NO132254B - - Google Patents
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- NO132254B NO132254B NO4972/70A NO497270A NO132254B NO 132254 B NO132254 B NO 132254B NO 4972/70 A NO4972/70 A NO 4972/70A NO 497270 A NO497270 A NO 497270A NO 132254 B NO132254 B NO 132254B
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- Prior art keywords
- phthalocyanine
- alpha
- approx
- pigment
- binder
- Prior art date
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- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000000049 pigment Substances 0.000 claims description 16
- 239000011230 binding agent Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 239000004576 sand Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 description 17
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 239000006185 dispersion Substances 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 8
- 239000000758 substrate Substances 0.000 description 7
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 239000011669 selenium Substances 0.000 description 6
- 229910052711 selenium Inorganic materials 0.000 description 6
- 230000035945 sensitivity Effects 0.000 description 6
- 238000010422 painting Methods 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- 239000000123 paper Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229920002050 silicone resin Polymers 0.000 description 3
- QKUNKVYPGIOQNP-UHFFFAOYSA-N 4,8,11,14,17,21-hexachlorotetracosane Chemical compound CCCC(Cl)CCCC(Cl)CCC(Cl)CCC(Cl)CCC(Cl)CCCC(Cl)CCC QKUNKVYPGIOQNP-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 206010034972 Photosensitivity reaction Diseases 0.000 description 2
- 229920000180 alkyd Polymers 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000005670 electromagnetic radiation Effects 0.000 description 2
- 230000036211 photosensitivity Effects 0.000 description 2
- 229920003227 poly(N-vinyl carbazole) Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000005488 sandblasting Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- KPAPHODVWOVUJL-UHFFFAOYSA-N 1-benzofuran;1h-indene Chemical compound C1=CC=C2CC=CC2=C1.C1=CC=C2OC=CC2=C1 KPAPHODVWOVUJL-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000000763 evoking effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920006287 phenoxy resin Polymers 0.000 description 1
- 239000013034 phenoxy resin Substances 0.000 description 1
- 229920002382 photo conductive polymer Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007761 roller coating Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229920000638 styrene acrylonitrile Polymers 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
- G03G5/02—Charge-receiving layers
- G03G5/04—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
- G03G5/06—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being organic
- G03G5/0664—Dyes
- G03G5/0696—Phthalocyanines
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Photoreceptors In Electrophotography (AREA)
Description
Den foreliggende oppfinnelse vedrører en fremgangsmåte til fremstilling av et fotoledende lag for en elektrofotografisk plate, hvor et ftalocyaninpigment og et bindemiddel blandes i et flytende medium. The present invention relates to a method for producing a photoconductive layer for an electrophotographic plate, where a phthalocyanine pigment and a binder are mixed in a liquid medium.
I xerografi som opprinnelig beskrevet i US-patentskrift 2.297.691, dannes et elektrostatisk latent bilde på et fotoledende, isolerende lag og fremkalles deretter ved hjelp av findelt elektroskopisk fremkallermateriale. Det fremkalte bilde kan så fikseres på plass eller overføres til et reproduksjonsark hvor det fikseres permanent. Generelt blir først det fotoledende, isolerende lag ladet for å gjøres, følsomt og eksponeres så av et lys-bilde eller annet mønster av aktiverende elektromagnetisk bestrål-ing for å utlade ladningen i de bestrålte områder. Det dannete lad-ningsmønster svarer således til det elektromagnetiske bestrålings-mønster som har truffet platen-. Dette ladningsmønster kan så, som ovenfor nevnt, fremkalles eller gjøres synlig ved på platen å på-føre et elektroskopisk eller elektrostatisk tiltrekkende, findelt, farget materiale som kalles "toner". In xerography as originally described in US Patent 2,297,691, an electrostatic latent image is formed on a photoconductive insulating layer and then developed using finely divided electroscopic developer material. The developed image can then be fixed in place or transferred to a reproduction sheet where it is permanently fixed. Generally, the photoconductive insulating layer is first charged to be made sensitive and then exposed by a light image or other pattern of activating electromagnetic radiation to discharge the charge in the irradiated areas. The resulting charge pattern thus corresponds to the electromagnetic radiation pattern that has hit the plate. This charge pattern can then, as mentioned above, be evoked or made visible by applying an electroscopic or electrostatically attractive, finely divided, colored material called "toner" to the plate.
Som beskrevet i ovennevnte US-patentskrift, kari egnete uorganiske og organiske materialer brukes for dannelse av det fotoledende, isolerende lag hvor det latente, elektrostatiske bilde dannes. Andre fotoledende materialer har tidligere vært foreslått som brukbare i liknende elektrofotografiske prosesser, for eksempel slik som i US-patentskrifter 2.357.809, 2.891.001 og 3.079.342. Noen av disse materialer er selenglass, polymerer som polyvinylkarbazol, og har-pikssuspensjoner av uorganiske, fotoledende pigmenter som for eksempel sinkoksyd og kadmiumsulfid. Selv om noen av disse materialer har vist en kommersiell anvendelse, er der visse iboende ulemper for den kommersielle anvendelse i hver av foreslåtte produkter. As described in the above-mentioned US patent, suitable inorganic and organic materials are used to form the photoconductive insulating layer where the latent electrostatic image is formed. Other photoconductive materials have previously been proposed as usable in similar electrophotographic processes, for example as in US patents 2,357,809, 2,891,001 and 3,079,342. Some of these materials are selenium glass, polymers such as polyvinylcarbazole, and resin suspensions of inorganic, photoconductive pigments such as zinc oxide and cadmium sulphide. Although some of these materials have shown commercial application, there are certain inherent disadvantages to commercial application in each of the proposed products.
Oppdagelsen av de fotoledende, isolerende egenskaper hos høy-renset selenglass har resultert i at dette materiale er blitt standard i kommersiell xerografi. Imidlertid er selenglass følsomt bare overfor bølgelengder som er kortere enn 5.800 Ångstrømenheter. Xerografiske plater laget med selen er dessuten kostbare i fremstilling da dette materiale må påføres det bærende underlag ved vakuum-pådampning under omhyggelig styrte betingelser. Dessuten er selen-glasslag metastabile og kan omkrystallisere til uvirksomme kry-stallinske former ved temperaturer bare litt i overkant av de som er fremherskende i vanlige xerografiske reproduksjonsapparater. The discovery of the photoconductive, insulating properties of highly purified selenium glass has resulted in this material becoming the standard in commercial xerography. However, selenium glass is sensitive only to wavelengths shorter than 5,800 Angstrom units. Xerographic plates made with selenium are also expensive to manufacture as this material must be applied to the supporting substrate by vacuum evaporation under carefully controlled conditions. Moreover, selenium glass layers are metastable and can recrystallize into inactive crystalline forms at temperatures only slightly in excess of those prevailing in ordinary xerographic reproduction apparatus.
Andre kjente xerografiske plater fremstilt med visse aromatiske organiske fotoledere har relativt lav følsomhet overfor lys, og dertil kommer at mesteparten av denne følsomhet ligger i det ultrafiolette område, hvilket ikke er fullt ut tilfredsstillende for bruk i vanlige elektrografiske reproduksjonsanordninger. Selv de mest følsomme organiske fotoledende polymerer mangler meget på å være tilfredsstillende for kommersielle formål. Valget av til-gjengelige materialer for bruk i aromatiske polymerplater er nat-urligvis begrenset på grunn av nødvendigheten av å velge et alle-rede fotoledende materiale. Dessuten mangler alle de ovenfornevnte xerografiske plater motstandsdyktighet mot slitasje og driftssta-bilitet spesielt ved høyere temperaturer. Other known xerographic plates made with certain aromatic organic photoconductors have relatively low sensitivity to light, and in addition most of this sensitivity lies in the ultraviolet range, which is not fully satisfactory for use in ordinary electrographic reproduction devices. Even the most sensitive organic photoconductive polymers fall far short of being satisfactory for commercial purposes. The choice of available materials for use in aromatic polymer sheets is inherently limited due to the necessity of selecting an already photoconductive material. Moreover, all the above-mentioned xerographic plates lack resistance to wear and operational stability, especially at higher temperatures.
Bindemiddelplater inneholdende sinkoksydpigmenter, som er relativt billige, har en lavere følsomhet enn selenglassplater og kan ikke gjenanvendes. Dessuten er deres synlige følsomhet som ovenfor nevnt, ganske begrenset. Det er videre nødvendig å bruke så store prosentvise andeler fotoledende pigment for oppnåelse av tilstrekkelig følsomhet, at det blir vanskelig ved sinkoksydplater å oppnå glatte overflater som egner seg for effektiv tonerover-føring og etterfølgende rensing for fornyet bruk. En ytterlig ulempe ved bruken av sinkoksydplater av bindemiddeltypen er at de lettere kan gjøres følsomme ved negativ korona enn ved positiv, noe .som resulterer i dårlig trykkvalitet. Denne egenskap gjør dem kommersielt uønskete idet negativ koronautladning frembringer meget mer ozon enn positiv koronautladning og er generelt vanskeligere å styre. Binder plates containing zinc oxide pigments, which are relatively cheap, have a lower sensitivity than selenium glass plates and cannot be reused. Moreover, as mentioned above, their visible sensitivity is quite limited. It is also necessary to use such large percentages of photoconductive pigment to achieve sufficient sensitivity that it becomes difficult with zinc oxide plates to achieve smooth surfaces that are suitable for efficient toner transfer and subsequent cleaning for renewed use. A further disadvantage of the use of zinc oxide plates of the binder type is that they can be more easily sensitized by negative corona than by positive, which results in poor print quality. This property makes them commercially undesirable as negative corona discharge produces much more ozone than positive corona discharge and is generally more difficult to control.
I britisk patentskrift 1.175.451 er det beskrevet elektrofotografiske plater og fremgangsmåter for anvendelse av ftalocyaninpigmenter dispergert i et bindemiddelmateriale. Disse plater, kan gjenanvendes eller kan være engangsplater og har følsomhet som strekker seg over hele spektret. I norsk patentsøknad 4925/70 er beskrevet ftalocyanin-bindemiddelsammensetninger. British patent document 1,175,451 describes electrophotographic plates and methods for using phthalocyanine pigments dispersed in a binder material. These plates can be reused or can be disposable plates and have sensitivities that span the entire spectrum. Phthalocyanine binder compositions are described in Norwegian patent application 4925/70.
Generelt fremstilles ftalocyaninpigment-bindemiddelplater ved å inkorporere ftalocyaninpigmenter i et oppløst eller smeltet Generally, phthalocyanine pigment binder sheets are prepared by incorporating phthalocyanine pigments into a dissolved or molten
bindemiddel ved kulemøllemaling. Slik maling må utføres i løpet binder in ball mill grinding. Such painting must be carried out during the race
av dager for oppnåelse av akseptable dispersjoner. Når kulemølle-maling anvendes, blir omkrystallisering av alfa-formen av ftalo-cyaninutgangsmaterialet til de langt mer følsomme beta polymorfe enten ytterst langsom eller finner overhodet ikke sted. of days to achieve acceptable dispersions. When ball mill grinding is used, recrystallization of the alpha form of the phthalocyanine starting material into the far more sensitive beta polymorph is either extremely slow or does not take place at all.
Formålet med den foreliggende oppfinnelse ér å frembringe The purpose of the present invention is to produce
en fremgangsmåte som muliggjør hurtig fremstilling av ftalocyånin-dispersjon hvorved alfa-ftalcyanin omdannes til mer fotofølsomt beta-ftalocyanin. a method that enables rapid production of phthalocyanine dispersion whereby alpha-phthalocyanine is converted into more photosensitive beta-phthalocyanine.
Dette oppnås ifølge oppfinnelsen ved en fremgangsmåte som kjennetegnes ved ^at ftalocyaninet omfatter en eller flere av alfa-, alfa- og beta- og alfa- og X-formen av ftalocyanin og sandmales inntil alfa-ftalocyaninet er stort sett fullstendig omdannet til beta-ftalocyanin, hvoretter det fotoledende lag dannes av den malte blanding. This is achieved according to the invention by a method characterized by the fact that the phthalocyanine comprises one or more of the alpha, alpha and beta and alpha and X forms of phthalocyanine and is sand-ground until the alpha-phthalocyanine is mostly completely converted to beta-phthalocyanine , after which the photoconductive layer is formed from the painted mixture.
Denne fremgangsmåte er langt hurtigere enn kulemøllemaling. Faktisk fremstilles dispersjonene i løpet av timer istedenfor dager. Ved bruk av sandmaling i motsetning til kulemøllemaling omkrystalliseres et langt mindre følsomt alfa-ftalocyaninutgangs-materiale til den langt følsommere beta-form på en overraskende kort tid. I noen tilfeller er sandmaling funnet å være den eneste metode som resulterer i denne omdannelse av alfa- til beta-ftalocyanin. Kommersielt akseptable dispersjoner kan ha et pigment-innhold på opp til 15-20 vektsprosent. Uansett hvilken pigmentkonsentrasjon som brukes, vil for en gitt pigmentkonsentrasjon dispersjoner fremstilt ved korttids kulemøllemaling ikke gi elek-trofotograf isk akseptable belegg. This method is far faster than ball mill grinding. In fact, the dispersions are prepared within hours instead of days. By using sand grinding as opposed to ball mill grinding, a far less sensitive alpha-phthalocyanine starting material is recrystallized into the far more sensitive beta form in a surprisingly short time. In some cases, sandblasting has been found to be the only method that results in this conversion of alpha- to beta-phthalocyanine. Commercially acceptable dispersions can have a pigment content of up to 15-20% by weight. Regardless of which pigment concentration is used, for a given pigment concentration, dispersions produced by short-term ball mill grinding will not produce electrophotographically acceptable coatings.
Den ovenfor beskrevne fremgangsmåte virker spesielt godt når det ønskes å fremstille en metallfri beta-ftalocyanin-bindemiddel-dispersjon ved å gå ut fra.alfa-formen som skal omdannes, samt mengder av beta-formen, X-formen eller blandinger av disse. I til-legg til alfa-formen som skal omdannes, kan det brukes hvilket som helst ftalocyanin. Typiske ftalocyaniner omfatter metallftalocyaniner og metallfri ftalocyaniner som alfa-, beta-og X-formen av ftalocyanin. The method described above works particularly well when it is desired to produce a metal-free beta-phthalocyanine binder dispersion by starting from the alpha form to be converted, as well as quantities of the beta form, the X form or mixtures thereof. In addition to the alpha form to be converted, any phthalocyanine can be used. Typical phthalocyanines include metal phthalocyanines and metal-free phthalocyanines such as the alpha, beta and X forms of phthalocyanine.
Hvilken som helst harpiks kan anvendes i fremgangsmåten ifølge oppfinnelsen. Typiske harpikser, omfatter petroleumhydrokarboner, styren-akrylnitriler, epoksyharpikser, polykarbonater, polysulfon-ater, styren-butadienkopolymerer, polyestere, fenolharpikser, al-kyder, silikonalkyder, kumaron-indenharpikser, fenoksyharpikser, polyvinylkarbazoler og polyuretaner. En foretrukken sammensetning for bruk i fremgangsmåten ifølge oppfinnelsen omfatter en kombinasjon av et ftalocyaninpigment med en alkyd-akrylatharpiksblanding, en silikonharpiks, og et klorert hydrokarbon, noe som er mer de-taljert beskrevet i norsk patentsøknad 4925/70 (US-søknad nr. 866. Any resin can be used in the method according to the invention. Typical resins include petroleum hydrocarbons, styrene-acrylonitriles, epoxy resins, polycarbonates, polysulfonates, styrene-butadiene copolymers, polyesters, phenolic resins, alkyds, silicone alkyds, coumarone-indene resins, phenoxy resins, polyvinylcarbazoles and polyurethanes. A preferred composition for use in the method according to the invention comprises a combination of a phthalocyanine pigment with an alkyd-acrylate resin mixture, a silicone resin, and a chlorinated hydrocarbon, which is described in more detail in Norwegian patent application 4925/70 (US application no. 866 .
926). ' 926). '
Sandmalingeh kan utføres i et vilkårlig tidsrom. Et foretrukket tidsrom varierer fra ca. 0,2 time til ca. 2,0 timer. Op-timale resultater oppnåes når sanctmalingen utføres i ca. 0,75 time under anvendelse av ca. 50 volumprosent sand og opprettholdelse av temperatur på ca. 4 9-82°C. Sandmalingeh can be done for any length of time. A preferred period varies from approx. 0.2 hour to approx. 2.0 hours. Optimum results are achieved when the sanct painting is carried out for approx. 0.75 hour using approx. 50 volume percent sand and maintaining a temperature of approx. 4 9-82°C.
Etter kombinasjon av materialene for dannelse av et fotoledende lag, kan dette lag anbringes på et vilkårlig egnet bærende underlag. Typiske bærende underlag omfatter papir, aluminium, messing og plast; After combining the materials to form a photoconductive layer, this layer can be placed on any suitable supporting substrate. Typical bearing substrates include paper, aluminium, brass and plastic;
Pigment-bindemiddel-løsningsmiddeloppslemningen kan påføres underlaget ved hvilken som helst kjent påstryknings- eller beleg-ningsmetode, som for eksempel sprøyting, flytebelegning, kniv-belegning, elektrobelegning, "Mayer bår"-trekkbelegning, dypping, rullebelegning, etc. Påsprøytning i et elektrisk felt kan være foretrukket for oppnåelse av mest mulig glatt overflate og dyppe-belegning som en bekvem metode i laboratoriet. The pigment-binder-solvent slurry can be applied to the substrate by any known application or coating method, such as spraying, float coating, knife coating, electrocoating, "Mayer stretcher" drag coating, dipping, roller coating, etc. Spraying in an electric field may be preferred for achieving the smoothest possible surface and dip-coating as a convenient method in the laboratory.
For ytterligere å definere særegenhetene ved foreliggende oppfinnelse er de følgende eksempler ment å illustrere og ikke begrense enkelthetene ved foreliggende oppfinnelse. De forekomm-ende deler og prosenter er basert på vekt med mindre annet er nevnt. In order to further define the peculiarities of the present invention, the following examples are intended to illustrate and not to limit the details of the present invention. The parts and percentages that occur are based on weight unless otherwise mentioned.
EksempelI Example I
Følgende materialer ble forhåndsblandet og anbrakt i en "L-3-J"-laboratoriesandmølle på forhånd halvfylt med 20-30 mesh Ottawa-sand: The following materials were pre-mixed and placed in an "L-3-J" laboratory sand mill pre-filled half-filled with 20-30 mesh Ottawa sand:
29 g av alfa-formen av metallfri ftalocyanin, 29 g of the alpha form of metal-free phthalocyanine,
192 g "Arotap EP8911-7-7", en akrylharpiks, 192 g "Arotap EP8911-7-7", an acrylic resin,
192 g "Chlorowax 70-LP", en klorert, upolymerisert harpiks-paraffin, 192 g "Chlorowax 70-LP", a chlorinated, unpolymerized resin-paraffin,
66 g silikonharpiks "SR-82", og 66 g silicone resin "SR-82", and
250 g toluen. 250 g of toluene.
Blandingen ble malt i en time ved 2.400 omdreininger pr. minutt. Temperaturen ble holdt på mellom 49-82°C. Mens alfa-ftalocyaninet ble findelt og jevnt dispergert, ble det også fullstendig omkrystallisert til den fotofølsomme beta-form under disse betingelser. Pigmentdispersjonen ble fortynnet til ca. 35 vektsprosent tørrstoffinnhold med toluen og deretter påført ved hjelp av en "Mayer rod" på et ledende underlag bestående av en ca. 0,127 mm tykk aluminiumfolie. Det resulterende pigment-bindemiddellag hadde en blågrønn farge. Underlaget ble belagt til en tørr tykkelse på ca. 0,076 mm. Pigment-bindemiddelbeleggets lysutladningsegenskaper ble bestemt ved koronaladning av laget til ca. 500 volt positiv (målt ved et "Keythley Model 610 BR"-elektrometer ved likestrøm), etterfulgt av eksponering ved hjelp av en wolframlampe (kvarts jod ved 2850° fargetemperatur). Under disse betingelser var en eksponering .på ca. 4:int. lumen/929 cm 2/sek. (4 foot-candle sec-onds) tilstrekkelig til å redusere spenningen til ca. 60 volt. Under anvendelse av vanlig xerografisk utstyr slik som et "Xerox Model D"-kopieringsapparat ble ftalocyaninpigme.nt-bindemiddel-belegget likeledes ladet, eksponert av en standard wolframprøve-lampe og deretter fremkalt med tørr toner ved vanlig kaskadefrem-kalling. Det tonete bilde ble deretter overført til vanlig skrive-papir. Det ble oppnådd en høy billedkvalitet. The mixture was ground for one hour at 2,400 rpm. minute. The temperature was kept between 49-82°C. While the alpha-phthalocyanine was finely divided and uniformly dispersed, it was also completely recrystallized to the photosensitive beta form under these conditions. The pigment dispersion was diluted to approx. 35% dry matter content by weight with toluene and then applied using a "Mayer rod" on a conductive substrate consisting of an approx. 0.127 mm thick aluminum foil. The resulting pigment-binder layer had a blue-green color. The substrate was coated to a dry thickness of approx. 0.076 mm. The light discharge properties of the pigment-binder coating were determined by corona charging the layer to approx. 500 volts positive (measured by a "Keythley Model 610 BR" electrometer at direct current), followed by exposure using a tungsten lamp (quartz iodine at 2850° color temperature). Under these conditions, an exposure of approx. 4:int. lumens/929 cm 2/sec. (4 foot-candle sec-onds) sufficient to reduce the voltage to approx. 60 volts. Using conventional xerographic equipment such as a "Xerox Model D" copier, the phthalocyanine pigment-nt binder coating was likewise charged, exposed by a standard tungsten sample lamp and then developed with dry toner by conventional cascade development. The tinted image was then transferred to plain writing paper. A high image quality was achieved.
Eksempel II Example II
Ca. 50 0 g av blandingen angitt i eksempel I ble anbrakt i About. 500 g of the mixture indicated in Example I was placed in
en kulemølle som var 1/3 fylt med flintkuler med diameter 12,7 mm og malt i ca. en time ved 140 omdreininger pr. minutt. Dispersjonen ble belakt som beskrevet i eksempel I. Det resulterende pigment-bindemiddellag hadde en dypblå farge. Ved prøving av fotofølsom-heten som beskrevet i eksempel I, mottok laget en spenning på bare ca. 120 volt og krevet ca. 6 int. lumen/020 cm 2/sek. eksponering for oppnåelse av en restspenning på 60 volt. Det ble ikke oppnådd noe bilde ved bruk av "Model D"-utstyret. a ball mill that was 1/3 filled with flint balls with a diameter of 12.7 mm and ground for approx. one hour at 140 rpm. minute. The dispersion was coated as described in Example I. The resulting pigment-binder layer had a deep blue color. When testing the photosensitivity as described in example I, the layer received a voltage of only approx. 120 volts and required approx. 6 int. lumens/020 cm 2/sec. exposure to achieve a residual voltage of 60 volts. No image was obtained using the "Model D" equipment.
Eksempel III Example III
Ca. 50 g av blandingen beskrevet i eksempel I ble anbrakt About. 50 g of the mixture described in Example I was placed
i en glassbeholder og malt i ca. en time i et "Gardner"-rystéappa-rat for maling under anvendelse av 3,17 mm polerkuler av stål som malemedium. Den dypblå dispersjon ble belakt på et underlag og prøvet som beskrevet i eksempel I. Belegget mottok bare ca. 140 volt og ble utladet til ca. 60 volt ved ca. 2 int. lumen/9 29 cm 2/ sek. eksponering. Intet bilde ble oppnådd ved bruk av "Model D"-utstyr. in a glass container and ground for approx. one hour in a "Gardner" shaker for painting using 3.17 mm steel polishing balls as the painting medium. The deep blue dispersion was coated on a substrate and tested as described in Example I. The coating received only approx. 140 volts and was discharged to approx. 60 volts at approx. 2 int. lumen/9 29 cm 2/ sec. exposure. No image was obtained using "Model D" equipment.
De følgende eksempler IV og V illustrerer tilfeller hvor sandmaling av en ftalocyanin-bindemiddelblanding ga akseptable fotofølsomme dispersjoner hvor kulemøllemaling ikke ga sådanne. Det synes klart at for samme ftalocyanin er det vanskelig, om overhodet mulig å tilveiebringe omdannelse av ftalocyaninet ved kulemølle-maling. The following examples IV and V illustrate cases where sand grinding of a phthalocyanine binder mixture produced acceptable photosensitive dispersions where ball mill grinding did not. It seems clear that for the same phthalocyanine it is difficult, if at all possible, to provide conversion of the phthalocyanine by ball mill grinding.
Eksempel IV Example IV
En forhåndsblanding av 196 g "Chlbrowax", 196 g "Arotop EP 9811-7-7", 66 g "SR-82", 22 g alfa-ftalocyanin og 150 g toluen ble tilsatt til en "L-3-J"-sandmølle og malt som beskrevet i eksempel I i to timer. Den malte blanding ble brukt som belegg og prøvet som i eksempel I. Det blågrønne lag ble funnet å motta 500 volt og ble utladet til 60 volt ved 4,8 int. lumen/929 cm 2/sek. eksponering. Et elektrostatisk bilde ble fremstilt, fremkalt og overført til papir som beskrevet i eksempel I. A premix of 196 g "Chlbrowax", 196 g "Arotop EP 9811-7-7", 66 g "SR-82", 22 g alpha-phthalocyanine and 150 g toluene was added to an "L-3-J"- sand mill and ground as described in Example I for two hours. The ground mixture was used as a coating and tested as in Example I. The blue-green layer was found to receive 500 volts and was discharged to 60 volts at 4.8 int. lumens/929 cm 2/sec. exposure. An electrostatic image was prepared, developed and transferred to paper as described in Example I.
Eksempel V Example V
Følgende materialer ble blandet i en 3,8 liters kulemølle, 1/3 fylt med 12,7 mm diameter flintkuler og malt i ca. 20 timer ved 14 0 omdreininger pr. minutt: The following materials were mixed in a 3.8 liter ball mill, 1/3 filled with 12.7 mm diameter flint balls and ground for approx. 20 hours at 14 0 revolutions per minute:
144 g metallfri alfa-ftalocyanin, 144 g metal-free alpha-phthalocyanine,
960 g "Arotrop EP9811-7-7", 960 g "Arotrope EP9811-7-7",
328 g silikonharpiks "SR-82", 328 g silicone resin "SR-82",
144 g "Syloid 244", et silisiumdioksydpigment, 144 g "Syloid 244", a silicon dioxide pigment,
960 g "Chlorowax 70-LP", og 960 g "Chlorowax 70-LP", and
3.000 g toluen. 3,000 g of toluene.
Dispersjonen ble belakt som beskrevet i eksempel I. Belegget var dypblått, noe som er karakteristisk for alfa-ftalocyaninet. Materialet ble funnet å motta bare 240 volt og krevet ca. 3,6 int. lumen/929 cm 2/sek. for utladning til ca. 60 volt restspenning. Det ble ikke oppnådd et brukbart bilde i "Model D"-utstyr. Det var klart at bare en del av pigmentet var omdannet til beta-formen, hvilket begrenset beleggets fotofølsomhet. The dispersion was coated as described in Example I. The coating was deep blue, which is characteristic of the alpha-phthalocyanine. The material was found to receive only 240 volts and required approx. 3.6 int. lumens/929 cm 2/sec. for discharge to approx. 60 volt residual voltage. A usable image was not obtained in "Model D" equipment. It was clear that only part of the pigment had been converted to the beta form, which limited the photosensitivity of the coating.
Selv om de foreliggende eksempler er spesifikke med hensyn til betingelser og anvendte materialer, vil hvilke som helst av Although the present examples are specific with respect to conditions and materials used, any of
de nevnte typiske materialer i eksemplene kunne erstattes med andre egnete materialer og med liknende resultater. the mentioned typical materials in the examples could be replaced with other suitable materials and with similar results.
Et silisiumdioksydpigment kan for eksempel inkorporeres i sandmaleprosessen for å tjene som antiblokkeringsmiddel. For example, a silicon dioxide pigment can be incorporated into the sandblasting process to serve as an antiblocking agent.
Claims (2)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US46270A | 1970-01-02 | 1970-01-02 |
Publications (2)
Publication Number | Publication Date |
---|---|
NO132254B true NO132254B (en) | 1975-06-30 |
NO132254C NO132254C (en) | 1975-10-08 |
Family
ID=21691616
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
NO4972/70A NO132254C (en) | 1970-01-02 | 1970-12-29 |
Country Status (12)
Country | Link |
---|---|
US (1) | US3672979A (en) |
JP (1) | JPS4917535B1 (en) |
BE (1) | BE761135A (en) |
CA (1) | CA951697A (en) |
CH (1) | CH571731A5 (en) |
DE (1) | DE2062900A1 (en) |
ES (1) | ES386759A1 (en) |
FR (1) | FR2075187A5 (en) |
GB (1) | GB1334060A (en) |
NL (1) | NL7100035A (en) |
NO (1) | NO132254C (en) |
PL (1) | PL82204B1 (en) |
Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3854943A (en) * | 1969-07-30 | 1974-12-17 | Xerox Corp | Manifold imaging method and member employing fundamental particles of alpha metal-free phthalocyanine |
US3789216A (en) * | 1973-01-02 | 1974-01-29 | Xerox Corp | Photodetection device and method comprising phthalocyanine |
JPS5389433A (en) * | 1977-01-17 | 1978-08-07 | Mita Industrial Co Ltd | Photosensitive body for electrophotography |
JPS53135126U (en) * | 1977-03-29 | 1978-10-26 | ||
GB1599430A (en) * | 1977-06-27 | 1981-09-30 | Konishiroku Photo Ind | Photoconductive composition for use in the preparation of an electrophotographic material |
JPS61200996A (en) * | 1985-03-04 | 1986-09-05 | Agency Of Ind Science & Technol | Production of organic electrically-conductive material crystal |
US4666802A (en) * | 1986-07-16 | 1987-05-19 | Eastman Kodak Company | Photoconductive elements sensitive to infrared radiation having a bromoindium phthalocyanine pigment |
JPS63301953A (en) * | 1987-06-01 | 1988-12-08 | Canon Inc | Manufacture of electrophotographic sensitive body |
GB2212510B (en) * | 1987-11-19 | 1991-12-18 | Toyo Ink Mfg Co | Optical semiconductor material and electrophotographic plate using same |
GB2231166B (en) * | 1989-04-13 | 1993-05-05 | Ind Tech Res Inst | Organic photoreceptor for use in electrophotography |
US5087540A (en) * | 1989-07-13 | 1992-02-11 | Matsushita Electric Industrial Co., Ltd. | Phthalocyanine photosensitive materials for electrophotography and processes for making the same |
GB2274848A (en) * | 1993-02-05 | 1994-08-10 | Citizen Watch Co Ltd | Modification of pigment and electrophotographic photoreceptor containing modified pigment |
-
1970
- 1970-01-02 US US462A patent/US3672979A/en not_active Expired - Lifetime
- 1970-09-14 CA CA093,039,A patent/CA951697A/en not_active Expired
- 1970-10-17 JP JP45091563A patent/JPS4917535B1/ja active Pending
- 1970-12-21 GB GB6055770A patent/GB1334060A/en not_active Expired
- 1970-12-21 DE DE19702062900 patent/DE2062900A1/en active Pending
- 1970-12-21 CH CH1891870A patent/CH571731A5/xx not_active IP Right Cessation
- 1970-12-22 ES ES386759A patent/ES386759A1/en not_active Expired
- 1970-12-29 FR FR7047702A patent/FR2075187A5/fr not_active Expired
- 1970-12-29 NO NO4972/70A patent/NO132254C/no unknown
- 1970-12-31 BE BE761135A patent/BE761135A/en unknown
- 1970-12-31 PL PL1970145397A patent/PL82204B1/pl unknown
-
1971
- 1971-01-04 NL NL7100035A patent/NL7100035A/xx unknown
Also Published As
Publication number | Publication date |
---|---|
BE761135A (en) | 1971-06-30 |
ES386759A1 (en) | 1974-01-16 |
NL7100035A (en) | 1971-07-06 |
US3672979A (en) | 1972-06-27 |
DE2062900A1 (en) | 1971-09-23 |
FR2075187A5 (en) | 1971-10-08 |
CH571731A5 (en) | 1976-01-15 |
CA951697A (en) | 1974-07-23 |
GB1334060A (en) | 1973-10-17 |
JPS4917535B1 (en) | 1974-05-01 |
PL82204B1 (en) | 1975-10-31 |
NO132254C (en) | 1975-10-08 |
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