-10 | 湖南豫园生物科技有限公司 | Concentration technology for zymogen liquid |
| CN102260354A (en) * | 2010-05-28 | 2011-11-30 | 淄博中轩生化有限公司 | Preprocessing method for increasing viscosity of xanthan gum product |
| CN103664518A (en) * | 2012-08-31 | 2014-03-26 | 郸城财鑫糖业有限责任公司 | Method for recycling waste alcohol in gellan gum production process |
| CN103897074A (en) * | 2014-03-12 | 2014-07-02 | 山东省食品发酵工业研究设计院 | Method for separating and purifying curdlan by use of membrane process |
| CN103897074B (en) * | 2014-03-12 | 2016-03-02 | 山东省食品发酵工业研究设计院 | A kind of method utilizing membrane process separation and purification curdlan |
| CN110093389A (en) * | 2019-03-25 | 2019-08-06 | 卢松 | The fermentation method for producing of instant xanthan gum |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103468766B (en) | Preparation method of high-purity mannan oligosaccharide | |
| CN101020724A (en) | Process of preparing low molecular weight sodium hyaluronate | |
| CN102180988B (en) | Method for preparing k-carrageenan with high gel strength from eucheuma | |
| CA2784226A1 (en) | Process for the preparation of homopolysaccharides | |
| CN103073652B (en) | A kind of extracting method of spirulina polysaccharide | |
| CN1876686A (en) | Method for producing xanthans using film-separated concentrated ferment liquor | |
| CN1289532C (en) | Post extraction production technology of pullulanose | |
| CN101434553B (en) | Method for all-film extraction of valine | |
| Pal et al. | Purification and concentration of gluconic acid from an integrated fermentation and membrane process using response surface optimized conditions | |
| CN103194545B (en) | Method for treating sugarcane mixed clear juice | |
| WO2023116142A1 (en) | System and method for preparing erythritol and polydextrose from corn starch | |
| CN101538593A (en) | Method for coupling production of Gamma-polyglutamic acid by technologies of microbial fermentation and membrane separation | |
| Lo et al. | Kinetic and feasibility studies of ultrafiltration of viscous xanthan gum fermentation broth | |
| AU2017299082A1 (en) | Separation of enzymes from trichoderma reesei by filter press and tangential filtration on a ceramic membrane | |
| CN1847266A (en) | Girasole synanthrin producing process based on two-stage ultrafiltering technology | |
| CN111777504B (en) | Method for purifying L-lactic acid extracted from fermentation liquor | |
| CN102432643B (en) | Separation method of rhamnolipid by using ultrafiltration membrane | |
| CN1554773A (en) | Method for extracting fermentikve macrolide antibiotics using membrane | |
| Singh et al. | Membrane Technology in Corn Refining and Bioproduct‐Processing | |
| JP2012528903A (en) | Post extraction method for higher order acyl group gellan gum | |
| Moosavi-Nasab et al. | Fermentative production and characterization of carboxymethyl bacterial cellulose using date syrup | |
| CN215162258U (en) | Device for extracting succinic acid from fermentation liquor | |
| CN100554284C (en) | A kind of extracting method of high transparent xanthan gum | |
| CN114471168A (en) | Method for separating and concentrating beet polysaccharide and betaine by combining thermal flocculation with multi-stage nanofiltration membrane | |
| CN103602652B (en) | A kind of method of purification of food-grade neutral protease |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |