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Preparation method of polymorphic photosensitive tiopc nanoparticles and its application in organic photoconductors

A nanoparticle, photosensitive technology, applied in nanotechnology, organic chemistry, titanium organic compounds, etc., to achieve the effect of simplifying the washing process, small particle size, and high sensitivity

Active Publication Date: 2016-09-14
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In summary, there are no reports on the preparation of α-TiOPc, β-TiOPc, and Y-TiOPc nanoparticles by combining purification and transformation into one step.

Method used

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  • Preparation method of polymorphic photosensitive tiopc nanoparticles and its application in organic photoconductors
  • Preparation method of polymorphic photosensitive tiopc nanoparticles and its application in organic photoconductors
  • Preparation method of polymorphic photosensitive tiopc nanoparticles and its application in organic photoconductors

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preparation example Construction

[0033] 1. The method for preparing α-TiOPc nanoparticles provided by the invention comprises the steps in sequence:

[0034] 1) Dissolve a certain mass of crude titanyl phthalocyanine in concentrated sulfuric acid with a mass fraction of 98% at -5°C to 5°C, and then drop it into the continuously stirring -15°C at a rate of 1mL / min to 60mL / min In transition solvent at ~5°C;

[0035] 2) After the dropwise addition, adjust the heat preservation temperature to -15~5℃, and continue to stir for 1~72 hours to obtain a blue emulsion, add low-carbon alcohol to it, let it stand, wait for layers, separate the liquid, and use deionized Water is repeatedly extracted until the water phase is neutral;

[0036] 3) Separate the organic phase, add a precipitant to it, and let it stand to make the TiOPc nanoparticles settle;

[0037] 4) Pour off the supernatant, filter, wash the filter cake with methanol, then beat with deionized water, and freeze-dry to obtain α-TiOPc nanoparticle powder;

...

Embodiment 1

[0042] Embodiment 1: prepare α-TiOPc nanoparticles

[0043]Dissolve 1g of crude titanyl phthalocyanine in 60mL of concentrated sulfuric acid with a mass fraction of 98%, and then add it dropwise at a rate of 1mL / min to 10mL of butanol, 20mL of water and 30mL of o-dichlorobenzene under constant stirring at -15°C In the transformation solvent formed, after the dropwise addition is completed, continue to maintain the temperature of the transformation system at -15°C, continue to stir for 1 hour, extract the mixed solution with water, extract all the phthalocyanine titanium into the o-dichlorobenzene phase, and separate the liquids to obtain the o- Dichlorobenzene phase, 100mL ethanol was added thereinto, the TiOPc nanoparticles were settled, filtered, and the filter cake was beaten with water, and vacuum freeze-dried to obtain blue powder particles, which were analyzed by X-ray powder diffraction ( figure 2 ) proves that the crystal form is α-TiOPc (characteristic diffraction an...

Embodiment 2

[0044] Embodiment 2: Preparation of α-TiOPc nanoparticles

[0045] Dissolve 1 g of crude titanyl phthalocyanine in 30 mL of concentrated sulfuric acid with a mass fraction of 98%, and then add it dropwise at a rate of 60 mL / min to 1000 mL of ethanol, 1000 mL of water, 500 mL of o-dichlorobenzene and 500 mL of In the transformation solvent composed of dichloromethane, after the dropwise addition is completed, continue to maintain the temperature of the transformation system at 5°C, continue to stir for 72 hours, extract the mixed solution with water, extract all the phthalocyanine titanium into the organic phase, and separate the liquids to obtain the organic phase , add 1000mL butanol to it, make the TiOPc nanoparticles settle, filter, beat the filter cake with water, and freeze-dry in vacuum to get blue powder particles. X-ray powder diffraction analysis proves that the crystal form is α-TiOPc (characteristic diffraction angle 2θ is 7.5°, 25.3°, 28.6°), and the particle size ...

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Abstract

The invention relates to a method for preparing a polymorphism photosensitivity TiOPc nano particle and application thereof in an organic photoconductor. The method comprises steps of dissolving crude oxotitanium phthalocyanine in -5 DEG C-5 DEG C concentrated sulfuric acid, dripping into a constantly stirring transformation solvent at certain speed at the feeding temperature; then regulating the heat preservation temperature, continuously stirring for 1-72 hours so as to obtain a blue emulsion, adding lower alcohol into the blue emulsion, repeatedly extracting through deionized water till the blue emulsion is neutral, separating an organic phase out; adding a precipitator to allow TiOPc nano particles to settle; washing filter cakes through methyl alcohol, pulping through deionized water, freeze drying so as to obtain different crystal forms of oxotitanium phthalocyanine nano particles corresponding to the feeding temperature. The polymorphism photosensitivity TiOPc nano particle has small grain size, has good compatibility with PVB (polyvinyl butyral) resin, and is applicable to the material of the organic photoconductor producing electric charge, and the prepared photoconductor has high sensitivity, low dark failure, low residual potential, and good photoconduction performance.

Description

technical field [0001] The invention relates to a preparation method of polymorphic photosensitive TiOPc nanoparticles and its application in organic photoconductors. Background technique [0002] Since C.F.Carlson invented electrophotographic technology in 1938, electrophotographic technologies for black and white and color copying and printing have made great progress. As the core component of the photoconductor—the charge generation layer material, the earliest inorganic materials, such as Se, ZnO, CdS, etc., have been gradually replaced by organic photoconductive materials, because organic materials have several advantages over inorganic materials: Excellent processing and forming performance; many varieties; good light transmission; no pollution pollution; short development cycle, etc. At present, the commonly used charge generation materials mainly include phthalocyanine compounds, perylene compounds, squarylium compounds, azo compounds, etc., among which phthalocyani...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22G03G5/06B82Y40/00
CPCB82Y40/00C07F7/28G03G5/06
Inventor 李祥高李小龙王世荣肖殷
Owner TIANJIN UNIV
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