DE1028262B - Process for improving the flowability of phosphors - Google Patents
Process for improving the flowability of phosphorsInfo
- Publication number
- DE1028262B DE1028262B DEA19656A DEA0019656A DE1028262B DE 1028262 B DE1028262 B DE 1028262B DE A19656 A DEA19656 A DE A19656A DE A0019656 A DEA0019656 A DE A0019656A DE 1028262 B DE1028262 B DE 1028262B
- Authority
- DE
- Germany
- Prior art keywords
- phosphors
- silica
- solution
- flowability
- phosphor
- 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
- 238000000034 method Methods 0.000 title claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 39
- 239000000377 silicon dioxide Substances 0.000 claims description 19
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims 2
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 239000000243 solution Substances 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 235000019353 potassium silicate Nutrition 0.000 description 6
- 239000004111 Potassium silicate Substances 0.000 description 4
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 4
- 229910052913 potassium silicate Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- CBKLNOZTOBKSDK-UHFFFAOYSA-L beryllium;diformate Chemical compound [Be+2].[O-]C=O.[O-]C=O CBKLNOZTOBKSDK-UHFFFAOYSA-L 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
- C09K11/72—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus also containing halogen, e.g. halophosphates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Description
Verfahren zur Verbesserung der Rieselfähigkeit von Leuchtstoffen Leuchtstoffe, die nach dem Einstäub- oder Perlverfahren in Leuchtstoffröhren eingebracht werden. sollen, müssen, um eine brauchbare, gleichmäßige Schicht erzielen zu können, von riesliger Beschaffenheit sein.Process to improve the flowability of phosphors Phosphors, which are introduced into fluorescent tubes using the dusting or beading process. should, in order to be able to achieve a usable, even layer, of be gigantic.
Im allgemeinen fallen die Leuchtstoffe aber als feinkörniges, klumpiges Material an und werden dann nach den verschiedensten bekannten Methoden nachbehandelt. Diese bisher bekannten Methoden haben aber ihre Nachteile. Zum Beispiel wurden bisher sämtliche Silicatleuchtstoffe durch Kochen mit verdünnten alkalischen Lösungen wie Natrium- oder Kaliumcarbonat rieselfähig gemacht. Es ist bekannt, daß hierdurch die Lebensdauer dieser Leuchtstoffe vermindert wird. Vor allen Dingen ist auch die heiße Behandlung in der Technik mit Schwierigkeiten verbunden.In general, however, the phosphors fall as fine-grained, lumpy ones Material and are then post-treated using a wide variety of known methods. However, these previously known methods have their disadvantages. For example, so far all silicate phosphors by boiling with dilute alkaline solutions such as Made free-flowing sodium or potassium carbonate. It is known that as a result the life of these phosphors is reduced. Above all else is that hot treatment in technology associated with difficulties.
Auch die Behandlung der Wolframate mit Ammonchlorid- oder Ammonffluoridlösung ist umständlich und setzt die Lebensdauer der Leuchtstoffe herab.Also the treatment of the tungstates with ammonium chloride or ammonium fluoride solution is cumbersome and reduces the lifespan of the phosphors.
Die Behandlung der Leuchtstoffe mit einer Berylliumformiatlösung geschieht auch in der Siedehitze. Außerdem sei auch auf die Giftigkeit des Berylliums hingewiesen. Es ist weiterhin ein Verfahren bekannt, bei dem das Leuchtstoffpulver mit einer warmen, verdünnten Lösung von Kaliumsilicat versetzt und längere Zeit durchgerührt wird. Die Kaliumsilicatlösung wird vorher mit Essigsäure angesäuert. Nach diesem Verfahren wird die Kieselsäure anschließend mit Ammoniak auf das Leuchtstoffpulver aufgefällt. Das Kaliumsilicat oder das verwendete Kaliwasserglas, das für die Behandlung verwendet wird, ist nie rein, da diese Stoffe aus ihrer Herstellung meist mit Schwermetallspuren behaftet sind. Durch die Behandlung des Leuchtstoffpulvers mit Wasserglas werden daher Schwermetallspuren eingeschleppt, die schon in geringster Menge den Leuchtstoffen schädlich sind und deren Emission stark herabsetzen.The phosphors are treated with a beryllium formate solution even at the boiling point. The toxicity of beryllium should also be noted. It is also known a method in which the phosphor powder with a added warm, dilute solution of potassium silicate and stirred for a long time will. The potassium silicate solution is previously acidified with acetic acid. After this In the process, the silica is then applied to the phosphor powder with ammonia noticed. The potassium silicate or potassium silicate used for the treatment is never pure, as these substances usually contain traces of heavy metals from their manufacture are afflicted. By treating the fluorescent powder with water glass therefore traces of heavy metals have been brought in, which are already present in the smallest quantities of the phosphors are harmful and greatly reduce their emissions.
Nach einem anderen Verfahren werden die Leuchtstoffpulver mit einer kolloidalen Lösung von Kieselsäure in Alkohol behandelt. Die Kolloidlösung wird durch Hydrolyse von Siliconestern hergestellt, also von organischen Kieselsäureverbindungen. Für die Technik ist diese Herstellung kaum durchführbar, da sie äußerst zeitraubend ist und dabei nur Lösungen erhalten werden, deren Kieselsäuregehalt 0,51/o nicht übersteigt. Diese Konzentration ist aber für die Verbesserung der Rieselfähigkeit von Leuchtstoffpulvern, z. B. Halophosphaten, zu schwach. Man braucht hierzu wesentlich höhere Konzentrationen kolloider Kieselsäure.Another method is to use a treated with colloidal solution of silica in alcohol. The colloid solution will produced by hydrolysis of silicone esters, i.e. organic silicic acid compounds. This production is hardly feasible for the technology because it is extremely time-consuming and only solutions are obtained with a silica content of 0.51 / o exceeds. This concentration is, however, for improving the flowability of fluorescent powders, e.g. B. halophosphates, too weak. One needs essential for this higher concentrations of colloidal silica.
Die Erfindung besteht darin, daß das Leuchtstoffpulver mit einer höchstgereinigten, praktisch neutralen Kieselsäurelösung behandelt und die Kieselsäure mittels Ammoniak auf den Leuchtstoff aufgefällt wird. Die Kieselsäurelösung soll dabei einen Kieselsäuregehalt zwischen 0,3 und 10% aufweisen.The invention consists in that the phosphor powder with a highly purified, treated practically neutral silica solution and the silica using ammonia is noticed on the phosphor. The silica solution should have a silica content between 0.3 and 10%.
Beispiel 1000 g Halophosphatleuchtstoffpulver werden in 4000 ccm destillierten Wassers aufgeschlämmt und mit 250 ccm Kieselsäurelösung versetzt. Während des Rührens wird die Kieselsäure durch 25 ccm Ammoniak (konzentriert) auf den Leuchtstoff aufgefällt. Nach 1stündigem Rühren wird der Leuchtstoff abgenutscht und mit destilliertem Wasser kurz ausgewaschen.Example 1000 g of halophosphate phosphor powder are distilled in 4000 ccm Slurried water and mixed with 250 ccm silica solution. While stirring the silica is precipitated onto the phosphor by means of 25 cc ammonia (concentrated). After stirring for 1 hour, the phosphor is suction filtered and washed with distilled water briefly washed out.
Bei den meisten so behandelten Leuchtstoffen ist gleichzeitig eine Steigerung der Leuchtintensität zu verzeichnen.In most of the phosphors treated in this way, there is one at the same time Increase in luminous intensity to be recorded.
Die neutrale Kieselsäurelösung kann wie folgt hergestellt werden: 5 kg Natronwasserglas (DAB 6) werden mit der 10fachen Menge destillierten Wassers verdünnt. Durch Zugabe von konzentrierter Salzsäure wird unter starkem Rühren die gesamte Kieselsäure ausgefällt. Diese stark wasserhaltige Kieselsäure wird nun mit destilliertem Wasser im sauren Gebiet weitestgehend eisenfrei gewaschen. Das Waschwasser darf mit Ammonrhodanid keine Rotfärbung mehr ergeben. Nach dem letzten Waschen wird das überstehende Wasser dekantiert und die wasserhaltige Kieselsäure mit 10%iger Natronlauge wieder in Lösung gebracht. Diese alkalische Kieselsäurelösung wird auf das Doppelte verdünnt und auf 10° C oder darunter abgekühlt. Danach wird so viel verdünnte Salzsäure zugesetzt, daß der pH-Wert zwischen 6 und 7 liegt. Von dieser praktisch neutralen Kieselsäurelösung wird eine Kieselsäurebestimmung gemächt, damit sie durch Verdünnen mit Wasser =auf den bevorzugten Prozentgehalt eingestellt werden kann.,The neutral silica solution can be prepared as follows: 5 kg of soda water glass (DAB 6) are mixed with 10 times the amount of distilled water diluted. By adding concentrated hydrochloric acid, while stirring vigorously, the all of the silica precipitated. This highly water-containing silica is now with washed iron-free as far as possible with distilled water in the acidic area. The wash water must not turn red with ammonrhodanide. After the last wash it will the supernatant water is decanted and the water-containing silica with 10% Sodium hydroxide solution brought back into solution. This alkaline silica solution is on diluted twice and cooled to 10 ° C or below. After that there will be so much Dilute hydrochloric acid added so that the pH is between 6 and 7. Of this practically neutral silica solution is a silica determination made so by diluting with water = to the preferred percentage can be set.,
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEA19656A DE1028262B (en) | 1954-02-09 | 1954-02-09 | Process for improving the flowability of phosphors |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEA19656A DE1028262B (en) | 1954-02-09 | 1954-02-09 | Process for improving the flowability of phosphors |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1028262B true DE1028262B (en) | 1958-04-17 |
Family
ID=6924497
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEA19656A Pending DE1028262B (en) | 1954-02-09 | 1954-02-09 | Process for improving the flowability of phosphors |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1028262B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1184009B (en) * | 1963-03-15 | 1964-12-23 | Pintsch Licht G M B H | Fluorescent lamp with argon as filling gas |
| DE2944943A1 (en) * | 1978-11-09 | 1980-05-14 | Tokyo Shibaura Electric Co | METHOD FOR TREATMENT OF LUMINOUS PARTICLES |
| DE3003699A1 (en) * | 1979-02-02 | 1980-08-07 | Tokyo Shibaura Electric Co | FLUORESCENT COATED WITH A FILTER |
| WO1991010715A1 (en) * | 1990-01-22 | 1991-07-25 | Gte Laboratories Incorporated | Phosphors with improved lumen output and lamps made therefrom |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB511038A (en) * | 1938-02-08 | 1939-08-08 | Ronald Puleston | Method of rendering a powder free flowing |
| GB521099A (en) * | 1938-11-07 | 1940-05-13 | British Thomson Houston Co Ltd | Improvements in and relating to luminescent powders, and methods of manufacturing the same |
-
1954
- 1954-02-09 DE DEA19656A patent/DE1028262B/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB511038A (en) * | 1938-02-08 | 1939-08-08 | Ronald Puleston | Method of rendering a powder free flowing |
| GB521099A (en) * | 1938-11-07 | 1940-05-13 | British Thomson Houston Co Ltd | Improvements in and relating to luminescent powders, and methods of manufacturing the same |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1184009B (en) * | 1963-03-15 | 1964-12-23 | Pintsch Licht G M B H | Fluorescent lamp with argon as filling gas |
| DE2944943A1 (en) * | 1978-11-09 | 1980-05-14 | Tokyo Shibaura Electric Co | METHOD FOR TREATMENT OF LUMINOUS PARTICLES |
| DE3003699A1 (en) * | 1979-02-02 | 1980-08-07 | Tokyo Shibaura Electric Co | FLUORESCENT COATED WITH A FILTER |
| WO1991010715A1 (en) * | 1990-01-22 | 1991-07-25 | Gte Laboratories Incorporated | Phosphors with improved lumen output and lamps made therefrom |
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