WO2018188554A1 - Preparation method for positively charged non-magnetic toner - Google Patents

Preparation method for positively charged non-magnetic toner Download PDF

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Publication number
WO2018188554A1
WO2018188554A1 PCT/CN2018/082331 CN2018082331W WO2018188554A1 WO 2018188554 A1 WO2018188554 A1 WO 2018188554A1 CN 2018082331 W CN2018082331 W CN 2018082331W WO 2018188554 A1 WO2018188554 A1 WO 2018188554A1
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minutes
rpm
parts
weight
mixed
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PCT/CN2018/082331
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French (fr)
Chinese (zh)
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袁誉炎
吴校荣
于普海
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珠海思美亚碳粉有限公司
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Publication of WO2018188554A1 publication Critical patent/WO2018188554A1/en

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    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03GELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00Developers
    • G03G9/08Developers with toner particles
    • G03G9/0802Preparation methods
    • G03G9/081Preparation methods by mixing the toner components in a liquefied state; melt kneading; reactive mixing
    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03GELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00Developers
    • G03G9/08Developers with toner particles
    • G03G9/0821Developers with toner particles characterised by physical parameters

Definitions

  • the present invention relates to a method of preparing a toner, and more particularly to a method of preparing a positively charged non-magnetic toner.
  • the present invention is based on a Chinese invention patent whose application date is April 12, 2017, and whose application number is CN201710235981.1, the contents of which are incorporated herein by reference.
  • Existing printers generally include two major categories, laser printers and inkjet printers.
  • Laser printers are widely used in office workplaces, especially in inkjet printers, which have the advantages of fast printing speed and low printing cost.
  • the popularity of color laser printing has become increasingly large, and the original toners (also commonly referred to as toners) used in laser printers tend to be expensive and limit the use of users.
  • An object of the present invention is to provide a method for preparing a positively-charged non-magnetic toner having a good printing effect.
  • the present invention provides a method for preparing a positively-charged non-magnetic toner, wherein the positively-charged non-magnetic toner includes a toner master batch and an additive; and the preparation method includes a pre-mixing step and a post-mixing step;
  • the premixing step includes first mixing the toner masterbatch in a mixer at 600 rpm for 2 minutes and then mixing at 1200 rpm for 2 minutes;
  • the postmixing step includes, first, the premixing step.
  • An additive was added to the obtained toner master batch mixture, and mixed in a mixer at 600 rpm for 2 minutes to 3 minutes, and then mixed at 1200 rpm for 2 minutes to 4 minutes.
  • the toner master batch comprises 100 parts by weight of styrene-acrylic resin, 3 parts by weight of a release agent,
  • the additive comprises 0.5 parts by weight of small particle size hydrophobic silica having a particle diameter of 7 nm to 20 nm, and 0.4 parts by weight of large particle size hydrophobic dioxide having a particle diameter of 40 nm to 200 nm. Silicon, 0.7 parts by weight of barium titanate and 0.3 parts by weight of polymethyl methacrylate.
  • a further solution is that in the post-mixing step, the mixture is first mixed at 600 rpm for 2 minutes and then at 1200 rpm for 2 minutes.
  • An alternative solution is to first mix at 600 rpm for 3 minutes and then at 1200 rpm for 3 minutes.
  • the mixture is first mixed at 600 rpm for 3 minutes and then at 1200 rpm for 4 minutes.
  • the pre-mixing step further comprises: a melt-kneading step of melt-kneading the mixed toner masterbatch mixture into a kneaded product in a kneader to control the temperature of the kneading at 100 degrees Celsius to Between 140 degrees Celsius; a cooling step, cooling the kneaded material to room temperature; a pulverizing and grading step, pulverizing the cooled kneaded material into granules, and grading a toner masterbatch having a diameter of 5 ⁇ m to 20 ⁇ m in the granules.
  • the post-mixing step further comprises: a screening step of sieving the toner masterbatch and the additive mixture obtained by post-mixing to remove coarse particles, the mesh number of which is 80 mesh to 150 mesh, preferably 100 Head.
  • the beneficial effects of the present invention are: by adding an additive to the toner masterbatch to change the charge amount and fluidity of the toner masterbatch, and premixing the toner masterbatch by a pre-mixing step, and passing the post-mixing
  • the step of post-mixing the toner masterbatch and the additive changes the distribution and embedding of the additive in the positively charged non-magnetic toner, and the same can also change its charge amount and fluidity.
  • the invention combines the selection of raw materials and the mixing process to prepare a positively charged non-magnetic toner having good printing quality.
  • FIG. 1 is a formulation of four sets of positively charged non-magnetic toner embodiments of different compositions and levels.
  • FIG. 3 is a table of premixing process parameters for premixing the toner master batches of Example 4 in three groups.
  • FIG. 4 is a table showing the results of printing test of the toner master batches of the three groups of the premixed Example 4.
  • FIG. 5 is a post-mixing process parameter table in which the additive of Example 4 is added to the toner master batch obtained by the third group premixing process for post-mixing test.
  • the positively-charged non-magnetic toner of the present invention includes a toner masterbatch including a styrene-acrylic resin, a mold release agent, a colorant, and a charge control agent, and the additive includes silica, barium titanate, and an additive.
  • the additive includes silica, barium titanate, and an additive.
  • Polymethyl methacrylate the inventors prepared a total of four sets of positively charged non-magnetic toners by adjusting the formula. The content of each component is shown in Fig. 1 (), wherein the particle size of fine-grained silica is from 7 nm to 20 nm.
  • the particle size of the large particle silica is between 40 nm and 200 nm, and the surfaces of the fine particle silica and the large particle silica are both subjected to hydrophobic treatment.
  • the coloring agent may be used in addition to carbon black, such as cyanine black, ferrite, aniline black, etc.
  • the wax used for the release agent may be paraffin wax, low molecular weight polypropylene wax, low molecular weight polyethylene wax, and Brazilian palm.
  • a wax or the like, a charge control agent may be a quaternary ammonium salt or the like in addition to the oil-soluble aniline black.
  • OPC ghosting refers to a phenomenon in which repetitive characters appear below the printed text.
  • BG is the bottom gray value
  • bottom ash refers to the case where the non-developing area is grayed out
  • the value of the blank area on the printing paper and the area covered by the additional paper can be measured by the gradation meter. The difference between the values of the values is obtained. The smaller the value of BG, the better the printing effect.
  • Blackboard smearing refers to printing a full blackboard, and the situation under the blackboard is grayed out.
  • Premixing process The toner master batch of Example 4 was subjected to three sets of premixing tests in accordance with the formulation in Table 1, and the premixing process is shown in Fig. 3.
  • R1 represents the rotational speed 1
  • the unit rpm is the revolution/minute
  • T1 represents the inter-turn of R1, and the unit is minute
  • R1 represents the rotational speed 2
  • the unit is also the revolution/minute
  • T2 represents the inter-turn of R2, and the unit is minute.
  • the first group 100 parts of styrene resin, 3 parts of wax, 3 parts of oil-soluble aniline black and 6 parts of carbon black in a mixer (such as a Henschel mixer) at 600 rpm
  • a mixer such as a Henschel mixer
  • the rotation speed is mixed for 5 minutes to form a toner masterbatch mixture; then the mixed toner masterbatch mixture is melt-kneaded into a kneaded product in a kneader (such as a parallel twin-screw kneader) to control the kneading temperature.
  • Group 2 100 parts of styrene resin, 3 parts of wax, 3 parts of oil-soluble aniline black and 6 parts of carbon black in a mixer (such as a Henschel mixer) at 1200 rpm The rotation speed is mixed for 5 minutes to form a toner masterbatch mixture; then the mixed toner masterbatch mixture is melt-kneaded into a kneaded product in a kneader (such as a parallel twin-screw kneader) to control the kneading temperature.
  • a mixer such as a Henschel mixer
  • the mixture is then cooled to room temperature; finally, the cooled kneaded material is pulverized into granules, and a toner masterbatch having a diameter of 5 micrometers to 20 micrometers is fractionated in the granules. .
  • the third group 100 parts of styrene resin, 3 parts of wax, 3 parts of oil-soluble aniline black and 6 parts of carbon black in a mixer (such as a Henschel mixer) first 600 rpm / Mixing at a minute speed for 2 minutes, mixing at 1200 rpm for 5 minutes to form a toner masterbatch mixture; then mixing the mixed toner masterbatch in a mixer (such as a parallel twin-screw mixer) Melt and knead into a kneaded product, control the mixing temperature between 100 ° C and 140 ° C; then cool the kneaded material to room temperature; finally, the cooled kneaded material is pulverized into particles and classified in the particles A toner masterbatch having a diameter of from 5 micrometers to 20 micrometers is produced.
  • a mixer such as a Henschel mixer
  • the toner masterbatch obtained by the first group, the second group and the third group process is respectively loaded into the TN580 toner cartridge, and the printing test is performed on the HL-5240 printer.
  • the test results are shown in FIG.
  • Post-mixing process The additive of Example 4 was added to the color masterbatch obtained in the third group of pre-mixing processes according to the formulation of Fig. 1 to carry out a post-mixing test, and the post-mixing process is shown in Fig. 5.
  • the fourth group adding 0.5 parts by weight to the toner masterbatch obtained in the third group premixing process, having a particle diameter of 7 nm to 2
  • ester is mixed in a mixer (such as a Henschel mixer) at 600 rpm for 2 minutes, then mixed at 1200 rpm for 2 minutes, and the mixture is sieved to remove coarse particles.
  • the number is 80 mesh to 150 mesh, preferably 1
  • the fifth group adding 0.5 parts by weight to the toner masterbatch obtained in the third group premixing process, having a particle diameter of 7 nm to 2
  • ester is mixed in a mixer (such as a Henschel mixer) at 600 rpm for 3 minutes, then mixed at 1200 rpm for 2 minutes, and the mixture is sieved to remove coarse particles.
  • the number is 80 mesh to 150 mesh, preferably 1
  • the sixth group adding 0.5 parts by weight to the toner masterbatch obtained in the third group premixing process, having a particle diameter of 7 nm to 2
  • ester is mixed in a mixer (such as a Henschel mixer) at 600 rpm for 3 minutes, then mixed at 1200 rpm for 3 minutes, and the mixture is sieved to remove coarse particles.
  • the number is 80 mesh to 150 mesh, preferably 1
  • Group 7 adding 0.5 parts by weight to the toner masterbatch obtained in the third group premixing process, having a particle diameter of 7 nm to 2
  • ester is mixed in a mixer (such as a Henschel mixer) at 600 rpm for 3 minutes, then mixed at 1200 rpm for 4 minutes, and the mixture is sieved to remove coarse particles.
  • the number is 80 mesh to 150 mesh, preferably 1
  • a positively charged non-magnetic toner A4 was obtained.
  • the positive non-magnetic toners A1, A2, A3, and A4 were respectively loaded into a TN580 toner cartridge, and a printing test was performed on the HL-5240 printer. The test results are shown in FIG.
  • the bursting process of the positively-charged non-magnetic toner is the result of the selection of the raw materials, the process and the equipment, and the slight difference in the process affects the charge amount and fluidity of the toner. Finally, it is reflected in the printing effect.
  • the invention successfully solves the problems of OPC ghosting, bottom ash and blackboard smearing appearing in the HL-5240 printer by the selection of materials and the improvement of the process.
  • a method for preparing a positively-charged non-magnetic toner of the present invention by adding an additive to a toner masterbatch to change a charge amount and fluidity of a toner master batch, and performing a toner master batch by a pre-mixing step Premixing, post-mixing the toner masterbatch and additives through a post-mixing step, changing the distribution and embedding of the additive in the positively charged non-magnetic toner, and also changing the charge amount and fluidity.
  • the invention combines the selection and mixing process of the raw materials to prepare a positively charged non-magnetic toner with good printing quality.
  • the positive electroless non-magnetic toner prepared by the present invention is loaded into a toner cartridge for printing test, and can solve the problems of OPC ghosting, bottom ash, and blackboard smearing which are often caused by the existing powder cartridge.

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  • General Physics & Mathematics (AREA)
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Abstract

Provided is a preparation method for a positively charged non-magnetic toner, wherein the positively charged non-magnetic toner includes a toner masterbatch and an additive. The toner masterbatch comprises 100 parts by weight of a styrene-acrylic resin, 3 parts by weight of a mold release agent, 6 parts by weight of a coloring agent, and 3 parts by weight of a charge controlling agent. The additive comprises 0.5 parts by weight of a small particle size hydrophobic silica having a particle size of 7 nm to 20 nm, 0.4 parts by weight of a large particle size hydrophobic silica having a particle size of 40 nm to 200 nm, 0.7 parts by weight of barium titanate, and 0.3 parts by weight of a polymethyl methacrylate. The preparation method comprises a pre-mixing step and a post-mixing step.

Description

正电非磁性色调剂的制备方法  Method for preparing positively charged non-magnetic toner
技术领域  Technical field
[0001] 本发明涉及一种色调剂的制备方法, 特别涉及一种正电非磁性色调剂的制备方 法。 本发明是基于申请日为 2017年 04月 12日, 申请号为 CN201710235981.1的中 国发明专利, 该专利的内容引入本文作为参考。  [0001] The present invention relates to a method of preparing a toner, and more particularly to a method of preparing a positively charged non-magnetic toner. The present invention is based on a Chinese invention patent whose application date is April 12, 2017, and whose application number is CN201710235981.1, the contents of which are incorporated herein by reference.
背景技术  Background technique
[0002] 现有的打印机一般包括两大类, 激光打印机和喷墨打印机, 激光打印机相较于 喷墨打印机具备打印速度快、 打印成本低等优点, 因此被广泛地应用于办公场 所, 特别是近年来彩色激光打印的普及, 激光打印的市场越来越大, 而激光打 印机所使用的原装色调剂 (通常也称为碳粉) 往往价格较高, 限制了用户的使 用。  [0002] Existing printers generally include two major categories, laser printers and inkjet printers. Laser printers are widely used in office workplaces, especially in inkjet printers, which have the advantages of fast printing speed and low printing cost. In recent years, the popularity of color laser printing has become increasingly large, and the original toners (also commonly referred to as toners) used in laser printers tend to be expensive and limit the use of users.
[0003] 通用耗材企业生产的兼容耗材因其价格低廉受到广大用户的青睐, 然而研究人 员在幵发兄弟激光打印机 HL-5240打印机的 TN580粉盒的色调剂吋, 在打印测试 过程中容易出现 OPC重影、 底灰和黑板拖尾等问题, 特别是寿命测试后期显影辊 出现上粉不良, 黑板拖尾严重, 仅通过调整色调剂的配方和改变添加剂均难以 完全解决上述问题。  [0003] The compatible consumables produced by general consumables companies are favored by the majority of users because of their low price. However, the researchers are licking the toner of the TN580 toner cartridge of the Brother Laser Printer HL-5240 printer, which is prone to OPC during the printing test. Problems such as ghosting, bottom ash and blackboard smearing, especially in the late development of the life test, the development roller has a poor powder, and the blackboard has a serious tailing. It is difficult to completely solve the above problem only by adjusting the toner formulation and changing the additive.
技术问题 technical problem
[0004] 本发明的目的是提供一种打印效果良好的正电非磁性色调剂的制备方法。  [0004] An object of the present invention is to provide a method for preparing a positively-charged non-magnetic toner having a good printing effect.
[0005] 技术解决手段 [0005] Technical solutions
[0006] 为了实现上述目的, 本发明提供一种正电非磁性色调剂的制备方法, 其中, 正 电非磁性色调剂包括色调剂母料和添加剂; 制备方法包括预混步骤和后混步骤 ; 预混步骤包括, 首先将色调剂母料在混合机中以 600转 /分钟的转速混合 2分钟 , 然后再以 1200转 /分钟的转速混合 2分钟; 后混步骤包括, 首先向预混步骤中得 到的色调剂母料混合物中添加添加剂, 在混合机中以 600转 /分钟的转速混合 2分 钟至 3分钟, 然后再以 1200转 /分钟的转速混合 2分钟至 4分钟。 [0007] 进一步的方案是, 色调剂母料包括 100重量份的苯丙树脂、 3重量份的脱模剂、[0006] In order to achieve the above object, the present invention provides a method for preparing a positively-charged non-magnetic toner, wherein the positively-charged non-magnetic toner includes a toner master batch and an additive; and the preparation method includes a pre-mixing step and a post-mixing step; The premixing step includes first mixing the toner masterbatch in a mixer at 600 rpm for 2 minutes and then mixing at 1200 rpm for 2 minutes; the postmixing step includes, first, the premixing step. An additive was added to the obtained toner master batch mixture, and mixed in a mixer at 600 rpm for 2 minutes to 3 minutes, and then mixed at 1200 rpm for 2 minutes to 4 minutes. [0007] Further, the toner master batch comprises 100 parts by weight of styrene-acrylic resin, 3 parts by weight of a release agent,
6重量份的着色剂和 3重量份的电荷控制剂。 6 parts by weight of the colorant and 3 parts by weight of the charge control agent.
[0008] 进一步的方案是, 添加剂包括 0.5重量份粒径为 7纳米至 20纳米的小粒径疏水性 二氧化硅、 0.4重量份粒径为 40纳米至 200纳米的大粒径疏水性二氧化硅、 0.7重 量份的钛酸钡和 0.3重量份的聚甲基丙烯酸甲酯。 [0008] A further solution is that the additive comprises 0.5 parts by weight of small particle size hydrophobic silica having a particle diameter of 7 nm to 20 nm, and 0.4 parts by weight of large particle size hydrophobic dioxide having a particle diameter of 40 nm to 200 nm. Silicon, 0.7 parts by weight of barium titanate and 0.3 parts by weight of polymethyl methacrylate.
[0009] 进一步的方案是, 后混步骤中, 首先以 600转 /分钟的转速混合 2分钟, 然后再 以 1200转 /分钟的转速混合 2分钟。 [0009] A further solution is that in the post-mixing step, the mixture is first mixed at 600 rpm for 2 minutes and then at 1200 rpm for 2 minutes.
[0010] 一个替代的方案是, 后混步骤中, 首先以 600转 /分钟的转速混合 3分钟, 然后 再以 1200转 /分钟的转速混合 2分钟。 [0010] An alternative is to mix the mixture for 3 minutes at 600 rpm for 3 minutes and then for 2 minutes at 1200 rpm.
[0011] 一个替代的方案是, 后混步骤中, 首先以 600转 /分钟的转速混合 3分钟, 然后 再以 1200转 /分钟的转速混合 3分钟。 [0011] An alternative solution is to first mix at 600 rpm for 3 minutes and then at 1200 rpm for 3 minutes.
[0012] 一个替代的方案是, 后混步骤中, 首先以 600转 /分钟的转速混合 3分钟, 然后 再以 1200转 /分钟的转速混合 4分钟。 [0012] Alternatively, in the post-mixing step, the mixture is first mixed at 600 rpm for 3 minutes and then at 1200 rpm for 4 minutes.
[0013] 进一步的方案是, 预混步骤还包括: 熔融混炼步骤, 将混合后的色调剂母料混 合物在混炼机中熔融混炼成混炼物, 控制混炼的温度在 100摄氏度至 140摄氏度 之间; 冷却步骤, 将混炼物冷却至室温; 粉碎分级步骤, 将冷却后的混炼物粉 碎成颗粒, 并在颗粒中分级出直径为 5微米至 20微米的色调剂母料。 [0013] Further, the pre-mixing step further comprises: a melt-kneading step of melt-kneading the mixed toner masterbatch mixture into a kneaded product in a kneader to control the temperature of the kneading at 100 degrees Celsius to Between 140 degrees Celsius; a cooling step, cooling the kneaded material to room temperature; a pulverizing and grading step, pulverizing the cooled kneaded material into granules, and grading a toner masterbatch having a diameter of 5 μm to 20 μm in the granules.
[0014] 更进一步的方案是, 后混步骤还包括: 筛选步骤, 将后混得到的色调剂母料和 添加剂混合物过筛去除粗颗粒, 筛网目数为 80目至 150目, 优选为 100目。 [0014] Still further, the post-mixing step further comprises: a screening step of sieving the toner masterbatch and the additive mixture obtained by post-mixing to remove coarse particles, the mesh number of which is 80 mesh to 150 mesh, preferably 100 Head.
问题的解决方案  Problem solution
发明的有益效果  Advantageous effects of the invention
有益效果  Beneficial effect
[0015] 本发明的有益效果是: 通过在色调剂母料中加入添加剂, 以改变色调剂母料的 带电量和流动性, 并通过预混步骤对色调剂母料进行预混合, 通过后混步骤对 色调剂母料和添加剂进行后混合, 改变添加剂在正电非磁性色调剂中的分布和 嵌入程度, 同吋也能改变其带电量和流动性。 本发明通过原材料的选择和混合 工艺配合, 制备出打印品质良好的正电非磁性色调剂。  [0015] The beneficial effects of the present invention are: by adding an additive to the toner masterbatch to change the charge amount and fluidity of the toner masterbatch, and premixing the toner masterbatch by a pre-mixing step, and passing the post-mixing The step of post-mixing the toner masterbatch and the additive changes the distribution and embedding of the additive in the positively charged non-magnetic toner, and the same can also change its charge amount and fluidity. The invention combines the selection of raw materials and the mixing process to prepare a positively charged non-magnetic toner having good printing quality.
对附图的简要说明 附图说明 Brief description of the drawing DRAWINGS
[0016] 图 1是 4组不同组分及含量的正电非磁性色调剂实施例的配方表。  [0016] FIG. 1 is a formulation of four sets of positively charged non-magnetic toner embodiments of different compositions and levels.
[0017] 图 2是实施例 1至实施例 4的正电非磁性色调剂的打印测试结果表。  2 is a print test result table of the positively-charged non-magnetic toners of Examples 1 to 4.
[0018] 图 3是实施例 4的色调剂母料分三组进行预混的预混工艺参数表。  3 is a table of premixing process parameters for premixing the toner master batches of Example 4 in three groups. [0018] FIG.
[0019] 图 4是三组预混后的实施例 4的色调剂母料的打印测试结果表。  4 is a table showing the results of printing test of the toner master batches of the three groups of the premixed Example 4. [0019] FIG.
[0020] 图 5是将实施例 4的添加剂加入到第三组预混工艺得到的色调剂母料中进行后混 试验的后混工艺参数表。  5 is a post-mixing process parameter table in which the additive of Example 4 is added to the toner master batch obtained by the third group premixing process for post-mixing test. [0020] FIG.
[0021] 图 6是经过后混得到的正电非磁性色调剂的打印测试结果表。 6 is a print test result table of a positively charged non-magnetic toner obtained by post-mixing.
[0022] 以下结合附图及实施例对本发明作进一步说明。 [0022] The present invention will be further described below in conjunction with the accompanying drawings and embodiments.
本发明的实施方式 Embodiments of the invention
[0023] 本发明的正电非磁性色调剂包括色调剂母料和添加剂, 色调剂母料包括苯丙树 脂、 脱模剂、 着色剂和电荷控制剂, 添加剂包括二氧化硅、 钛酸钡和聚甲基丙 烯酸甲酯, 发明人通过调整配方, 共制备出 4组正电非磁性色调剂, 各组分含量 参见图 1 () 其中, 细颗粒二氧化硅的粒径在 7纳米至 20纳米之间, 大颗粒二氧化 硅的粒径在 40纳米至 200纳米之间, 细颗粒二氧化硅和大颗粒二氧化硅的表面均 经过疏水性处理。 本发明中, 着色剂除了碳黑外, 还可使用花青黑、 铁酸盐、 苯胺黑等, 脱模剂使用的蜡可以是石蜡、 低分子聚丙烯蜡、 低分子聚乙烯蜡、 巴西棕榈蜡等, 电荷控制剂除了油溶性苯胺黑外, 还可使用季铵盐等。 [0023] The positively-charged non-magnetic toner of the present invention includes a toner masterbatch including a styrene-acrylic resin, a mold release agent, a colorant, and a charge control agent, and the additive includes silica, barium titanate, and an additive. Polymethyl methacrylate, the inventors prepared a total of four sets of positively charged non-magnetic toners by adjusting the formula. The content of each component is shown in Fig. 1 (), wherein the particle size of fine-grained silica is from 7 nm to 20 nm. Between, the particle size of the large particle silica is between 40 nm and 200 nm, and the surfaces of the fine particle silica and the large particle silica are both subjected to hydrophobic treatment. In the present invention, the coloring agent may be used in addition to carbon black, such as cyanine black, ferrite, aniline black, etc., and the wax used for the release agent may be paraffin wax, low molecular weight polypropylene wax, low molecular weight polyethylene wax, and Brazilian palm. A wax or the like, a charge control agent may be a quaternary ammonium salt or the like in addition to the oil-soluble aniline black.
[0024] 将实施例 1至实施例 4的正电非磁性色调剂装入 TN580粉盒中, 在 HL-5240打印 机上进行打印测试, 测试结果参见图 2。 [0024] The positively charged non-magnetic toners of Examples 1 to 4 were placed in a TN580 toner cartridge, and a printing test was performed on an HL-5240 printer. The test results are shown in FIG.
[0025] 其中, OPC重影是指打印文字的下方出现重复性文字的现象。 [0025] wherein, OPC ghosting refers to a phenomenon in which repetitive characters appear below the printed text.
[0026] BG即底灰值, 底灰是指非显影区域出现灰蒙蒙的情况, 可通过灰度仪测量打 印纸上空白区域的值与被另外的纸张覆盖的区域 (未经过转印的区域) 的值的 差值来获得, BG的数值越小说明打印效果越好。 [0026] BG is the bottom gray value, and bottom ash refers to the case where the non-developing area is grayed out, and the value of the blank area on the printing paper and the area covered by the additional paper (the untransferred area) can be measured by the gradation meter. The difference between the values of the values is obtained. The smaller the value of BG, the better the printing effect.
[0027] 黑板拖尾是指打印全黑板, 黑板下方的局部出现灰蒙蒙的情况。 [0027] Blackboard smearing refers to printing a full blackboard, and the situation under the blackboard is grayed out.
[0028] 可见, 按照实施例 4的配方制备的正电非磁性色调剂的质量最佳, 但是还是存 在 OPC重影和黑板拖尾的现象。 [0029] 发明人对实施例 4的配方继续进行研究, 通过工艺的改进, 彻底解决了上述问 题。 [0028] It can be seen that the quality of the positively charged non-magnetic toner prepared according to the formulation of Example 4 is the best, but there is still a phenomenon of OPC ghosting and blackboard smearing. [0029] The inventors continued to study the formulation of Example 4, and solved the above problems thoroughly by the improvement of the process.
[0030] 预混工艺: 将实施例 4的色调剂母料按照表 1中的配方进行 3组预混试验, 预混 工艺参见图 3。 其中, R1代表转速 1, 其单位 rpm为转 /分钟, T1代表 R1对应的吋 间, 单位为分钟; R1代表转速 2, 其单位也为转 /分钟, T2代表 R2对应的吋间, 单位为分钟。  [0030] Premixing process: The toner master batch of Example 4 was subjected to three sets of premixing tests in accordance with the formulation in Table 1, and the premixing process is shown in Fig. 3. Wherein, R1 represents the rotational speed 1, the unit rpm is the revolution/minute, T1 represents the inter-turn of R1, and the unit is minute; R1 represents the rotational speed 2, and the unit is also the revolution/minute, and T2 represents the inter-turn of R2, and the unit is minute.
[0031] 第一组: 将 100份的苯丙树脂、 3份的蜡、 3份的油溶性苯胺黑和 6份的碳黑在混 合机 (如亨舍尔混合机) 中以 600转 /分钟的转速混合 5分钟, 形成色调剂母料混 合物; 然后将混合后的色调剂母料混合物在混炼机 (如平行双螺杆混炼机) 中 熔融混炼成混炼物, 控制混炼的温度在 100摄氏度至 140摄氏度之间; 接着将混 炼物冷却至室温; 最后将冷却后的混炼物粉碎成颗粒, 并在所述颗粒中分级出 直径为 5微米至 20微米的色调剂母料。  [0031] The first group: 100 parts of styrene resin, 3 parts of wax, 3 parts of oil-soluble aniline black and 6 parts of carbon black in a mixer (such as a Henschel mixer) at 600 rpm The rotation speed is mixed for 5 minutes to form a toner masterbatch mixture; then the mixed toner masterbatch mixture is melt-kneaded into a kneaded product in a kneader (such as a parallel twin-screw kneader) to control the kneading temperature. Between 100 degrees Celsius and 140 degrees Celsius; then cooling the mixture to room temperature; finally, pulverizing the cooled kneaded material into granules, and grading the toner masterbatch having a diameter of 5 micrometers to 20 micrometers in the particles .
[0032] 第二组: 将 100份的苯丙树脂、 3份的蜡、 3份的油溶性苯胺黑和 6份的碳黑在混 合机 (如亨舍尔混合机) 中以 1200转 /分钟的转速混合 5分钟, 形成色调剂母料混 合物; 然后将混合后的色调剂母料混合物在混炼机 (如平行双螺杆混炼机) 中 熔融混炼成混炼物, 控制混炼的温度在 100摄氏度至 140度之间; 接着将混炼物 冷却至室温; 最后将冷却后的混炼物粉碎成颗粒, 并在所述颗粒中分级出直径 为 5微米至 20微米的色调剂母料。  [0032] Group 2: 100 parts of styrene resin, 3 parts of wax, 3 parts of oil-soluble aniline black and 6 parts of carbon black in a mixer (such as a Henschel mixer) at 1200 rpm The rotation speed is mixed for 5 minutes to form a toner masterbatch mixture; then the mixed toner masterbatch mixture is melt-kneaded into a kneaded product in a kneader (such as a parallel twin-screw kneader) to control the kneading temperature. Between 100 degrees Celsius and 140 degrees; the mixture is then cooled to room temperature; finally, the cooled kneaded material is pulverized into granules, and a toner masterbatch having a diameter of 5 micrometers to 20 micrometers is fractionated in the granules. .
[0033] 第三组: 将 100份的苯丙树脂、 3份的蜡、 3份的油溶性苯胺黑和 6份的碳黑在混 合机 (如亨舍尔混合机) 中先以 600转 /分钟的转速混合 2分钟, 再以 1200转 /分钟 的转速混合 5分钟, 形成色调剂母料混合物; 然后将混合后的色调剂母料混合物 在混炼机 (如平行双螺杆混炼机) 中熔融混炼成混炼物, 控制混炼的温度在 100 摄氏度至 140度之间; 接着将混炼物冷却至室温; 最后将冷却后的混炼物粉碎成 颗粒, 并在所述颗粒中分级出直径为 5微米至 20微米的色调剂母料。  [0033] The third group: 100 parts of styrene resin, 3 parts of wax, 3 parts of oil-soluble aniline black and 6 parts of carbon black in a mixer (such as a Henschel mixer) first 600 rpm / Mixing at a minute speed for 2 minutes, mixing at 1200 rpm for 5 minutes to form a toner masterbatch mixture; then mixing the mixed toner masterbatch in a mixer (such as a parallel twin-screw mixer) Melt and knead into a kneaded product, control the mixing temperature between 100 ° C and 140 ° C; then cool the kneaded material to room temperature; finally, the cooled kneaded material is pulverized into particles and classified in the particles A toner masterbatch having a diameter of from 5 micrometers to 20 micrometers is produced.
[0034] 取第一组、 第二组和第三组工艺得到的色调剂母料分别装入 TN580粉盒中, 在 HL-5240打印机上进行打印测试, 测试结果参见图 4。  [0034] The toner masterbatch obtained by the first group, the second group and the third group process is respectively loaded into the TN580 toner cartridge, and the printing test is performed on the HL-5240 printer. The test results are shown in FIG.
[0035] 由图 4的测试结果可知, 预混工艺中, 转速和吋间的不同, 对 OPC重影和 BG值 影响不大, 对黑板拖尾有一定的影响, 第三组预混工艺解决了黑板拖尾的问题 , 但是还是存在 OPC重影的问题, 发明人对第三组预混工艺得到的色调剂母料进 行了后混工艺试验。 [0035] It can be seen from the test result of FIG. 4 that in the premixing process, the difference between the rotation speed and the turn has little effect on the OPC ghost and the BG value, and has a certain influence on the blackboard tailing, and the third group premixing process is solved. Blackboard trailing problem However, there is still the problem of OPC ghosting. The inventors conducted a post-mixing process test on the toner masterbatch obtained from the third premixing process.
[0036] 后混工艺: 将实施例 4的添加剂按照图 1的配方加入到第三组预混工艺得到的色 调剂母料中, 进行后混试验, 后混工艺参见图 5。  [0036] Post-mixing process: The additive of Example 4 was added to the color masterbatch obtained in the third group of pre-mixing processes according to the formulation of Fig. 1 to carry out a post-mixing test, and the post-mixing process is shown in Fig. 5.
[0037] 第四组: 向第三组预混工艺得到的色调剂母料中加入 0.5重量份粒径为 7纳米至 2[0037] The fourth group: adding 0.5 parts by weight to the toner masterbatch obtained in the third group premixing process, having a particle diameter of 7 nm to 2
0纳米的小粒径疏水性二氧化硅、 0.4重量份粒径为 40纳米至 200纳米的大粒径疏 水性二氧化硅、 0.7重量份的钛酸钡和 0.3重量份的聚甲基丙烯酸甲酯, 在混合机 (如亨舍尔混合机) 中以 600转 /分钟的转速先混合 2分钟, 再以 1200转 /分钟的转 速先混合 2分钟, 将混合物过筛去除粗颗粒, 筛网目数为 80目至 150目, 优选为 10 nm of small particle size hydrophobic silica, 0.4 parts by weight of large particle size hydrophobic silica having a particle diameter of 40 nm to 200 nm, 0.7 part by weight of barium titanate, and 0.3 part by weight of polymethyl methacrylate The ester is mixed in a mixer (such as a Henschel mixer) at 600 rpm for 2 minutes, then mixed at 1200 rpm for 2 minutes, and the mixture is sieved to remove coarse particles. The number is 80 mesh to 150 mesh, preferably 1
00目, 得到正电非磁性色调剂 Al。 00 mesh, a positively charged non-magnetic toner Al was obtained.
[0038] 第五组: 向第三组预混工艺得到的色调剂母料中加入 0.5重量份粒径为 7纳米至 2[0038] The fifth group: adding 0.5 parts by weight to the toner masterbatch obtained in the third group premixing process, having a particle diameter of 7 nm to 2
0纳米的小粒径疏水性二氧化硅、 0.4重量份粒径为 40纳米至 200纳米的大粒径疏 水性二氧化硅、 0.7重量份的钛酸钡和 0.3重量份的聚甲基丙烯酸甲酯, 在混合机 (如亨舍尔混合机) 中以 600转 /分钟的转速先混合 3分钟, 再以 1200转 /分钟的转 速先混合 2分钟, 将混合物过筛去除粗颗粒, 筛网目数为 80目至 150目, 优选为 10 nm of small particle size hydrophobic silica, 0.4 parts by weight of large particle size hydrophobic silica having a particle diameter of 40 nm to 200 nm, 0.7 part by weight of barium titanate, and 0.3 part by weight of polymethyl methacrylate The ester is mixed in a mixer (such as a Henschel mixer) at 600 rpm for 3 minutes, then mixed at 1200 rpm for 2 minutes, and the mixture is sieved to remove coarse particles. The number is 80 mesh to 150 mesh, preferably 1
00目, 得到正电非磁性色调剂 A2。 At 00 mesh, a positively charged non-magnetic toner A2 was obtained.
[0039] 第六组: 向第三组预混工艺得到的色调剂母料中加入 0.5重量份粒径为 7纳米至 2[0039] The sixth group: adding 0.5 parts by weight to the toner masterbatch obtained in the third group premixing process, having a particle diameter of 7 nm to 2
0纳米的小粒径疏水性二氧化硅、 0.4重量份粒径为 40纳米至 200纳米的大粒径疏 水性二氧化硅、 0.7重量份的钛酸钡和 0.3重量份的聚甲基丙烯酸甲酯, 在混合机 (如亨舍尔混合机) 中以 600转 /分钟的转速先混合 3分钟, 再以 1200转 /分钟的转 速先混合 3分钟, 将混合物过筛去除粗颗粒, 筛网目数为 80目至 150目, 优选为 10 nm of small particle size hydrophobic silica, 0.4 parts by weight of large particle size hydrophobic silica having a particle diameter of 40 nm to 200 nm, 0.7 part by weight of barium titanate, and 0.3 part by weight of polymethyl methacrylate The ester is mixed in a mixer (such as a Henschel mixer) at 600 rpm for 3 minutes, then mixed at 1200 rpm for 3 minutes, and the mixture is sieved to remove coarse particles. The number is 80 mesh to 150 mesh, preferably 1
00目, 得到正电非磁性色调剂 A3。 At 00 mesh, a positively charged non-magnetic toner A3 was obtained.
[0040] 第七组: 向第三组预混工艺得到的色调剂母料中加入 0.5重量份粒径为 7纳米至 2[0040] Group 7: adding 0.5 parts by weight to the toner masterbatch obtained in the third group premixing process, having a particle diameter of 7 nm to 2
0纳米的小粒径疏水性二氧化硅、 0.4重量份粒径为 40纳米至 200纳米的大粒径疏 水性二氧化硅、 0.7重量份的钛酸钡和 0.3重量份的聚甲基丙烯酸甲酯, 在混合机 (如亨舍尔混合机) 中以 600转 /分钟的转速先混合 3分钟, 再以 1200转 /分钟的转 速先混合 4分钟, 将混合物过筛去除粗颗粒, 筛网目数为 80目至 150目, 优选为 10 nm of small particle size hydrophobic silica, 0.4 parts by weight of large particle size hydrophobic silica having a particle diameter of 40 nm to 200 nm, 0.7 part by weight of barium titanate, and 0.3 part by weight of polymethyl methacrylate The ester is mixed in a mixer (such as a Henschel mixer) at 600 rpm for 3 minutes, then mixed at 1200 rpm for 4 minutes, and the mixture is sieved to remove coarse particles. The number is 80 mesh to 150 mesh, preferably 1
00目, 得到正电非磁性色调剂 A4。 [0041] 取正电非磁性色调剂 Al、 A2、 A3和 A4分别装入 TN580粉盒中, 在 HL-5240打 印机上进行打印测试, 测试结果参见图 6。 At 00 mesh, a positively charged non-magnetic toner A4 was obtained. [0041] The positive non-magnetic toners A1, A2, A3, and A4 were respectively loaded into a TN580 toner cartridge, and a printing test was performed on the HL-5240 printer. The test results are shown in FIG.
[0042] 由图 6的测试结果可知, 后混工艺中, 转速和吋间的不同, 对 OPC重影和黑板 拖尾产生影响, 因为后混工艺影响了添加剂在正电非磁性色调剂中的分布和嵌 入程度。 其中, 第六组后混工艺得到的正电非磁性色调剂品质最优, 解决了原 有的色调剂的问题。 [0042] From the test results of FIG. 6, it can be seen that in the post-mixing process, the difference between the rotational speed and the turn-to-turn affects the OPC ghost and the blackboard tailing because the post-mixing process affects the additive in the positively-charged non-magnetic toner. Distribution and embedding. Among them, the positive electric non-magnetic toner obtained by the sixth group of post-mixing process has the best quality, and solves the problem of the original toner.
[0043] 综上所述, 正电非磁性色调剂的幵发过程是原材料的选择、 工艺和设备高度配 合的结果, 其工艺的微小差异, 都会对色调剂的带电量和流动性产生影响, 最 终体现在打印效果上。 本发明通过对材料的选择和工艺的改进, 成功的解决了 T N580粉盒在 HL-5240打印机中出现的 OPC重影、 底灰和黑板拖尾的问题。  [0043] In summary, the bursting process of the positively-charged non-magnetic toner is the result of the selection of the raw materials, the process and the equipment, and the slight difference in the process affects the charge amount and fluidity of the toner. Finally, it is reflected in the printing effect. The invention successfully solves the problems of OPC ghosting, bottom ash and blackboard smearing appearing in the HL-5240 printer by the selection of materials and the improvement of the process.
[0044] 本发明的技术构思并不仅限于上述实施例, 还可以依据本发明的构思得到许多 不同的具体方案, 如对各物料的配比进行合理范围内的调整、 对混合吋搅拌的 速度及吋间在合理范围内进行调整等等, 此等微小改变以及等效变换均应包含 在权利要求所述范围之内。  [0044] The technical idea of the present invention is not limited to the above embodiments, and many different specific solutions can be obtained according to the concept of the present invention, such as adjusting the ratio of each material within a reasonable range, and the speed of mixing the mixing and mixing. Such minor changes and equivalent transformations are intended to be included within the scope of the claims.
[0045] 工业应用性  Industrial Applicability
[0046] 本发明的正电非磁性色调剂的制备方法, 通过在色调剂母料中加入添加剂, 以 改变色调剂母料的带电量和流动性, 并通过预混步骤对色调剂母料进行预混合 , 通过后混步骤对色调剂母料和添加剂进行后混合, 改变添加剂在正电非磁性 色调剂中的分布和嵌入程度, 同吋也能改变其带电量和流动性。 本发明通过原 材料的选择和混合工艺配合, 制备出打印品质良好的正电非磁性色调剂。 通过 本发明制备的正电非磁性色调剂装入粉盒中进行打印测试, 可以解决现有的粉 盒常出现的 OPC重影、 底灰和黑板拖尾的问题。  [0046] A method for preparing a positively-charged non-magnetic toner of the present invention, by adding an additive to a toner masterbatch to change a charge amount and fluidity of a toner master batch, and performing a toner master batch by a pre-mixing step Premixing, post-mixing the toner masterbatch and additives through a post-mixing step, changing the distribution and embedding of the additive in the positively charged non-magnetic toner, and also changing the charge amount and fluidity. The invention combines the selection and mixing process of the raw materials to prepare a positively charged non-magnetic toner with good printing quality. The positive electroless non-magnetic toner prepared by the present invention is loaded into a toner cartridge for printing test, and can solve the problems of OPC ghosting, bottom ash, and blackboard smearing which are often caused by the existing powder cartridge.

Claims

权利要求书 Claim
正电非磁性色调剂的制备方法, 其特征在于: A method for preparing a positively-charged non-magnetic toner, characterized in that:
所述正电非磁性色调剂包括色调剂母料和添加剂; The positively charged non-magnetic toner includes a toner master batch and an additive;
所述制备方法包括预混步骤和后混步骤; The preparation method includes a pre-mixing step and a post-mixing step;
所述预混步骤包括: The premixing step includes:
将色调剂母料在混合机中以 600转 /分钟的转速混合 2分钟, 然后再以 1 200转 /分钟的转速混合 2分钟; The toner masterbatch was mixed in a mixer at 600 rpm for 2 minutes, and then mixed at 1 200 rpm for 2 minutes;
所述后混步骤包括: The post-mixing step includes:
向所述预混步骤中得到的色调剂母料混合物中添加所述添加剂, 在混 合机中以 600转 /分钟的转速混合 2分钟至 3分钟, 然后再以 1200转 /分钟 的转速混合 2分钟至 4分钟。 Adding the additive to the toner masterbatch mixture obtained in the pre-mixing step, mixing in a mixer at 600 rpm for 2 minutes to 3 minutes, and then mixing at 1200 rpm for 2 minutes. Up to 4 minutes.
根据权利要求 1所述的制备方法, 其特征在于: The preparation method according to claim 1, wherein:
所述色调剂母料包括 100重量份的苯丙树脂、 3重量份的脱模剂、 6重 量份的着色剂和 3重量份的电荷控制剂。 The toner master batch comprises 100 parts by weight of a styrene-acrylic resin, 3 parts by weight of a releasing agent, 6 parts by weight of a coloring agent, and 3 parts by weight of a charge control agent.
根据权利要求 2所述的制备方法, 其特征在于: The preparation method according to claim 2, wherein:
所述添加剂包括 0.5重量份粒径为 7纳米至 20纳米的小粒径疏水性二氧 化硅、 0.4重量份粒径为 40纳米至 200纳米的大粒径疏水性二氧化硅、The additive comprises 0.5 parts by weight of a small particle size hydrophobic silica having a particle diameter of 7 nm to 20 nm, 0.4 parts by weight of a large particle size hydrophobic silica having a particle diameter of 40 nm to 200 nm,
0.7重量份的钛酸钡和 0.3重量份的聚甲基丙烯酸甲酯。 0.7 parts by weight of barium titanate and 0.3 parts by weight of polymethyl methacrylate.
根据权利要求 1至 3任一项所述的制备方法, 其特征在于: The preparation method according to any one of claims 1 to 3, characterized in that:
所述后混步骤中, 以 600转 /分钟的转速混合 2分钟, 然后再以 1200转 / 分钟的转速混合 2分钟。 In the post-mixing step, the mixture was mixed at 600 rpm for 2 minutes and then mixed at 1200 rpm for 2 minutes.
根据权利要求 1至 3任一项所述的制备方法, 其特征在于: The preparation method according to any one of claims 1 to 3, characterized in that:
所述后混步骤中, 以 600转 /分钟的转速混合 3分钟, 然后再以 1200转 / 分钟的转速混合 2分钟。 In the post-mixing step, the mixture was mixed at 600 rpm for 3 minutes and then mixed at 1200 rpm for 2 minutes.
根据权利要求 1至 3任一项所述的制备方法, 其特征在于: The preparation method according to any one of claims 1 to 3, characterized in that:
所述后混步骤中, 以 600转 /分钟的转速混合 3分钟, 然后再以 1200转 / 分钟的转速混合 3分钟。 In the post-mixing step, the mixture was mixed at 600 rpm for 3 minutes and then mixed at 1200 rpm for 3 minutes.
根据权利要求 1至 3任一项所述的制备方法, 其特征在于: 所述后混步骤中, 以 600转 /分钟的转速混合 3分钟, 然后再以 1200转 / 分钟的转速混合 4分钟。 The preparation method according to any one of claims 1 to 3, characterized in that: In the post-mixing step, the mixture was mixed at 600 rpm for 3 minutes and then mixed at 1200 rpm for 4 minutes.
[权利要求 8] 根据权利要求 1至 7任一项所述的制备方法, 其特征在于: [Claim 8] The preparation method according to any one of claims 1 to 7, characterized in that:
所述预混步骤还包括  The premixing step further includes
熔融混炼步骤, 将混合后的色调剂母料混合物在混炼机中熔融混炼成 混炼物, 控制混炼的温度在 100摄氏度至 140摄氏度之间;  In the melt-kneading step, the mixed toner masterbatch mixture is melt-kneaded into a kneaded product in a kneader, and the temperature for controlling the kneading is between 100 degrees Celsius and 140 degrees Celsius;
冷却步骤, 将所述混炼物冷却至室温;  a cooling step of cooling the kneaded material to room temperature;
粉碎分级步骤, 将冷却后的混炼物粉碎成颗粒, 并在所述颗粒中分级 出直径为 5微米至 20微米的色调剂母料。  The pulverization and classification step, the cooled kneaded product is pulverized into granules, and a toner master batch having a diameter of 5 μm to 20 μm is classified in the granules.
[权利要求 9] 根据权利要求 1至 8任一项所述的制备方法, 其特征在于: [Claim 9] The preparation method according to any one of claims 1 to 8, characterized in that:
所述后混步骤还包括  The post-mixing step further includes
筛选步骤, 将后混得到的色调剂母料和添加剂混合物过筛去除粗颗粒 , 筛网目数为 80目至 150目之间。  In the screening step, the toner masterbatch and the additive mixture obtained by post-mixing are sieved to remove coarse particles, and the mesh number is between 80 mesh and 150 mesh.
[权利要求 10] 根据权利要求 9所述的制备方法, 其特征在于: [Claim 10] The preparation method according to claim 9, wherein:
所述筛网目数为 100目。  The mesh number is 100 mesh.
PCT/CN2018/082331 2017-04-12 2018-04-09 Preparation method for positively charged non-magnetic toner WO2018188554A1 (en)

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