CN101108741A - Industrial process for preparing nm-class active calcium carbonate - Google Patents
Industrial process for preparing nm-class active calcium carbonate Download PDFInfo
- Publication number
- CN101108741A CN101108741A CNA2006100888598A CN200610088859A CN101108741A CN 101108741 A CN101108741 A CN 101108741A CN A2006100888598 A CNA2006100888598 A CN A2006100888598A CN 200610088859 A CN200610088859 A CN 200610088859A CN 101108741 A CN101108741 A CN 101108741A
- Authority
- CN
- China
- Prior art keywords
- calcium carbonate
- carbonization
- accordance
- acid
- crystal
- 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
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides the industrial preparation method of the nano activated calcium carbonate. The crystal control agent is added in the suspending liquid of the calcium hydroxide and is carbonized by the kiln gas containing the carbon dioxide. Through controlling the temperature and concentration of the calcium hydroxide, the concentration of the carbon dioxide and the addition and variety of the crystal control agent, the initial nucleation rate and nucleation quantity of the crystal and the growth rate of each crystal face of the crystal during carbonization are adjusted to realize the shape control of the crystal, and then surfactant is added to conduct activating treatment. The nano activated calcium carbonate is gained after filtering and drying, which has a shape of cube and is regulable when the grain size is between 20nm to 100nm. The product gained by the method has excellent performance and can work as the functional filler, which can be widely used in such industries as top-grade coating, rubber, plastic and adhesive.
Description
Technical field
The present invention relates to a kind of industrial production process of lime carbonate, be specifically related to a kind of industrial production process of nm-class active calcium carbonate.
Technical background
Nano-calcium carbonate is meant the calcium carbonate powder of particle diameter less than 100nm, and the lime carbonate surface is hydrophilic under usual conditions, becomes lipophilicity after surperficial organic process, becomes nm-class active calcium carbonate.Being widely used in improving product performance in plastics, rubber, the macromolecule resin, improving the quality of products, is a kind of new type functional mineral filler.
At present, the preparation method of nano-calcium carbonate has continuous spray method, hypergravity carborization, stirred pot carborization.The spray method nozzle easily stops up continuously, is difficult to guarantee the consistence of droplet in suitability for industrialized production, and production control is had relatively high expectations.The hypergravity carborization by lab scale in the process of industrialized conversion, factors such as its original field of force distribution have restricted production application.Mainly be still the carbonization at low temperature method at present, adopt the refrigerator refrigeration cool-down, carbonization temperature remains on below 20 degree, makes finished product grain size below 100 nanometers, but the unstable product quality that generates, even particle size distribution is big, and energy consumption is big.
Summary of the invention
The technical issues that need to address of the present invention provide a kind of industrial production process of new nm-class active calcium carbonate, this method is according to the performance requriements of product, at finite concentration, in the calcium hydroxide suspension under the temperature condition, add the crystal control agent, feed kiln gas again and carry out carbonization, how much control initial stage crystalline nucleation, and the growth velocity of each crystal face of crystal subsequently, make its even growth, thereby it is controlled to reach even particle size distribution, and crystal shape is complete, has the cubes nano-calcium carbonate of good dispersion, add tensio-active agent then and carry out activation treatment, make it become the product of excellent property.
The crystal control agent is made up of sugar (polysaccharide or monose) and vitriol, and composition and ratio require to adjust according to product cut size.Sugar wherein begins the crystalline nucleus grown up in carbonization and plays the promotion regulating effect, and vitriol is regulated the electric charge of each crystal face in crystal growing process subsequently, makes its equilibrium, regular growth, and plays the effect of the adhesion of avoiding reuniting.
Step of the present invention is as follows:
(1) the unslaked lime hydrolysis generates calcium hydroxide suspension, through slag removal and purification, concentration is adjusted in 15-45 degree scope in 5-14%, temperature as required, add the crystal control agent then, the kiln gas that feeding contains carbonic acid gas carries out carbonization, carbonization is 7-8 to slurries ph value, recarbonize 5 to 10 minutes.Generate nano-calcium carbonate, temperature rising 20-30 degree in carbonization process, the slurries outlet temperature reaches the 35--45 degree.
Wherein the crystal control agent of Jia Ruing is the mixing solutions of sugar (polysaccharide, monose) and vitriol, and concentration is 5-25%, and add-on is for generating the 0.5-8% of lime carbonate.
Vitriol is: Tai-Ace S 150, zinc sulfate, ammonium sulfate, sal epsom, polysaccharide and monose are: sucrose, glucose, lactose, the consumption ratio range of vitriol that adds and sugar is adjusted according to the purposes difference of the nm-class active calcium carbonate that generates between 0.1-10.
The kiln gas that contains carbonic acid gas that feeds is through water washing cleaning, and the volumetric concentration of carbonic acid gas is 20-30%.
(2) after carbonization finishes, add surface treatment agent in slurries, carry out activation treatment under the insulated and stirred state, the treatment time is 1.5--2.5 hour.The concentration of surface treatment agent is 5--25%, and temperature is the 80-100 degree.
Said surface treatment agent is the aqueous solution that lipid acid and sodium soap and water soluble borate fat coupling agent are made into, or resinous acid (sodium) saponification liquor, and concentration is 5-25%, and temperature is the 80-100 degree, and add-on is the nano-calcium carbonate 1-4.5% that generates.
Lipid acid (sodium) is that carbonatoms is the lipid acid (sodium) between the C10--C18, and boric acid fat coupling agent is SBW-3, SBW-1.
The consumption ratio of lipid acid acid, sodium soap and boric acid fat coupling agent is between the 0.1---10, adjusts according to the different purposes of the nm-class active calcium carbonate that generates,
When adopting resinous acid (sodium) as treatment agent, resinous acid saponification liquid added after 1.5 hours, added Tai-Ace S 150 or solution of zinc sulfate that concentration is 5-20% again, handled 1 hour again, filtered then.
Resinous acid (sodium) is meant sylvic acid (sodium), hydroabietic acid (sodium) etc.
(3) the slurries activation treatment finishes, and nano-calcium carbonate slurries filtered while hot, in the oven dry of the temperature condition of routine makes the nm-class active calcium carbonate finished product through fragmentation.
Embodiment
Below just the present invention describe in the mode of embodiment, but embodiment does not limit protection scope of the present invention.
Embodiment 1
In the carbonating tower that 5 cubic metres bands stir, add 3.5m
3Calcium hydroxide suspension, calcium hydroxide suspension is that mass concentration is 9%, adds crystal control agent sucrose 20kg simultaneously through purified, zinc sulfate 10kg, (volumetric concentration: 20-30%) carry out carbonization, it is 16 degree that carbonization begins temperature, and carbonization is 7-8 to the ph value of slurries to feed carbonated kiln gas, recarbonize 5-10 minute, make the suspension of nano-calcium carbonate, along with the carrying out of carburizing reagent, slurry temperature is elevated to about 44 degree.
Adding temperature in these slurries is the aqueous solution liquid 500kg that 85 degree contain sodium stearate (20kg) boric acid fat coupling agent SBW-3 (5kg), continue to stir, insulation was handled 2 hours, filtered while hot then, dry at 100 degree, must be shaped as cubes through broken, size distribution is at 60-90nm, and oil-absorption(number) is less than 30gDop/100gCaCO
3, specific surface area is greater than 20%, and do not have the nm-class active calcium carbonate of reunion.
Embodiment 2
In the carbonating tower that 5 cubic metres bands stir, add purified calcium hydroxide suspension 3.5m
3The mass concentration of calcium hydroxide suspension is 6%, add the crystal control agent simultaneously: glucose 15kg, ammonium sulfate 5kg feeds the kiln gas (concentration is 20-30%) that contains carbonic acid gas and carries out carbonization, it is 22 degree that carbonization begins temperature, carbonization is 7-8 to slurries ph value, recarbonize 5-10 minute, makes the suspension of nano-calcium carbonate, along with carburizing reagent must be carried out, slurry temperature is elevated to about 42 degree.
Adding temperature in these slurries is 90 degree, concentration is that 10% sodium abietate saponification liquor 300kg carries out surface activation process, handle after 1.5 hours, add concentration again and be 20% alum liquor 50kg, continued stir process one hour, and filtered,, pulverize to such an extent that be shaped as cubes in 100 degree oven dry, size distribution is at 20-50nm, and oil-absorption(number) is less than 50gDOP/100gCaCO
3, specific surface area is greater than 20%, and the nm-class active calcium carbonate of not reuniting.
Embodiment 3
In the carbonating tower that 5 cubic metres bands stir, add purified calcium hydroxide suspension 3.5m
3The mass concentration of calcium hydroxide suspension is 11.5%, add the crystal control agent simultaneously: ammonium sulfate 30kg, lactose 15kg, the kiln gas (concentration is 20-30%) that the back feeding that stirs contains carbonic acid gas carries out carbonization, and it is 20 degree that carbonization begins temperature, and carbonization is 7-8 to slurries ph value, recarbonize 5-10 minute, make the suspension of nm-class active calcium carbonate, along with the carrying out of carbonization, the temperature of slurries is elevated to 45 degree.
Adding temperature in these slurries is 90 degree, the aqueous solution solution 500kg that contains SBW-1 boric acid fat coupling agent 20kg, sodium stearate 15kg, continue insulated and stirred, handled 2 hours, filter, dry at 100 degree, fragmentation is made and is shaped as cubes, and size distribution is at 70-100nm, and oil-absorption(number) is at 20-30Dop/100gCaCO
3, specific surface area is greater than 20%, and the nm-class active calcium carbonate of not reuniting.
Claims (9)
1. the industrial production process of a nm-class active calcium carbonate is characterized in that:
(1) in calcium hydroxide suspension, adds the crystal control agent, in the carbonating tower that band stirs, feed carbon dioxide and carry out carbonization;
Said crystal control agent is the mixture of vitriol and carbohydrate;
(2) carbonization to pH value is 7-8, ventilates 5-10 minute again, and carbonization finishes, and adds surface treatment agent, carries out surface activation process, and the treatment time is 1.5-3 hour, filters, dries, and makes nm-class active calcium carbonate;
Said surface treatment agent is the mixture of lipid acid and water soluble borate fat coupling agent, or resinous acid;
2. in accordance with the method for claim 1, it is characterized in that the carbonization calcium hydroxide suspension is at 4-13% through slag removal and purification, weight concentration.
3. in accordance with the method for claim 1, it is characterized in that the carbon dioxide of feeding is lime calcining generation kiln gas, the wherein CO through water washing cleaning
2Content is at 20--30%.
4. in accordance with the method for claim 1, it is characterized in that, add crystal control agent in calcium hydroxide suspension, its crystal control agent is the mixture that carbohydrate and vitriol are formed, and add-on is for generating the 0.5--8% of lime carbonate;
Sugar is polysaccharide or monose: sucrose, lactose, glucose, and vitriol is: Tai-Ace S 150, zinc sulfate, ammonium sulfate etc.; Sugar is 0.1-10 with the ratio of vitriol, and additional proportion is adjusted according to the purposes difference of the nm-class active calcium carbonate that generates.
5. in accordance with the method for claim 1, it is characterized in that its carbonization process is to carry out in the carbonating tower that band stirs, carbonization temperature is at 15 ℃--and 45 ℃.
6. in accordance with the method for claim 1, it is characterized in that, the treatment agent that surface activation process is used is: the mixture of C atom number lipid acid and soap and boric acid fat coupling agent between 8--22, or resinate, add-on is for generating the 1.0--4.5% of lime carbonate.
The consumption ratio of lipid acid acid, sodium soap and boric acid fat coupling agent is between the 0.1---10, adjusts according to the different purposes of the nm-class active calcium carbonate that generates.
7. in accordance with the method for claim 6, it is characterized in that when adopting resinous acid as treatment agent, resinous acid saponification liquid added after 1.5 hours, added Tai-Ace S 150 or solution of zinc sulfate that concentration is 5-20% again, handled 1 hour again, filtered then.
8. in accordance with the method for claim 6, it is characterized in that water soluble borate fat coupling agent is SBW-3, SBW-1.
9. in accordance with the method for claim 6, its special type is, treatment agent is to be made into to concentration is that the aqueous solution of 5-30% adds later on, and temperature is at the 70-100 degree.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100888598A CN101108741A (en) | 2006-07-21 | 2006-07-21 | Industrial process for preparing nm-class active calcium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100888598A CN101108741A (en) | 2006-07-21 | 2006-07-21 | Industrial process for preparing nm-class active calcium carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101108741A true CN101108741A (en) | 2008-01-23 |
Family
ID=39041036
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006100888598A Pending CN101108741A (en) | 2006-07-21 | 2006-07-21 | Industrial process for preparing nm-class active calcium carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101108741A (en) |
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863503A (en) * | 2010-06-22 | 2010-10-20 | 恩平市燕华化工实业有限公司 | Preparation method of nanometer calcium carbonate applied to top-grade silicone adhesive |
| CN101967000A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Method for preparing high-solid-content and low-viscosity suspended nano calcium carbonate slurry and re-suspended nano calcium carbonate power |
| CN101967308A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Method for preparing nano calcium carbonate for high-temperature resistant polymers |
| CN101531391B (en) * | 2009-04-16 | 2011-05-18 | 芜湖卓越纳米新材料有限公司 | Method for industrially preparing nanometer calcium carbonate for solvent type ink addition agent |
| CN102674425A (en) * | 2012-05-19 | 2012-09-19 | 祁阳建明化工有限责任公司 | Production technique of nano calcium carbonate by normal temperature method |
| CN102702795A (en) * | 2012-05-02 | 2012-10-03 | 石家庄市三兴钙业有限公司 | Preparation method of special nano calcium carbonate for polyurethane adhesives |
| CN102732065A (en) * | 2011-04-15 | 2012-10-17 | 池州凯尔特纳米科技有限公司 | Preparation method of PVC special-purpose functional filler superfine active calcium carbonate with low oil absorption |
| CN103395812A (en) * | 2013-07-11 | 2013-11-20 | 大连理工大学 | Method for controlling shape of calcium carbonate in solid carbonization process |
| CN103483874A (en) * | 2013-09-29 | 2014-01-01 | 昆山市华浦塑业有限公司 | Method for modifying nano calcium carbonate by using boric acid ester and preparation method of PVC (polyvinyl chloride) plastic |
| CN104016391A (en) * | 2014-04-10 | 2014-09-03 | 连州市凯恩斯纳米材料有限公司 | Method for preparing nanometer calcium carbonate for organic silicone electronic sealant by adopting continuous carbonization device |
| CN104263014A (en) * | 2014-06-17 | 2015-01-07 | 池州市大恒生化有限公司 | Preparing method of high-purity active calcium carbonate used for coating |
| CN104497633A (en) * | 2014-11-25 | 2015-04-08 | 广西华纳新材料科技有限公司 | Nano calcium carbonate surface treatment method |
| CN106186022A (en) * | 2015-05-05 | 2016-12-07 | 上海华明高技术（集团）有限公司 | Low alkalinity super-fine active calcium carbide and preparation method thereof |
| CN107459841A (en) * | 2017-08-10 | 2017-12-12 | 青阳县永诚钙业有限责任公司 | A kind of preparation method of modified purity calcium carbonate |
| CN107555461A (en) * | 2017-09-30 | 2018-01-09 | 广西华洋矿源材料有限公司 | A kind of Nano calcium carbonate dedicated preparation method of plastics |
| CN107814404A (en) * | 2016-09-13 | 2018-03-20 | 北京化工大学 | A kind of production method of cube nano-calcium carbonate |
| CN110228986A (en) * | 2018-12-13 | 2019-09-13 | 湖北工业大学 | A method of promoting quick lime carbonization |
| CN111413332A (en) * | 2020-04-09 | 2020-07-14 | 吉林大学 | Saccharide distinguishing method based on natural pigment anthocyanin |
| CN112174183A (en) * | 2020-11-18 | 2021-01-05 | 湖北湖大天沭新能源材料工业研究设计院有限公司 | Method for preparing nano calcium carbonate by purifying and concentrating flue gas of rotary kiln |
| CN113247936A (en) * | 2021-06-25 | 2021-08-13 | 安徽前江超细粉末科技有限公司 | Method for reducing energy consumption in production of nano calcium carbonate |
| CN113307295A (en) * | 2021-06-25 | 2021-08-27 | 安徽前江超细粉末科技有限公司 | Method for producing nano calcium carbonate by using kiln gas with low carbon dioxide concentration |
| CN114231053A (en) * | 2021-11-15 | 2022-03-25 | 中科乐美科技集团有限公司 | Preparation method of needle-shaped cluster calcium carbonate-silver composite antibacterial material |
-
2006
- 2006-07-21 CN CNA2006100888598A patent/CN101108741A/en active Pending
Cited By (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531391B (en) * | 2009-04-16 | 2011-05-18 | 芜湖卓越纳米新材料有限公司 | Method for industrially preparing nanometer calcium carbonate for solvent type ink addition agent |
| CN101863503A (en) * | 2010-06-22 | 2010-10-20 | 恩平市燕华化工实业有限公司 | Preparation method of nanometer calcium carbonate applied to top-grade silicone adhesive |
| CN101967000A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Method for preparing high-solid-content and low-viscosity suspended nano calcium carbonate slurry and re-suspended nano calcium carbonate power |
| CN101967308A (en) * | 2010-07-14 | 2011-02-09 | 山东海泽纳米材料有限公司 | Method for preparing nano calcium carbonate for high-temperature resistant polymers |
| CN101967000B (en) * | 2010-07-14 | 2013-04-24 | 山东海泽纳米材料有限公司 | Method for preparing high-solid-content and low-viscosity suspended nano calcium carbonate slurry |
| CN102732065A (en) * | 2011-04-15 | 2012-10-17 | 池州凯尔特纳米科技有限公司 | Preparation method of PVC special-purpose functional filler superfine active calcium carbonate with low oil absorption |
| CN102702795A (en) * | 2012-05-02 | 2012-10-03 | 石家庄市三兴钙业有限公司 | Preparation method of special nano calcium carbonate for polyurethane adhesives |
| CN102674425A (en) * | 2012-05-19 | 2012-09-19 | 祁阳建明化工有限责任公司 | Production technique of nano calcium carbonate by normal temperature method |
| CN103395812A (en) * | 2013-07-11 | 2013-11-20 | 大连理工大学 | Method for controlling shape of calcium carbonate in solid carbonization process |
| CN103483874A (en) * | 2013-09-29 | 2014-01-01 | 昆山市华浦塑业有限公司 | Method for modifying nano calcium carbonate by using boric acid ester and preparation method of PVC (polyvinyl chloride) plastic |
| CN104016391A (en) * | 2014-04-10 | 2014-09-03 | 连州市凯恩斯纳米材料有限公司 | Method for preparing nanometer calcium carbonate for organic silicone electronic sealant by adopting continuous carbonization device |
| CN104263014A (en) * | 2014-06-17 | 2015-01-07 | 池州市大恒生化有限公司 | Preparing method of high-purity active calcium carbonate used for coating |
| CN104497633A (en) * | 2014-11-25 | 2015-04-08 | 广西华纳新材料科技有限公司 | Nano calcium carbonate surface treatment method |
| CN104497633B (en) * | 2014-11-25 | 2017-04-19 | 广西华纳新材料科技有限公司 | Nano calcium carbonate surface treatment method |
| CN106186022A (en) * | 2015-05-05 | 2016-12-07 | 上海华明高技术（集团）有限公司 | Low alkalinity super-fine active calcium carbide and preparation method thereof |
| CN107814404A (en) * | 2016-09-13 | 2018-03-20 | 北京化工大学 | A kind of production method of cube nano-calcium carbonate |
| CN107814404B (en) * | 2016-09-13 | 2019-06-21 | 北京化工大学 | A kind of production method of cube nanometer calcium carbonate |
| CN107459841A (en) * | 2017-08-10 | 2017-12-12 | 青阳县永诚钙业有限责任公司 | A kind of preparation method of modified purity calcium carbonate |
| CN107555461A (en) * | 2017-09-30 | 2018-01-09 | 广西华洋矿源材料有限公司 | A kind of Nano calcium carbonate dedicated preparation method of plastics |
| CN110228986A (en) * | 2018-12-13 | 2019-09-13 | 湖北工业大学 | A method of promoting quick lime carbonization |
| CN111413332A (en) * | 2020-04-09 | 2020-07-14 | 吉林大学 | Saccharide distinguishing method based on natural pigment anthocyanin |
| CN112174183A (en) * | 2020-11-18 | 2021-01-05 | 湖北湖大天沭新能源材料工业研究设计院有限公司 | Method for preparing nano calcium carbonate by purifying and concentrating flue gas of rotary kiln |
| CN113247936A (en) * | 2021-06-25 | 2021-08-13 | 安徽前江超细粉末科技有限公司 | Method for reducing energy consumption in production of nano calcium carbonate |
| CN113307295A (en) * | 2021-06-25 | 2021-08-27 | 安徽前江超细粉末科技有限公司 | Method for producing nano calcium carbonate by using kiln gas with low carbon dioxide concentration |
| CN114231053A (en) * | 2021-11-15 | 2022-03-25 | 中科乐美科技集团有限公司 | Preparation method of needle-shaped cluster calcium carbonate-silver composite antibacterial material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101108741A (en) | Industrial process for preparing nm-class active calcium carbonate | |
| CN100455515C (en) | Method for preparing nano calcium carbonate particle | |
| CN101774623B (en) | Industrial preparation method of rice-shaped ultra-fine activated calcium carbonate | |
| CN103663527B (en) | The preparation method of cubic ultra-fine calcium carbonate particle | |
| JP4537379B2 (en) | Process and apparatus for producing precipitated silica from rice husk ash | |
| CN101723429A (en) | Method for manufacturing nano calcium carbonate from high-concentration carbon dioxide industrial exhaust gases | |
| CN100567159C (en) | A kind of method for preparing superfine light calcium carbonate | |
| CN1330039A (en) | Industrial process for preparing nm-class active calcium carbonate | |
| CN102020878A (en) | Method for preparing superfine calcium carbonate compound particles | |
| CN103011226A (en) | Method for preparing nano calcium carbonate through nucleation and growth step by step | |
| CN113549341A (en) | Preparation method of core-shell type silicon dioxide coated nano calcium carbonate | |
| CN106830043A (en) | A kind of method of surface modified nano calcium carbonate | |
| CN102757075A (en) | Method for preparing calcium carbonate powders of different structures and shapes | |
| CN112811456A (en) | Nano calcium carbonate with high specific surface area and preparation method thereof | |
| CN100372773C (en) | Method for producing nano calcium carbonate particles for printing ink | |
| CN103275264A (en) | Water reducing agent capable of reducing viscosity of slurry as well as preparation method and application thereof | |
| CN113666380B (en) | Preparation method of spherical silicon dioxide | |
| CN111302347B (en) | Preparation method of high-purity large-particle-size silica sol | |
| CN105217673A (en) | A kind of preparation method of high thixotropic silicone adhesive special-purpose nanometer activated Calcium carbonate | |
| CN102453101A (en) | Method for preparing starch derivative | |
| CN102807485B (en) | Composite cobalt salt bonding promoter and preparation method thereof | |
| US4629508A (en) | Process for forming hydrated calcium silicate products | |
| CN110965122B (en) | Preparation method of layered octahedral aragonite crystal and obtained product | |
| CN113830782A (en) | Method for preparing 4A zeolite by kaolin crucible melting method | |
| CN110156054B (en) | Preparation method of rhombohedral anhydrous magnesium carbonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20080123 |