KR100864315B1 - Process of preparing composition for positive-charged single layer of organic photo conductor drum - Google Patents
Process of preparing composition for positive-charged single layer of organic photo conductor drum Download PDFInfo
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- KR100864315B1 KR100864315B1 KR1020070066601A KR20070066601A KR100864315B1 KR 100864315 B1 KR100864315 B1 KR 100864315B1 KR 1020070066601 A KR1020070066601 A KR 1020070066601A KR 20070066601 A KR20070066601 A KR 20070066601A KR 100864315 B1 KR100864315 B1 KR 100864315B1
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- 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
- G03G5/043—Photoconductive layers characterised by having two or more layers or characterised by their composite structure
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- 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
- G03G5/043—Photoconductive layers characterised by having two or more layers or characterised by their composite structure
- G03G5/047—Photoconductive layers characterised by having two or more layers or characterised by their composite structure characterised by the charge-generation layers or charge transport layers
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- 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
- G03G5/05—Organic bonding materials; Methods for coating a substrate with a photoconductive layer; Inert supplements for use in photoconductive layers
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- 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
- G03G5/05—Organic bonding materials; Methods for coating a substrate with a photoconductive layer; Inert supplements for use in photoconductive layers
- G03G5/0503—Inert supplements
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- 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
- G03G5/05—Organic bonding materials; Methods for coating a substrate with a photoconductive layer; Inert supplements for use in photoconductive layers
- G03G5/0525—Coating methods
Abstract
Description
발명의 분야Field of invention
본 발명은 프린터의 토너 카트리지에 사용되는 전자 사진 감광체(organic photo conductor: "OPC") 드럼에 관한 것이다. 보다 구체적으로, 본 발명은 정대전 단층형 OPC 드럼에 사용되는 전자 사진 감광체 조성물 및 그 제조방법에 관한 것이다.The present invention relates to an organic photo conductor ("OPC") drum used in a toner cartridge of a printer. More specifically, the present invention relates to an electrophotographic photoconductor composition for use in a positively charged single-layer OPC drum and a method of manufacturing the same.
발명의 배경Background of the Invention
전자 사진 감광체가 형성된 OPC 드럼은 정대전(positive-charged) 단층형과 부대전(negative-charged) 적층형으로 구분된다. 이들 전자 사진 감광체는 모두 알루마이트 도금층이 형성된 알루미늄 파이프에 형성된다.OPC drums formed with electrophotographic photosensitive members are classified into positive-charged monolayers and negative-charged laminates. All of these electrophotographic photosensitive members are formed in an aluminum pipe on which an alumite plating layer is formed.
부대전 적층형 OPC 드럼은 알루마이트 도금층 위에 전하 발생재료로 이루어진 전하 발생층을 형성하고, 다시 전하 발생층 위에 전자 수송재료로 이루어진 전하 수송층을 형성한다. 그리고 OPC 드럼 내부에 +전하를 걸어주어 드럼 표면에 -전하가 형성되도록 한다. 부대전 2층형 OPC 드럼에서는 전하 발생층을 형성하기 위한 전하 발생재료 조성액과 전하 수송층을 형성하기 위한 전하 수송재료 조성액이 서로 각각 제조된다.The secondary charge stacked OPC drum forms a charge generating layer made of a charge generating material on the alumite plating layer, and further forms a charge transport layer made of an electron transporting material on the charge generating layer. Then, + charge is applied to the inside of the OPC drum so that-charge is formed on the drum surface. In the incident charge two-layer type OPC drum, the charge generating material composition liquid for forming the charge generating layer and the charge transport material composition liquid for forming the charge transport layer are respectively prepared.
정대전 단층형 OPC 드럼은 전하 발생재료와 전하 소송재료를 함께 혼합한 감광체 조성액을 제조하고, 그 감광체 조성액을 알루마이트 도금층 위에 단층으로 코팅하여 제조한다. 정대전 단층형 OPC 드럼은 드럼 내부에 -전하를 걸어주어 드럼 표면에 +전하가 형성되도록 한다.The positively charged single-layer OPC drum is prepared by preparing a photoconductor composition liquid in which a charge generating material and a charge lawsuit material are mixed together, and coating the photoconductor composition liquid as a single layer on the alumite plating layer. The positively charged single-layer OPC drums impose negative charges on the drums so that positive charges form on the drum surface.
그런데 정대전 단층형 전자 사진 감광체 조성물은 안정성이 좋지 못한 결점이 있다. 여기서 감광체 조성물의 액 안정성이 좋지 못하다는 것은 전하 발생재료와 전하 수송재료가 함께 혼합되어야 하는데 이들이 용제에 고르게 분산되지 않고 일정한 시간이 경과하면 밑으로 가라앉는 침전물이 생기는 것을 의미한다.By the way, the positive electrostatic tomographic electrophotographic photosensitive member composition has a drawback in that stability is not good. Here, the poor liquid stability of the photoconductor composition means that the charge generating material and the charge transporting material should be mixed together, but they do not disperse evenly in the solvent, and after a certain time, a sediment that sinks down is formed.
종래의 정대전 단층형 전자 사진 감광체 조성물은 통상 30일 정도의 액 안정성을 갖는데, 이는 감광체 조성액을 제조한 후 30일이 경과하면 침전물이 생성하여 감광체 조성액을 그대로 사용할 수 없게 되는 것을 의미한다.Conventional positive electrostatic tomographic electrophotographic photoconductor compositions usually have a liquid stability of about 30 days, which means that after 30 days have elapsed from the preparation of the photoconductor composition solution, a precipitate is generated and the photoconductor composition solution cannot be used as it is.
종래의 정대전 단층형 전자 사진 감광체 조성물이 갖는 상기와 같은 문제점을 해결하고자, 본 발명자는 액 안정성이 현저하게 개선된 본 발명의 감광체 조성물 및 이를 제조하는 방법을 개발하기에 이른 것이다.In order to solve the above problems with the conventional positive charge tomography electrophotographic photosensitive composition, the present inventors have come to develop the photosensitive member composition of the present invention and the method for producing the same that the liquid stability is significantly improved.
본 발명의 목적은 액 안정성이 우수한 OPC 드럼용 정대전 단층형 감광체 조성물을 제공하기 위한 것이다.An object of the present invention is to provide a positively charged single layer photosensitive member composition for an OPC drum excellent in liquid stability.
본 발명의 다른 목적은 전하 발생제인 티타늄 프탈로시아닌(TiOPc)을 균일하게 분산시키기 위하여 분산안정제를 부가시킨 정대전 단층형 감광체 조성물을 제공하기 위한 것이다.Another object of the present invention is to provide a positively charged monolayer photoconductor composition in which a dispersion stabilizer is added to uniformly disperse the titanium phthalocyanine (T i OPc), which is a charge generating agent.
본 발명의 또 다른 목적은 액 안정성이 우수한 정대전 단층형 감광체 조성물을 제조하기 위한 방법을 제공하기 위한 것이다.Another object of the present invention is to provide a method for producing a positive charge monolayer photosensitive composition having excellent liquid stability.
본 발명의 상기 및 기타의 목적들은 상세히 설명되는 본 발명에 의하여 모두 달성될 수 있다.The above and other objects of the present invention can be achieved by the present invention described in detail.
발명의 요약Summary of the Invention
본 발명에 따른 OPC 드럼용 정대전 단층형 전자 사진 감광체 조성물은 전하 발생제 0.2∼1중량%, 상기 전하 발생제를 분산시키기 위한 분산 안정제 0.05∼0.5 중량%, 전자수송물질(electron transport material: "ETM") 2∼5중량%, 홀 수송물질(hole transport material: "HTM") 3∼7중량%, 바인더 수지 6∼15중량%, 및 유기용제로 이루어진다.The positively charged single-layer electrophotographic photoconductor composition for an OPC drum according to the present invention comprises 0.2 to 1% by weight of a charge generator, 0.05 to 0.5% by weight of a dispersion stabilizer for dispersing the charge generator, and an electron transport material: ETM ") 2 to 5% by weight, 3 to 7% by weight hole transport material (" HTM "), 6 to 15% by weight binder resin, and an organic solvent.
전하 발생제는 티타늄 프탈로시아닌(TiOPc)이 바람직하고 분산 안정제는 무금속 프탈로시아닌(H2Pc: metal free phthalocyanine)이 바람직하다.Preferably, the charge generator is titanium phthalocyanine (TiOPc), and the dispersion stabilizer is metal free phthalocyanine (H 2 Pc).
전자 수송물질로는 스틸벤 퀴논 또는 안트라퀴논 계열 화합물이 바람직하고, 홀 수송물질로는 스틸벤 계열 화합물이, 바인더 수지로는 폴리카보네이트가 바람직하다.As the electron transporting material, stilbenequinone or anthraquinone-based compound is preferable, a stilbene-based compound is preferable as the hole transporting material, and polycarbonate is preferable as the binder resin.
본 발명에서 사용되는 용제로는 THF(테트라히드로퓨란), MC(메틸렌 클로라이드), EC(에틸렌 클로라이드), 시클로헥사논(cyclohexanone), 1,4-디옥산(1,4-dioxane), 아세톤 등이 있다.Solvents used in the present invention include THF (tetrahydrofuran), MC (methylene chloride), EC (ethylene chloride), cyclohexanone, 1,4-dioxane, acetone, etc. There is this.
본 발명에 따른 정대전 단층형 감광체 조성물은 우선 분말상태의 H2Pc를 유기용제의 일부와 1:7 내지 1:15의 중량비가 되도록 4∼6 시간 제1차 밀링하고(milling); ETM, HTM, 및 바인더 수지를 나머지 유기 용제에 용해시켜 용액을 제조하고; 그리고 상기 밀링된 용액에 상기 유기 용제 용액과 분말상태의 티타늄 프탈로시아닌(TiOPc)을 넣어 약 15∼25시간 동안 제2차 밀링하여 제조한다.The positively charged monolayer photoconductor composition according to the present invention firstly mills the powdered H 2 Pc for 4 to 6 hours in a weight ratio of 1: 7 to 1:15 with a part of the organic solvent; A solution was prepared by dissolving ETM, HTM, and binder resin in the remaining organic solvent; Then, the organic solvent solution and powdered titanium phthalocyanine (T i OPc) are added to the milled solution, and the second milling is performed for about 15 to 25 hours.
이하 본 발명의 구체적인 내용을 하기에 상세히 설명한다. Hereinafter, specific contents of the present invention will be described in detail below.
발명의 구체예에 대한 상세한 설명Detailed Description of the Invention
정대전 단층형 OPC 드럼은 전하 발생재료와 전하 소송재료를 함께 혼합한 감광체 조성액을 제조하고, 그 감광체 조성액을 알루마이트 도금층 위에 단층으로 코팅하여 제조한다. 정대전 단층형 OPC 드럼은 드럼 내부에 -전하를 걸어주어 드럼 표면에 +전하가 형성되도록 한다.The positively charged single-layer OPC drum is prepared by preparing a photoconductor composition liquid in which a charge generating material and a charge lawsuit material are mixed together, and coating the photoconductor composition liquid as a single layer on the alumite plating layer. The positively charged single-layer OPC drums impose negative charges on the drums so that positive charges form on the drum surface.
그런데 정대전 단층형 전자 사진 감광체 조성물은 전하 발생재료와 전하 수송재료가 함께 혼합되기 때문에 액 안정성이 좋지 못한 결점이 있다. 즉 전하 발생재료와 전하 수송재료는 용제에 분산되는데, 시간이 경과함에 따라 이들이 밑으로 가라앉아 침전물이 생기게 된다. 침전물이 생성되면 감광체 조성액을 그대로 사용할 수 없게 된다. 따라서 본 발명에서는 오랜 시간이 경과하여도 침전물이 생기지 않는 액 안정성을 향상시키기 위하여 분산 안정제를 사용하고, 밀링(milling) 공정을 2 단계로 행하는 새로운 제조 방법을 채용한 것이다.However, the positive charge monolayer electrophotographic photoconductor composition has a drawback in that the liquid stability is poor because the charge generating material and the charge transporting material are mixed together. That is, the charge generating material and the charge transporting material are dispersed in the solvent, and as time passes, they sink to the bottom and precipitates are formed. If a precipitate is formed, the photoconductor composition cannot be used as it is. Therefore, in the present invention, in order to improve the stability of the liquid which does not form a precipitate even after a long time, a new production method using a dispersion stabilizer and performing a milling process in two stages is adopted.
본 발명에 따른 OPC 드럼용 정대전 단층형 전자 사진 감광체 조성물은 전하 발생제 0.2∼1 중량%, 상기 전하 발생제를 분산시키기 위한 분산 안정제 0.05∼0.5 중량%, 전자수송물질(electron transport material: "ETM") 2∼5중량%, 홀 수송물질(hole transport material: "HTM") 3∼7중량%, 바인더 수지 6∼15중량%, 및 나머지는 유기용제로 이루어진다.The positively charged single-layer electrophotographic photoconductor composition for an OPC drum according to the present invention comprises 0.2 to 1% by weight of a charge generator, 0.05 to 0.5% by weight of a dispersion stabilizer for dispersing the charge generator, and an electron transport material: ETM ") 2 to 5% by weight, 3 to 7% by weight of a hole transport material (" HTM "), 6 to 15% by weight of a binder resin, and the remainder of the organic solvent.
전하 발생제는 티타늄 프탈로시아닌(TiOPc)이 바람직하고 분산 안정제는 무금속 프탈로시아닌(H2Pc: metal free phthalocyanine)이 바람직하다. 티타늄 프탈로시아닌(TiOPc)은 분자식이 C32H16N8OTi 이고 그 구조식은 하기와 같다.Preferably, the charge generator is titanium phthalocyanine (TiOPc), and the dispersion stabilizer is metal free phthalocyanine (H 2 Pc). Titanium phthalocyanine (TiOPc) has a molecular formula of C 32 H 16 N 8 OTi and the structural formula is as follows.
분산 안정제는 무금속 프탈로시아닌(H2Pc)은 분자식이 C32H18N8 이고, 그 구조식은 하기와 같다.Dispersion stabilizer metal-free phthalocyanine (H 2 Pc) has a molecular formula of C 32 H 18 N 8 , the structural formula is as follows.
본 발명의 전자 수송물질로는 스틸벤 퀴논 또는 안트라퀴논 계열 화합물이 바람직하고, 홀 수송물질로는 스틸벤 계열 화합물이, 바인더 수지로는 폴리카보네이트가 바람직하다.As the electron transporting material of the present invention, stilbenequinone or anthraquinone-based compound is preferable, stilbene-based compound is preferable as the hole transporting material, and polycarbonate is preferable as the binder resin.
본 발명에서 사용되는 용제로는 THF(테트라히드로퓨란), MC(메틸렌 클로라이드), EC(에틸렌 클로라이드), 시클로헥사논(cyclohexanone), 1,4-디옥산(1,4-dioxane), 아세톤 등이 있다. 이들은 단독으로 또는 둘 이상의 조합으로 사용될 수 있으며, 이는 본 발명이 속하는 기술분야의 당업자에 의하여 용이하게 실시될 수 있다.Solvents used in the present invention include THF (tetrahydrofuran), MC (methylene chloride), EC (ethylene chloride), cyclohexanone, 1,4-dioxane, acetone, etc. There is this. These may be used alone or in combination of two or more, which can be easily carried out by those skilled in the art.
본 발명에서는 밀링(milling) 공정을 2 단계로 행하고, 각 단계에서의 성분을 다르게 함으로써 분산성을 향상시킬 수 있도록 하였다.In the present invention, the milling process is performed in two stages, and the dispersibility can be improved by changing the components in each stage.
우선 분말상태의 H2Pc를 유기용제의 일부와 1:7 내지 1:15의 중량비가 되도록 4∼6 시간 제1차 밀링한다.First, H 2 Pc in powder form is first milled for 4 to 6 hours in a weight ratio of 1: 7 to 1:15 with a part of the organic solvent.
상기 ETM, HTM, 및 바인더 수지를 나머지 유기 용제에 용해시켜 용액을 제조한다. The ETM, HTM, and binder resin are dissolved in the remaining organic solvent to prepare a solution.
상기 제1차 밀링한 용액에 상기 유기 용제 용액과 분말상태의 티타늄 프탈로시아닌(TiOPc)을 넣어 약 15∼25시간 동안 제2차 밀링하여 본 발명의 OPC 드럼용 정대전 단층형 전자 사진 감광체 조성물을 제조한다.In the first milled solution, the organic solvent solution and powdered titanium phthalocyanine (T i OPc) were added to the second milling for about 15 to 25 hours, and the positively charged tomographic electrophotographic photoconductor composition for the OPC drum of the present invention. To prepare.
종래의 정대전 단층형 전자 사진 감광체 조성물은 통상 30일 정도의 액 안정성을 갖는데, 본 발명에 따른 정대전 단층형 전자 사진 감광체 조성물은 60일 정도의 액 안정성을 갖는다. 즉 본 발명에서는 감광체 조성액을 제조한 후 60일 정도 경과하였을 때 침전물이 생성하는 것으로 관찰되었다. Conventional positively charged tomographic electrophotographic photoconductor compositions usually have a liquid stability of about 30 days, but the positively charged tomographic electrophotographic photosensitive composition according to the present invention has a liquid stability of about 60 days. That is, in the present invention, it was observed that a precipitate is formed when about 60 days have elapsed after the photoconductor composition was prepared.
본 발명은 전하 발생제인 티타늄 프탈로시아닌(TiOPc)을 균일하게 분산시키기 위하여 분산안정제를 부가시키고, 밀링 공정을 2 단계로 행함으로써 액 안정성이 우수한 OPC 드럼용 정대전 단층형 감광체 조성물을 제공하는 발명의 효과를 갖는다. 또한 본 발명은 액 안정성이 우수한 정대전 단층형 감광체 조성물을 제조하기 위한 방법을 제공한다.The present invention provides a positively charged single-layer photoconductor composition for an OPC drum having excellent liquid stability by adding a dispersion stabilizer to uniformly disperse the titanium phthalocyanine (T i OPc), which is a charge generator, and performing a milling process in two steps. Has the effect of. In addition, the present invention provides a method for producing a positive charge monolayer photoconductor composition excellent in liquid stability.
본 발명의 단순한 변형 내지 변경은 이 분야의 통상의 지식을 가진 자에 의하여 용이하게 실시될 수 있으며, 이러한 변형이나 변경은 모두 본 발명의 영역에 포함되는 것으로 볼 수 있다. Simple modifications or changes of the present invention can be easily carried out by those skilled in the art, and all such modifications or changes can be seen to be included in the scope of the present invention.
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KR20010109182A (en) * | 2000-05-31 | 2001-12-08 | 추후제출 | Electrophotographic photoconductor and method for manufacturing same |
JP2002287435A (en) | 2002-01-23 | 2002-10-03 | Kyocera Mita Corp | Method for forming image by using positive electrification monolayer type electrophotographic photoreceptor |
JP2005200358A (en) | 2004-01-16 | 2005-07-28 | Kyocera Mita Corp | Stilbene derivative, method for producing the same, and electrophotographic photoreceptor |
JP2005338716A (en) * | 2004-05-31 | 2005-12-08 | Kyocera Mita Corp | Image forming method and image forming apparatus |
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KR20010109182A (en) * | 2000-05-31 | 2001-12-08 | 추후제출 | Electrophotographic photoconductor and method for manufacturing same |
JP2002287435A (en) | 2002-01-23 | 2002-10-03 | Kyocera Mita Corp | Method for forming image by using positive electrification monolayer type electrophotographic photoreceptor |
JP2005200358A (en) | 2004-01-16 | 2005-07-28 | Kyocera Mita Corp | Stilbene derivative, method for producing the same, and electrophotographic photoreceptor |
JP2005338716A (en) * | 2004-05-31 | 2005-12-08 | Kyocera Mita Corp | Image forming method and image forming apparatus |
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