SE509300C2 - Cationically dispersed aluminum hydroxide slurries - Google Patents

Cationically dispersed aluminum hydroxide slurries

Info

Publication number
SE509300C2
SE509300C2 SE9600238A SE9600238A SE509300C2 SE 509300 C2 SE509300 C2 SE 509300C2 SE 9600238 A SE9600238 A SE 9600238A SE 9600238 A SE9600238 A SE 9600238A SE 509300 C2 SE509300 C2 SE 509300C2
Authority
SE
Sweden
Prior art keywords
pac
weight
cationic
aluminum hydroxide
dicyandiamide
Prior art date
Application number
SE9600238A
Other languages
Swedish (sv)
Other versions
SE9600238D0 (en
SE9600238L (en
Inventor
Hermann Pangerl
Benedikt Hammer
Original Assignee
Sueddeutsche Kalkstickstoff
Prechel Gmbh
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sueddeutsche Kalkstickstoff, Prechel Gmbh filed Critical Sueddeutsche Kalkstickstoff
Publication of SE9600238D0 publication Critical patent/SE9600238D0/en
Publication of SE9600238L publication Critical patent/SE9600238L/en
Publication of SE509300C2 publication Critical patent/SE509300C2/en

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/021After-treatment of oxides or hydroxides
    • C01F7/026Making or stabilising dispersions
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00Pigment pastes, e.g. for mixing in paints
    • C09D17/004Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/22Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Medicinal Chemistry (AREA)
  • Materials Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Wood Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
  • Colloid Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

Cationically dispersed Al(OH), suspensions with a high solids content, contg. 0.1-3.0 wt.% of a dispersant consisting of poly-aluminium hydroxide-chloride (PAC) and/or mixts. of PAC with cationic polymers and/or co-condensation prods. of PAC and cationic dicyandiamide resin. Pref. the PAC is prepd. in situ by adding AlCl3 and/or HCl to the Al hydroxide suspension. Pref. PAC has an Al2O3 content of 5-25 wt.%. Suitable cationic polymers (CP) are polyethyleneimine, polydiallyldimethylammonium chloride and dicyandiamide (DCD) resins, with a wt. ratio of (PAC):(CP = (30:70)-(95:5). Co-condensates of PAC and cationic DCD resin have a mole ratio of (DCD):(Al) - (1:15)-(1:2).

Description

509 som 2 slamningens totala vikt. Medan aluminiumhydroxid i pulverforrn redan vid halter om 30 viktprocent i vatten bildar en pasta som inte går att röra om utan tillsatsen enligt upp- ñnningen, kan man med tillsatsen enligt uppfinningen framställa lågviskösa aluminium- hydroxiduppslamningar med en halt fasta partiklar om 60 viktprocent eller mera. 509 as 2 the total weight of the slurry. While aluminum hydroxide in powder form already at concentrations of 30% by weight in water forms a paste which can not be stirred without the additive according to the invention, the additive according to the invention can produce low-viscosity aluminum hydroxide slurries with a solids content of 60% by weight or more.

Inom ramen för föreliggande uppfmning är det också möjligt, att framställa PAC interrnediärt i aluminiumhydroxiduppslamningen, vilket är möjligt mycket enkelt genom tillsats av bestämda mängder saltsyra och/eller aluminiumklorid (AlCl3).Within the scope of the present invention, it is also possible to produce PAC internally in the aluminum hydroxide slurry, which is possible very simply by adding certain amounts of hydrochloric acid and / or aluminum chloride (AlCl 3).

PAC, som lämpligen har en Al2O3-halt om 5 till 25 viktprocent, kan användas antingen ensamt eller i kombination med katjoniska polymerer. Som katjoniska polymerer kan härvid lämpligen användas polyetylenimin (Polyminø SK från BASF), polydiallyldime- tylammoniumklorid (Polydadmacø 570 från SNF Floerger) eller katjoniska dicyandiamid- harts (Melflockø C3 från SKW Trostberg AG). Dessa katjoniska dicyandiamidharts respektive deras framställning beskrivs t ex i DE-OS 35 00 408.PAC, which suitably has an Al 2 O 3 content of 5 to 25% by weight, can be used either alone or in combination with cationic polymers. As cationic polymers, polyethyleneimine (Polyminø SK from BASF), polydiallyldimethylammonium chloride (Polydadmacø 570 from SNF Floerger) or cationic dicyandiamide resin (Mel fl ockø C3 from SKW Trostberg AG) can be suitably used. These cationic dicyandiamide resins and their preparation are described, for example, in DE-OS 35 00 408.

De bägge komponenterna PAC och katjoniska polymerer i dessa blandningar kan visserligen varieras inom vida gränser, men det har dock visat sig särskilt lämpligt att använda PAC och den katjoniska polymeren i ett viktförhållande om 30:70 till 9525.Although the two components PAC and cationic polymers in these mixtures can be varied within wide limits, it has been found to be particularly suitable to use PAC and the cationic polymer in a weight ratio of 30:70 to 9525.

Inom ramen för föreliggande uppfmning är det även möjligt, att använda motsva-_ rande samkondensationsprodukt i stället för blandningen av PAC och katjoniskt dicyandi- amidharts. Dessa samkondensationsprodukter respektive deras framställning är känd genom DE-OS 37 42 764. Förhållandet mellan PAC och katjoniskt dicyandiamidharts i denna samkondensationsprodukt kan likaså variera inom vida gränser, dock är ett molför- hållande mellan dicyandiarnid och aluminium om 1:15 till 1:2 lämpligt.Within the scope of the present invention, it is also possible to use the corresponding co-condensation product instead of the mixture of PAC and cationic dicyandiamide resin. These co-condensation products and their preparation are known from DE-OS 37 42 764. The ratio of PAC to cationic dicyandiamide resin in this co-condensation product can also vary within wide limits, however a molar ratio of dicyandiarnide to aluminum of 1:15 to 1: 2 is suitable. .

Framställningen av aluminiumhydroxiduppslamningar enligt uppfinningen är relativt problemfri. Det katjoniska dispergerrnedlet kan t ex sättas till blandningsvattnet varpå den pulverforrniga aluminiumhydroxiden (lämplig partikelstorlek 1 till 2 um) inblandas. Dispergermedlet kan dock också sättas till redan fuktad aluminiumhydroxid.The production of aluminum hydroxide slurries according to the invention is relatively trouble-free. The cationic dispersant can be added, for example, to the mixing water, after which the powdered aluminum hydroxide (suitable particle size 1 to 2 μm) is mixed in. However, the dispersant can also be added to already moistened aluminum hydroxide.

Dessutom kan också en blandning av aluminiumhydroxid och dispergermedel ske med eller utan efterföljande torkning.In addition, a mixture of aluminum hydroxide and dispersant can also take place with or without subsequent drying.

Slutligen är det också möjligt, att spraytorka den uppfinningsenligt framställda aluminiumhydroxiduppslamningen och, genom tillsats av vatten, på nyttàstadkomma en uppslarnning. I samtliga fall är det möjligt att problemfritt framställa lágviskösa alumi- niumhydroxiduppslamningar med en halt fasta partiklar om 60 viktprocent eller mera.Finally, it is also possible to spray-dry the aluminum hydroxide slurry prepared according to the invention and, by adding water, to obtain a slurry in a useful manner. In all cases, it is possible to easily produce low-viscosity aluminum hydroxide slurries with a solids content of 60% by weight or more.

Följande exempel belyser uppfinningen närmare.The following examples illustrate the invention in more detail.

P33089SEOO/MI-l/MF 3 509 500 Exempel 1 (jämförande exempel) Aluminiumhydroxid med en genomsnittlig kornstorlek om 2 um sätts till 160 g vatten tills en pasta bildas, vilken inte mer kan omröras. Endast 70 g kan tillsättas (pastans halt av fasta partiklar: 30 viktprocent).Example 1 (Comparative Example) Aluminum hydroxide with an average grain size of 2 μm is added to 160 g of water until a paste is formed, which can no longer be stirred. Only 70 g can be added (paste content of solid particles: 30% by weight).

Exempel 2 (jämförande exempel) 2 g av ett dicyandiamidharts (Melflockø C3 från SKW Trostberg AG) sätts till 160 g vatten och i anslutning därmed tillsätts också aluminiumhydroxid i pulverform under omrörning. Den maximala tillsatsmängden till pastaaktig form uppgår till 175 g (halt av fasta partiklar: 52 viktprocent).Example 2 (comparative example) 2 g of a dicyandiamide resin (Mel fl ockø C3 from SKW Trostberg AG) are added to 160 g of water and in connection therewith, aluminum hydroxide in powder form is also added with stirring. The maximum amount of additive to a paste-like form is 175 g (solids content: 52% by weight).

Exempel 3 (jämförande exempel) I stället för dicyandiamidhartset enligt exempel 2 sätts 2 g polydiallyldimetylam- moniumklorid (Polydadmacø 570 från SNF Floerger) till vatten. Den halt fasta partiklar som är möjlig att uppnå i pastan ligger vid 38 viktprocent.Example 3 (Comparative Example) Instead of the dicyandiamide resin of Example 2, 2 g of polydiallyldimethylammonium chloride (Polydadmacø 570 from SNF Floerger) are added to water. The content of solid particles that can be achieved in the paste is 38% by weight.

Exempel 4 (jämförande exempel) 2 g av en polyetylenimin (Polyminø SK från BASF) tillsätts på motsvarande sätt som i exempel 2. Den halt fasta partiklar som är möjlig att uppnå i pastan ligger vid 50 viktprocent.Example 4 (comparative example) 2 g of a polyethyleneimine (Polyminø SK from BASF) are added in the same manner as in Example 2. The content of solid particles that can be obtained in the paste is 50% by weight.

Exempel 5 (jämförande exempel) 2 g av en SO-viktprocentig aluminiumsulfatlösning tillsätts, på motsvarande sätt som i exempel 2. Den halt fasta partiklar som är möjlig att uppnå i pastan ligger vid 43 viktprocent.Example 5 (Comparative Example) 2 g of an SO% by weight of aluminum sulphate solution are added, in the same way as in Example 2. The content of solid particles which can be obtained in the paste is 43% by weight.

Exempel 6 (utföringsexempel) 2 g av en samkondensationsprodukt av PAC och dicyandiamidharts (Alzofix® P9 från SKW Trostberg AG) sätts till 160 g vatten och i anslutning därmed tillsätts 240 g aluminiumhydroxidpulver under omrörning. En uppslamning med en Brookfield-viskositet om 90 mPas bildas; först efter flera dagar bildas en bottensats.Example 6 (working example) 2 g of a co-condensation product of PAC and dicyandiamide resin (Alzo fi x® P9 from SKW Trostberg AG) are added to 160 g of water and 240 g of aluminum hydroxide powder are added with stirring. A slurry with a Brookfield viscosity of 90 mPas is formed; only after fl your days a sediment is formed.

Exempel 7 (utföringsexempel) Pâ motsvarande sätt som i exempel 6 tillsätts 2 g av en PAC-lösning med en Al- halt om 9 viktprocent och en basicitet om 40. Den resulterande uppslamnipgen har en viskositet om 50 mPas och en bottensats bildas först efter att uppslamningen stått en längre tid.Example 7 (working example) In the same manner as in Example 6, 2 g of a PAC solution with an Al content of 9% by weight and a basicity of 40 are added. The resulting slurry nipgen has a viscosity of 50 mPas and a precipitate is formed only after the slurry lasted a long time.

Exempel 8 (utföringsexempel) 2 g av en blandning av 90 viktprocent av en PAC-lösning (Al-halt: 9,1 viktpro- P33089SE00/MH/MF 509 zoo 4 cent, basicitet 39) och 10 viktprocent polydiallyldirnetylammoniumklorid (Polydadmacm) tillsätts på motsvarande sätt som i exempel 6. Den resulterande uppslamningen uppvisar en viskositet om 120 mPas; efter flera dagar bildas en bottensats.Example 8 (working example) 2 g of a mixture of 90% by weight of a PAC solution (Al content: 9.1% by weight) are added to 10% by weight of polydiallyldirmethylammonium chloride (Polydadmacm). similar to Example 6. The resulting slurry has a viscosity of 120 mPas; after fl your days a precipitate forms.

Exempel 9 (utföringsexempel) 2 g av en blandning av 90 viktprocent av en PAC-lösning (Al-halt: 9,1 viktpro- cent, basicitet 40) och 10 viktprocent polyetylenimin (Polyminø SK från BASF) tillsätts på motsvarande sätt som i exempel 6. Den resulterande uppslarrmingen uppvisar en viskositet om 70 mPas; först efter flera dagar bildas en bottensats.Example 9 (working example) 2 g of a mixture of 90% by weight of a PAC solution (Al content: 9.1% by weight, basicity 40) and 10% by weight of polyethyleneimine (Polyminø SK from BASF) are added in the same manner as in Example 6. The resulting storage arm has a viscosity of 70 mPas; only after fl your days a sediment is formed.

Exempel 10 (utföringsexempel) 2 g av en SO-viktprocentig (AlCl3°6I-I2O)-lösning i vatten tillsätts på motsvarande sätt som i exempel 6. Den resulterande uppslamningen uppvisar en viskositet om 350 mPas; efter flera dagar bildas en tydlig bottensats.Example 10 (working example) 2 g of an SO% by weight (AlCl 3 ° 6I-I 2 O) solution in water are added in the same manner as in Example 6. The resulting slurry has a viscosity of 350 mPas; after fl your days a clear sediment is formed.

P3 3089SEOO/MH/MFP3 3089SEOO / MH / MF

Claims (6)

10 15 5 509 zoo Patentkrav10 15 5 509 zoo Patent claim 1. Katjoniskt dispergerade aluminiumhydroxiduppslainrtingar med hög halt av fasta partiklar, k ä n n e t e c k n a d e därav, att man, som dispergermedel, använder 0,1 till 3,0 viktprocent med avseende på uppslarnningens totala vikt polyalumi- niumhydroxiklorid (PAC) och/eller blandningar av PAC med katjoniska polymerer och/eller en samkondensationsprodukt av PAC och katjoniskt dicyandiamidharts. därav, att PACCationically dispersed aluminum hydroxide slurries with a high content of solid particles, characterized in that, as dispersant, 0.1 to 3.0% by weight is used with respect to the total weight of the slurry, polyaluminum hydroxychloride (PAC) and / or mixtures of PACs. with cationic polymers and / or a co-condensation product of PAC and cationic dicyandiamide resin. hence, that PAC 2.Uppslamningarenligtkrav1, kännetecknade framställs intermediärt i aluminiumhydroxiduppslamningen genom tillsats av aluminium- klorid (AlClg) och/eller saltsyra.2. The slurry according to claim 1, characterized is prepared intermediate in the aluminum hydroxide slurry by adding aluminum chloride (AlCl 3) and / or hydrochloric acid. 3. Uppslamningar enligt krav 1 och 2, k ä n n e t e c k n a d e därav, att PAC uppvisar en Al2O3-halt om 5 till 25 viktprocent.3. Slurries according to claims 1 and 2, characterized in that PAC has an Al 2 O 3 content of 5 to 25% by weight. 4. Uppslamningar enligt krav 1 till 3, k ä n n e t e c k n a d e därav, att man, som katjonisk polymer, använder en förening vald ur gruppen innefattande polyetyl- enimin, polydiallyldirnetylarnrnoniumklorid och dicyandiamidharts.Sluices according to claims 1 to 3, characterized in that, as the cationic polymer, a compound selected from the group comprising polyethyleneimine, polydiallyldirmethylnonium chloride and dicyandiamide resin is used. 5. Uppslamningar enligt krav 1 till 4, k ä n n e t e c k n a d e därav, att viktförhâllandet PAC till katjonisk polymer uppgår till 30:70 till 95:5.5. Slurries according to claims 1 to 4, characterized in that the weight ratio of PAC to cationic polymer amounts to 30:70 to 95: 5. 6. Uppslamningar enligt krav 1 till 4, k ä n n e t e c k n a d e därav, att sarnkondensationsprodukten av PAC och katjoniskt dicyandiamidharts uppvisar ett molförhâllande mellan dicyandiamid och aluminium om 1:15 till 1:2. P33089SEOO/MH/MFSlurries according to claims 1 to 4, characterized in that the co-condensation product of PAC and cationic dicyandiamide resin has a molar ratio of dicyandiamide to aluminum of 1:15 to 1: 2. P33089SEOO / MH / MF
SE9600238A 1995-02-02 1996-01-23 Cationically dispersed aluminum hydroxide slurries SE509300C2 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19503265 1995-02-02

Publications (3)

Publication Number Publication Date
SE9600238D0 SE9600238D0 (en) 1996-01-23
SE9600238L SE9600238L (en) 1996-08-03
SE509300C2 true SE509300C2 (en) 1999-01-11

Family

ID=7752924

Family Applications (1)

Application Number Title Priority Date Filing Date
SE9600238A SE509300C2 (en) 1995-02-02 1996-01-23 Cationically dispersed aluminum hydroxide slurries

Country Status (5)

Country Link
DE (1) DE19603584A1 (en)
FI (1) FI960468A (en)
FR (1) FR2730224B1 (en)
SE (1) SE509300C2 (en)
ZA (1) ZA96833B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005059960A1 (en) * 2005-12-15 2007-06-28 Degussa Gmbh Highly filled transition alumina-containing dispersion
DE102005059961A1 (en) * 2005-12-15 2007-06-28 Degussa Gmbh Highly filled alumina-containing dispersions

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2999790A (en) * 1959-08-24 1961-09-12 Sterling Drug Inc Stable aluminum hydroxide suspension
SE7905972L (en) * 1979-07-09 1981-01-10 Haessle Ab PROCEDURE FOR THE PREPARATION OF Gastric Acid-Neutralizing Agents, Gastric Acid-Neutralizing Agents, AND METHOD OF TREATING HYPERACIDITY AND RELATED DISEASE CONDITIONS
JPS62286925A (en) * 1986-06-06 1987-12-12 Terumo Corp Aluminum hydroxide gel composition
DE3730833A1 (en) * 1987-09-14 1989-03-23 Nicolaus Md Papier CATIONICALLY PIGMENT DISPERSION AND STRIP COLOR
JPH01111439A (en) * 1987-10-26 1989-04-28 Nippon Shokubai Kagaku Kogyo Co Ltd Preparation of aluminum hydroxide dispersed aqueous suspension
DE3742764A1 (en) * 1987-12-17 1989-06-29 Sueddeutsche Kalkstickstoff FLOCKING AND / OR FIXING AGENTS FOR PAPER SIZING

Also Published As

Publication number Publication date
SE9600238D0 (en) 1996-01-23
FR2730224A1 (en) 1996-08-09
DE19603584A1 (en) 1996-08-08
FI960468A0 (en) 1996-02-01
FI960468A (en) 1996-08-03
FR2730224B1 (en) 1998-01-30
SE9600238L (en) 1996-08-03
ZA96833B (en) 1996-08-13

Similar Documents

Publication Publication Date Title
CN101300292B (en) Process for producing ultrafine powders based on polyamides,ultrafine polyamide powders and their use
US3975496A (en) Process for settling red mud in the digestion of bauxite
RU2016121400A (en) METHOD FOR PRODUCING SUSPENSION WITH HIGH CONTENT OF SOLID PIGMENT PARTICLES, INCLUDING A DISPERSANT SUBSTANCE BASED ON CARBOXYMETHYLL CELLULOSE
TW502048B (en) Spray-dried polymer compositions and methods
SE446969B (en) WAY TO MAKE A FLOCKING AGENT
JPS5831211B2 (en) Rapid dispersion method for aqueous suspensions
JPH0364373A (en) Highly concentrated aqueous suspension of inorganic material and/or filler and/or pigment
US4883537A (en) Aqueous suspension of carboxymethylcellulose
CN104478238B (en) A kind of bentonite-based mineral gel and preparation method thereof
US5487777A (en) Stable CMC slurry
SE509300C2 (en) Cationically dispersed aluminum hydroxide slurries
SE409814B (en) WATERWATERABLE, WATER-FREE COMPOSITION THAT HAS EXCELLENT WETABILITY PROPERTIES FOR THE PROVISION OF DENTAL BINDER POWDER, TOOTH PASTE AND VAGINAL POWDER SPRAY
JPH06157670A (en) Method of synthesizing oligomer vinyl amine
US3467608A (en) Cationic starch compositions and a method of preparation
CN103910423A (en) Polysilicic acid modified melamine coagulant for paint fog and preparation method thereof
AU2004226986A1 (en) Storage-stable particle composition of polysaccharides and/or polysaccharide derivatives and at least one synthetic polymer, a process for production thereof and use in thereof in construction material mixtures
CA2995491C (en) Method for producing magnesium aluminate spinels
US6559301B1 (en) Dispersing agent
WO1993024582A1 (en) Method of gluing wood-based products
ATE280812T1 (en) AQUEOUS COATING COMPOSITIONS
TWI293967B (en) Biopolymere dispersable et a hydratation rapide
CN113881227B (en) Ultraviolet-resistant polyether sulfone resin and preparation method thereof
JP2004002692A (en) Water-soluble polymer having lowered molecular weight, its preparation process, and method of using it
JPS6028818A (en) Dispersing agent for calcium carbonate
GB1593582A (en) Process for the production of viscosity-stable aqueous dispersions for paper coating compositions

Legal Events

Date Code Title Description
NUG Patent has lapsed

Ref document number: 9600238-1

Format of ref document f/p: F