DE4039014A1 - Prepn. of agent for redn. of calcium sulphate content of soln. - by heating ash contg. aluminosilicate with alkali hydroxide soln. and sepg. solid - Google Patents
Prepn. of agent for redn. of calcium sulphate content of soln. - by heating ash contg. aluminosilicate with alkali hydroxide soln. and sepg. solidInfo
- Publication number
- DE4039014A1 DE4039014A1 DE19904039014 DE4039014A DE4039014A1 DE 4039014 A1 DE4039014 A1 DE 4039014A1 DE 19904039014 DE19904039014 DE 19904039014 DE 4039014 A DE4039014 A DE 4039014A DE 4039014 A1 DE4039014 A1 DE 4039014A1
- Authority
- DE
- Germany
- Prior art keywords
- solid
- soln
- ash
- alkali hydroxide
- hydroxide solution
- 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
- 229910001854 alkali hydroxide Inorganic materials 0.000 title claims abstract description 12
- 150000008044 alkali metal hydroxides Chemical class 0.000 title claims abstract description 12
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 title claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 5
- 229910000323 aluminium silicate Inorganic materials 0.000 title claims abstract 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract 3
- 239000007787 solid Substances 0.000 title abstract description 9
- 238000010438 heat treatment Methods 0.000 title abstract 2
- 235000011132 calcium sulphate Nutrition 0.000 title 1
- 239000001175 calcium sulphate Substances 0.000 title 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000011575 calcium Substances 0.000 claims description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000012265 solid product Substances 0.000 claims description 5
- 239000002956 ash Substances 0.000 abstract description 17
- 239000010881 fly ash Substances 0.000 abstract description 4
- 239000003077 lignite Substances 0.000 abstract description 4
- -1 sulphate ions Chemical class 0.000 abstract description 3
- 229910052925 anhydrite Inorganic materials 0.000 abstract 2
- 229910052593 corundum Inorganic materials 0.000 abstract 2
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 229910021653 sulphate ion Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 16
- 239000002351 wastewater Substances 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Processing Of Solid Wastes (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
Die Verwendung der bei der Verbrennung von fossilen festen Brennstoffen anfallenden Flugasche als Absorptionsmittel in Rauchgasreinigungsanlagen ist bekannt (DD 2 47 587). Weiterhin wird Asche zur Neutralisation von Abwässern (DD 1 48 945) oder in Verbindung mit Flockungsmitteln zur Klärung kohlegetrüb ter Wässer eingesetzt (DD 43 118).The use of solid when burning fossil Fuel fly ash as an absorbent in Flue gas cleaning systems are known (DD 2 47 587). Farther becomes ash for neutralizing waste water (DD 1 48 945) or in connection with flocculants for clarification of coal ter waters used (DD 43 118).
In DD 1 47 057 wird ein Verfahren zur Gewinnung von Aluminium oxid aus Braunkohlenfilteraschen beschrieben. Aus der Lite ratur ist ebenfalls bekannt, daß Asche in Verbindung mit Salzsäure zur Gewinnung von Aluminiumverbindungen bei der Herstellung von Zeolithen genutzt werden kann.DD 1 47 057 describes a process for the production of aluminum oxide from brown coal filter ash. From the lite It is also known that ash is associated with Hydrochloric acid for the production of aluminum compounds in the Production of zeolites can be used.
Um gelöste Anionen in wäßrigen Lösungen, z. B. Sulfatablauf konzentrationen, zu verringern, wird in der Fachliteratur die Verwendung von Kalk/Calciumaluminatmonosulfathydrat beschrieben.To dissolved anions in aqueous solutions, e.g. B. sulfate drain concentrations, to decrease, is in the specialist literature the use of lime / calcium aluminate monosulfate hydrate described.
Es ist Stand der Technik, Asche als Wertstoff für verschie dene Zwecke einzusetzen. Zur Senkung der Sulfationenkonzen tration in Lösungen kann man speziell hergestellte chemische Verbindungen verwenden. Der Einsatz bzw. die Aktivierung von Asche zu diesem Zweck ist bisher noch nicht bekannt.It is state of the art to use ash as a valuable material for various purposes use their purposes. To reduce the sulfate ion concentration tration in solutions you can use specially manufactured chemical Use connections. The use or activation of Ashes for this purpose are not yet known.
Aufgabe der Erfindung ist es, mit einfachen Mitteln den Calcium- und Sulfationengehalt von Lösungen zu verringern und damit Maßnahmen des Umweltschutzes zu unterstützen.The object of the invention is the simple Reduce the calcium and sulfate ion content of solutions and thus support environmental protection measures.
Die genannte Aufgabe wird dadurch gelöst, daß alumosilikat haltige Asche mit einer Alkalihydroxidlösung versetzt, erwärmt und nach einer Reaktionszeit von 5 bis 30 Minuten die Lösung einer Fest-Flüssig-Trennung unterzogen wird, wobei die Anwendung des erhaltenen Mittels so erfolgt, daß das aktivierte Festprodukt der calcium- und/oder sulfat ionenhaltigen Lösung im Verhältnis 5 bis 30 Gramm Trocken substanz auf 1 Liter gesättigte Calciumsulfatlösung zuge setzt wird und nach einer Reaktionszeit von 1 bis 2 Stunden eine Fest-Flüssig-Trennung erfolgt.The above object is achieved in that alumosilicate containing ash with an alkali hydroxide solution, warmed and after a reaction time of 5 to 30 minutes the solution is subjected to a solid-liquid separation, the application of the agent obtained is such that the activated solid product of calcium and / or sulfate ionic solution in a ratio of 5 to 30 grams dry substance added to 1 liter of saturated calcium sulfate solution is set and after a reaction time of 1 to 2 hours a solid-liquid separation takes place.
Die verwendete Asche soll einen Aluminiumoxidgehalt von größer 8% besitzen.The ash used is said to have an alumina content of own more than 8%.
Als Alkalihydroxidlösung wird 5-30%ige Natriumhydroxidlösung oder Kaliumhydroxidlösung verwendet.5-30% sodium hydroxide solution is used as the alkali hydroxide solution or potassium hydroxide solution.
Zur Erhöhung der Reaktionsgeschwindigkeit wird die mit Alkalihydroxidlösung versetzte, alumosilikathaltige Asche auf eine Temperatur größer gleich 50°C erwärmt. Vor der Fest-Flüssig-Trennung kann sie im Verhältnis 1 : 1 mit Wasser versetzt werden, um eine einfache Filtration zu ermöglichen.To increase the reaction rate with Alkali hydroxide solution containing ash containing alumosilicate heated to a temperature greater than or equal to 50 ° C. Before the Solid-liquid separation can be done in a 1: 1 ratio Water can be added for easy filtration enable.
Eine Fest-Flüssig-Trennung vor der Anwendung des Mittels ist notwendig, um die Alkalihydroxidlösung einer Wiederverwen dung zuführen zu können und sie nicht in die calcium- und/oder sulfationenhaltige Lösung einzutragen. Das bei der Fest-Flüssig-Trennung anfallende Festprodukt kann vor der Anwendung getrocknet werden.There is a solid-liquid separation before using the agent necessary to reuse the alkali hydroxide solution be able to feed them and not into the calcium and / or enter solution containing sulfate ions. That at the Solid-liquid separation resulting solid product can before Application can be dried.
Nachdem die aktivierte Asche der calcium- und/oder sulfat ionenhaltigen Lösung zugegeben wurde, erfolgt während der Reaktionszeit eine Umwandlung der gelösten Ionen. Der Anteil der Calciumionen Ca2+ verringert sich um mehr als 90% und die Sulfationenkonzentration SO4 2- um 50 bis 70%. Bei der abschließenden Fest-Flüssig-Trennung werden diese umgewan delten Ionen in einer schwer löslichen Form, hauptsächlich als Calcium-Aluminat-Sulfat-Verbindungen, mit dem Fest produkt abgeschieden. Damit kann die so behandelte Flüssig keit nach der Einstellung des erforderlichen pH-Wertes ohne Belastung der Umwelt abgeleitet werden. After the activated ash of the calcium and / or sulfate ion-containing solution has been added, the dissolved ions are converted during the reaction time. The proportion of calcium ions Ca 2+ decreases by more than 90% and the sulfate ion concentration SO 4 2- by 50 to 70%. In the final solid-liquid separation, these converted ions are separated in a poorly soluble form, mainly as calcium aluminate sulfate compounds, with the solid product. This means that the liquid treated in this way can be drained off without polluting the environment after the required pH has been set.
Ein wesentlicher, mit der Erfindung zu erzielender Vorteil besteht darin, daß die bei der Verbrennung von Braunkohle in Wärmeerzeugungsanlagen anfallende Flugasche, die mindestens zu 8% aus Aluminiumoxid besteht, als Ausgangsstoff verwendet werden kann.An essential advantage to be achieved with the invention is that when lignite is burned in Fly ash accumulating at least consists of 8% aluminum oxide, used as a starting material can be.
Ein Ausführungsbeispiel der Erfindung zur Senkung des Calciumsulfatgehaltes im Abwasser von Rauchgasentschwe felungsanlagen wird im folgenden Abschnitt beschrieben und anhand der Fig. 1 erläutert.An embodiment of the invention for reducing the calcium sulfate content in the wastewater from Rauchgasentschwe treatment plants is described in the following section and explained with reference to FIG. 1.
1 t alumosilikatreicher Flugasche einer Braunkohlenfeuerung (a) mit einem Aluminiumoxidgehalt von 20% wird mit 3-6 m3 30%iger Natronlauge (b) versetzt. Danach wird die Lösung auf 70°C erwärmt und für ca. 20 Minuten bei dieser Temperatur gehalten (c). Durch eine Fest-Flüssig-Trennung (d) wird die Restnatronlauge (e) abgeschieden, mit höher konzentrierter Natronlauge (f) zu 30%iger ergänzt und zur Aktivierung weiterer Asche wieder eingesetzt.1 t alumosilicate-rich fly ash from a lignite furnace (a) with an aluminum oxide content of 20% is mixed with 3-6 m 3 30% sodium hydroxide solution (b). The solution is then heated to 70 ° C. and kept at this temperature for about 20 minutes (c). The residual sodium hydroxide solution (e) is separated by a solid-liquid separation (d), supplemented with 30% strength sodium hydroxide solution (f) and used again to activate further ash.
Der feste Rückstand, die aktivierte Asche (g), wird dem gipshaltigen Abwasser einer Rauchgasentschwefelungsanlage (h) zugesetzt. Mit 1 t aktivierter Asche kann je nach Aluminium oxidgehalt der Rohasche der Calcium- und Sulfationengehalt in 30 bis 60 m3 gipsgesättigtem Abwasser auf 8-12 mg/l bzw. 300-700 mg/l gesenkt werden. Dazu beträgt die Reak tionszeit bei 20°C ca. 2 Stunden (i). Es bilden sich Calcium-Aluminat-Sulfate, die schwer löslich sind und deshalb mit einer Fest-Flüssig-Trennung (j) abgeschieden werden können.The solid residue, the activated ash (g), is added to the gypsum-containing waste water from a flue gas desulphurization plant (h). With 1 t activated ash, depending on the aluminum oxide content of the raw ash, the calcium and sulfate ion content in 30 to 60 m 3 of gypsum-saturated wastewater can be reduced to 8-12 mg / l or 300-700 mg / l. The reaction time at 20 ° C is approx. 2 hours (i). Calcium aluminate sulfates are formed, which are sparingly soluble and can therefore be separated with a solid-liquid separation (j).
Der abgeschiedene feste Rückstand (k), mit einer Masse von ca. 1-1,2 t, ist problemlos deponiefähig. Das Abwasser besitzt einen pH-Wert von 9 bis 11,5. Es wird durch Zumischen saurer Abwässer (l) auf den zur Einleitung in Fließgewässer (m) notwendigen pH-Wert eingestellt.The deposited solid residue (k), with a mass of approx. 1-1.2 t, can be landfilled without any problems. The sewage has a pH of 9 to 11.5. It is through Add acidic wastewater (l) to the discharge in Rivers (m) set the necessary pH.
Die Fest-Flüssig-Trennungen können mit geeigneten Apparatu ren, wie zum Beispiel Hydrozyklone, erfolgen.The solid-liquid separations can be carried out with suitable apparatus ren, such as hydrocyclones.
Claims (7)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19904039014 DE4039014C2 (en) | 1990-12-04 | 1990-12-04 | Process for the preparation and use of an agent for reducing the calcium sulfate content in solutions |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19904039014 DE4039014C2 (en) | 1990-12-04 | 1990-12-04 | Process for the preparation and use of an agent for reducing the calcium sulfate content in solutions |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| DE4039014A1 true DE4039014A1 (en) | 1992-06-11 |
| DE4039014C2 DE4039014C2 (en) | 1994-07-07 |
Family
ID=6419769
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19904039014 Expired - Fee Related DE4039014C2 (en) | 1990-12-04 | 1990-12-04 | Process for the preparation and use of an agent for reducing the calcium sulfate content in solutions |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE4039014C2 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011048135A1 (en) * | 2009-10-20 | 2011-04-28 | Solvay Sa | Process for the combined regeneration of soluble salts contained in a residue of an industrial process |
| NL2008574C2 (en) * | 2012-03-30 | 2013-10-01 | Nieuwpoort Beheer B V Van | Method for manufacturing concrete, mortar or grout using lignite fly ash and concrete, mortar or grout obtainable by said method. |
| NL2008575C2 (en) * | 2012-03-30 | 2013-10-01 | Nieuwpoort Beheer B V Van | Binder composition comprising lignite fly ash. |
| CN105692831A (en) * | 2016-02-26 | 2016-06-22 | 武汉理工大学 | Efficient slag-based inorganic phosphorous removal flocculating agent and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4642304A (en) * | 1984-05-16 | 1987-02-10 | Degussa Aktiengesellschaft | Activated carbon and process for its production |
| US4769359A (en) * | 1985-09-24 | 1988-09-06 | The British Petroleum Company P.L.C. | Process for the production of adsorbent carbon |
-
1990
- 1990-12-04 DE DE19904039014 patent/DE4039014C2/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4642304A (en) * | 1984-05-16 | 1987-02-10 | Degussa Aktiengesellschaft | Activated carbon and process for its production |
| US4769359A (en) * | 1985-09-24 | 1988-09-06 | The British Petroleum Company P.L.C. | Process for the production of adsorbent carbon |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011048135A1 (en) * | 2009-10-20 | 2011-04-28 | Solvay Sa | Process for the combined regeneration of soluble salts contained in a residue of an industrial process |
| US8906117B2 (en) | 2009-10-20 | 2014-12-09 | Solvay Sa | Process for the combined regeneration of soluble salts contained in a residue of an industrial process |
| NL2008574C2 (en) * | 2012-03-30 | 2013-10-01 | Nieuwpoort Beheer B V Van | Method for manufacturing concrete, mortar or grout using lignite fly ash and concrete, mortar or grout obtainable by said method. |
| NL2008575C2 (en) * | 2012-03-30 | 2013-10-01 | Nieuwpoort Beheer B V Van | Binder composition comprising lignite fly ash. |
| WO2013147607A1 (en) * | 2012-03-30 | 2013-10-03 | Van Nieuwpoort Beheer B.V. | Method for manufacturing concrete, mortar or grout using lignite fly ash and concrete, mortar or grout obtainable by said method |
| WO2013147608A1 (en) * | 2012-03-30 | 2013-10-03 | Van Nieuwpoort Beheer B.V. | Binder composition comprising lignite fly ash |
| CN105692831A (en) * | 2016-02-26 | 2016-06-22 | 武汉理工大学 | Efficient slag-based inorganic phosphorous removal flocculating agent and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| DE4039014C2 (en) | 1994-07-07 |
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| OP8 | Request for examination as to paragraph 44 patent law | ||
| 8122 | Nonbinding interest in granting licenses declared | ||
| D2 | Grant after examination | ||
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