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Method for preparing oxytitanium phthalocyanine chartge generating material and apparatus for preparing the same

A technology of titanyl phthalocyanine and charge, which is applied in the field of devices implementing the method, can solve the problems of storage stability deterioration, poor crystal stability, and shortened storage period

Inactive Publication Date: 2006-11-15
安徽秀朗新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The advantage of titanyl phthalocyanine charge generation material lies in its excellent electrophotographic properties, but its disadvantage is poor crystal stability in organic solvents such as tetrahydrofuran
Due to this disadvantage, when a coating solution for a charge generation layer is prepared using titanyl phthalocyanine, the storage stability is extremely deteriorated, resulting in a shortened shelf life

Method used

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  • Method for preparing oxytitanium phthalocyanine chartge generating material and apparatus for preparing the same
  • Method for preparing oxytitanium phthalocyanine chartge generating material and apparatus for preparing the same
  • Method for preparing oxytitanium phthalocyanine chartge generating material and apparatus for preparing the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Embodiment 1 (synthesis of crude titanium phthalocyanine)

[0054] synthesis 1

[0055] Charge 51.26g 1,2-dicyanobenzene, 12.14g urea, 34.38g tetrabutoxybenzene and 100g nonanol image 3 In the pyrex glass vessel 9 in the synthesis apparatus of the present invention shown in . Afterwards, uniformly stir the reactant at 160-170° C. for 0.1-6 hours, and simultaneously apply microwave, 28 kHz frequency and 250 W ultrasonic energy to prepare crude titanium phthalocyanine. During the reaction, the temperature of the reactants was precisely controlled within the error range of ±0.1° C. by using a PID temperature controller 8 . At this time, the microwave power is controlled at 10-3000W. Both microwave and ultrasonic energy are used from the very beginning of the reaction. The X-ray diffraction pattern of crude titanyl phthalocyanine is shown in figure 1 middle.

[0056] synthesis 2

[0057] 12.5 g of 1,3-diiminoisoindoline, 29.31 g of tetrabutoxybenzene and 100 g of qu...

Embodiment 2

[0059] Pour 300g of 97% sulfuric acid into the beaker and stir. While maintaining the sulfuric acid temperature at 10° C. or lower, 10 g of the crude titanyl phthalocyanine prepared in Synthesis 2 of Example 1 was slowly dissolved and stirred for 2 hours. After the sulfuric acid solution was slowly poured on ice water to recrystallize the crude titanyl phthalocyanine, the crude titanyl phthalocyanine was separated by filtration and washed with water until the pH of the filtrate was 7.0. The obtained titanyl phthalocyanine filter cake was added to a mixed solution of chlorobenzene (100 ml) and water (100 ml, including the water contained in the filter cake), and placed in a microwave generating device. The reaction was heated to 50°C over 30 minutes using a PID type temperature controller, stirred at 50°C for 1 hour, then cooled to room temperature. The cooled reaction was filtered to isolate titanyl phthalocyanine and washed with methanol. The titanyl phthalocyanine was drie...

Embodiment 3

[0070] 9.8 g of a titanyl phthalocyanine charge generating material was prepared in the same manner as in Example 2 except that microwave treatment was performed at 60°C. The X-ray diffraction pattern of titanyl phthalocyanine charge generation material is shown in Figure 5 middle.

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Abstract

Disclosed herein are a method and an apparatus for preparing oxytitanium phthalocyanine as a charge generating material. The method comprises the steps of homogeneously mixing an oxytitanium phthalocyanine crude with an organic solvent while microwave energy having afrequency of 0.1~100 GHz and a power of 10~3,000W and ultrasonic wave energy having a frequency of 1~1,000kHz and a power of 10~5,000W are applied thereto, and reacting the mixture at 30~100 DEG C for 0.5~5 hours. The apparatus comprises: a magnetron 1 capable of generating a frequency of 0.1~100GHz and a power of 100~3,000W; a mode stirrer 3 for making the wavelength of microwaves uniform in a microwave container 2; a PID type temperature controller 9 for accurately measurement and controlling the temperature of reactants; a K-type thermocouple shielded from microwaves 4; a condenser 5; an agitator 6, the thermocouple 4, the condenser 5 and the agitator 6 being inserted into three openings formed at a top of the microwave container 2; an ultrasonic tip 7 inserted into an opening formed at a bottom of the microwave container 2; a Pyrex container 9 into which the reactants are introduced; and a solvent tank 10. According to the method and the apparatus, an oxytitanium phthalocyanine charge generating material having superior thermal stability and crystal stability can be prepared in an efficient manner.

Description

technical field [0001] The present invention relates to methods and apparatus for preparing titanyl phthalocyanines suitable for use as charge generating materials. More specifically, the present invention relates to a method of producing titanyl phthalocyanine as a charge generating material having excellent crystal stability by utilizing ultrasonic waves and microwaves, and an apparatus for carrying out the method. Background technique [0002] Photoconductors are highly photosensitive in the visible region and are widely used in various devices such as copiers, printers, etc. Photoconductors currently used are mostly produced by coating a photosensitive layer including an inorganic charge generating material selected from selenium, zinc oxide, cadmium sulfide, and the like as a main component on a conductive substrate. However, these inorganic charge generating materials are still unsatisfactory in terms of photosensitivity, thermal stability, water resistance, durabilit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G03G5/04G03GG03G5/05G03G5/06
CPCC07D487/22C09B67/0026G03G5/051G03G5/0525G03G5/0696H05B6/74G03G5/04
Inventor 权鐘浩郑起硕孙佑镐朴圣秀高秦必郑铉锡
Owner 安徽秀朗新材料科技有限公司