CN1841216A - 调色剂方法 - Google Patents
调色剂方法 Download PDFInfo
- Publication number
- CN1841216A CN1841216A CNA2006100683901A CN200610068390A CN1841216A CN 1841216 A CN1841216 A CN 1841216A CN A2006100683901 A CNA2006100683901 A CN A2006100683901A CN 200610068390 A CN200610068390 A CN 200610068390A CN 1841216 A CN1841216 A CN 1841216A
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- CN
- China
- Prior art keywords
- toner particle
- sulfonated polyester
- poly
- toner
- coagulator
- Prior art date
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- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 239000011654 magnesium acetate Substances 0.000 description 1
- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
- OTCKOJUMXQWKQG-UHFFFAOYSA-L magnesium bromide Chemical compound [Mg+2].[Br-].[Br-] OTCKOJUMXQWKQG-UHFFFAOYSA-L 0.000 description 1
- 229910001623 magnesium bromide Inorganic materials 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- BLQJIBCZHWBKSL-UHFFFAOYSA-L magnesium iodide Chemical compound [Mg+2].[I-].[I-] BLQJIBCZHWBKSL-UHFFFAOYSA-L 0.000 description 1
- 229910001641 magnesium iodide Inorganic materials 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- WXPNTKUIDRYHOP-UHFFFAOYSA-L magnesium;3-oxobutanoate Chemical compound [Mg+2].CC(=O)CC([O-])=O.CC(=O)CC([O-])=O WXPNTKUIDRYHOP-UHFFFAOYSA-L 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- IKUGFMANZPAVJJ-UHFFFAOYSA-L manganese(2+);3-oxobutanoate Chemical compound [Mn+2].CC(=O)CC([O-])=O.CC(=O)CC([O-])=O IKUGFMANZPAVJJ-UHFFFAOYSA-L 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- QWYFOIJABGVEFP-UHFFFAOYSA-L manganese(ii) iodide Chemical compound [Mn+2].[I-].[I-] QWYFOIJABGVEFP-UHFFFAOYSA-L 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- NYGZLYXAPMMJTE-UHFFFAOYSA-M metanil yellow Chemical group [Na+].[O-]S(=O)(=O)C1=CC=CC(N=NC=2C=CC(NC=3C=CC=CC=3)=CC=2)=C1 NYGZLYXAPMMJTE-UHFFFAOYSA-M 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- SGXHANSUXZAOSN-UHFFFAOYSA-N methyl 2-cyclobutylacetate Chemical compound COC(=O)CC1CCC1 SGXHANSUXZAOSN-UHFFFAOYSA-N 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
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- WNWZKKBGFYKSGA-UHFFFAOYSA-N n-(4-chloro-2,5-dimethoxyphenyl)-2-[[2,5-dimethoxy-4-(phenylsulfamoyl)phenyl]diazenyl]-3-oxobutanamide Chemical compound C1=C(Cl)C(OC)=CC(NC(=O)C(N=NC=2C(=CC(=C(OC)C=2)S(=O)(=O)NC=2C=CC=CC=2)OC)C(C)=O)=C1OC WNWZKKBGFYKSGA-UHFFFAOYSA-N 0.000 description 1
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- 239000012071 phase Substances 0.000 description 1
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 1
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- 229920000058 polyacrylate Chemical group 0.000 description 1
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- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 239000012925 reference material Substances 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
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- YJPVTCSBVRMESK-UHFFFAOYSA-L strontium bromide Chemical compound [Br-].[Br-].[Sr+2] YJPVTCSBVRMESK-UHFFFAOYSA-L 0.000 description 1
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- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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Abstract
公开了一种方法,该方法包括混合磺化聚酯树脂、着色剂和凝结剂;加热获得的磺化聚酯混合物;加入聚金属卤化物和阴离子胶乳以形成涂覆的调色剂粒子;和加热涂覆的调色剂粒子。
Description
技术领域
本公开内容涉及调色剂方法。
背景技术
磺化聚酯(SPE)调色剂粒子是已知的并已用许多类型的材料表面改性,并且在某些情况下,显示摩擦电改进。这些表面处理可能难以再现和可能对放大是不实际的。再现性的主要缺点在于对于要成功的任何表面处理,粒子的胶体性能必须在调色剂粒子表面上存在的所有基团中较好地表征出来。此外,当粒度增加到例如50微米和以上时,表面处理变得更加可再现和放大。在SPE粒子的情况下,在水相中存在大量凝结金属盐如乙酸锌。这反过来在表面处理期间进一步聚集/聚结调色剂尺寸粒子,由此以不可控方式增加粒度。已经计算出仅约1/6的乙酸锌在调色剂粒子中,而剩余的在水相中。因此,可能有价值的是洗涤调色剂粒子几次以除去过量乙酸锌,由此也清洁调色剂粒子的表面并因此从表面除去未知实体。不管存在的乙酸锌数量,SPE调色剂的目标粒度可以为约3-约15微米。每个可以是通用批次到批次再现性中的因素。
如以上讨论的那样,表面处理尽管在小型试验水平下在一定程度上是成功的,但难以放大,如调色剂的体积。外部添加剂部分有帮助,但一旦添加剂离开调色剂粒子,显影成为问题。因此,需要使调色剂粒子的表面对水分较不敏感和大规模制备粒子而不影响显影。
发明内容
本发明的各个方面涉及一种方法,该方法包括混合磺化聚酯树脂、着色剂和凝结剂;加热获得的磺化聚酯混合物;加入聚金属卤化物和阴离子胶乳以形成涂覆的调色剂粒子;和加热涂覆的调色剂粒子;一种方法,该方法包括混合着色剂、磺化聚酯树脂和凝结剂以形成粒度为约1-约5微米的调色剂粒子;加热获得的磺化聚酯调色剂粒子;加入聚金属卤化物和包括乙烯基聚合物树脂的阴离子胶乳;和通过加热将乙烯基聚合物树脂熔凝到调色剂粒子表面;一种方法,该方法包括混合磺化聚酯调色剂粒子与凝结剂以形成核调色剂粒子;和加入聚金属卤化物到核调色剂粒子的表面上以形成涂覆的调色剂粒子;在实施方案中,磺化聚酯调色剂粒子的粒度为约25-约100nm;在实施方案中,核调色剂粒子的粒度为约3-约4微米;一种方法,该方法包括混合磺化聚酯树脂、着色剂和凝结剂的第一部分;加热混合物;和加入凝结剂的第二部分以形成磺化聚酯调色剂粒子;和一种方法,该方法包括混合磺化聚酯树脂、着色剂、蜡和凝结剂;加热获得的磺化聚酯调色剂粒子;加入聚金属卤化物和阴离子胶乳以形成涂覆的调色剂粒子;和加热涂覆的调色剂粒子。
具体实施方式
本公开内容的各个方面涉及一种方法,该方法包括混合磺化聚酯树脂、着色剂和凝结剂,由此形成核磺化聚酯调色剂粒子。然后可以加热核调色剂粒子。公开的方法进一步包括加入聚金属卤化物和阴离子胶乳以形成涂覆的调色剂粒子,然后可以加热该涂覆的调色剂粒子。在实施方案中,第一次加热低于磺化聚酯树脂的Tg而第二次加热高于磺化聚酯树脂的Tg。
在实施方案中,方法涉及包括聚酯树脂如磺化聚酯树脂的核调色剂粒子与包括乙烯基聚合物如苯乙烯丙烯酸酯羧酸的壳的原位制备。由于聚酯树脂可包括磺化基团,它可容易地在水中分散,如在70℃下,并可导致亚微米粒子。此外,由于例如磺化聚酯树脂是水性树脂,来自它的调色剂可以是水分敏感的。
用于公开方法的着色剂可以在着色剂分散体中存在,该分散体包括着色剂、水和表面活性剂,如离子和/或非离子表面活性剂。着色剂可以选自染料和颜料,如在美国专利4,788,123;4,828,956;4,894,308;4,948,686;4,963,455;和4,965,158中公开的那些。颜料的非限制性例子包括黑色、青色、品红色、黄色、绿色、橙色、棕色、紫罗兰色、蓝色、红色、紫色、白色和银色颜料。着色剂的非限制性例子包括炭黑(例如REGAL 330),Flexiverse颜料BFD1121,苯胺黑染料,苯胺蓝,磁铁矿和着色磁铁矿如Mobay磁铁矿MO8029TM,MO8060TM;Columbian磁铁矿;MAPICO BLACKSTM和表面处理的磁铁矿;Pfizer磁铁矿CB4799TM,CB5300TM,CB5600TM,MCX6369TM;Bayer磁铁矿,BAYFERROX 8600TM,8610TM;NorthernPigments磁铁矿,NP-604TM,NP-608TM;Magnox磁铁矿TMB-100TM或TMB-104TM;酞菁,在染料索引中标识为CI60710,CI分散红15的2,9-二甲基-取代的喹吖啶酮和蒽醌染料,在染料索引中标识为CI26050的重氮染料,CI溶剂红19,铜四(十八烷基磺酰胺)酞菁,在染料索引中以CI74160列出的x-铜酞菁颜料,CI颜料蓝,在染料索引中标识为CI69810的Anthradanthrene蓝,特殊蓝X-2137,二芳基化物黄3,3-二氯benzidene乙酰乙酰苯胺,在染料索引中标识为CI12700的单偶氮颜料,CI溶剂黄16,在染料索引中标识为Foron黄SE/GLN的硝基苯基胺磺酰胺,CI分散黄33,2,5-二甲氧基-4-磺酰苯胺苯基偶氮-4’-氯-2,5-二甲氧基乙酰乙酰苯胺,永久黄FGL,颜料黄74,B 15:3青色颜料分散体,购自Sun Chemicals,品红色红色81:3颜料分散体,购自Sun Chemicals,黄色180颜料分散体,购自Sun Chemicals,青色组分等以及其混合物。从SunChemical或Ciba作为含水颜料分散体得到的其它颜料商业来源包括但不限于颜料黄17,颜料黄14,颜料黄93,颜料黄74,颜料紫23,颜料紫1,颜料绿7,颜料橙36,颜料橙21,颜料橙16,颜料红185,颜料红122,颜料红81:3,颜料蓝15:3,和颜料蓝61,和能够再现最大Pantone颜色空间的其它颜料。其它合适的着色剂包括但不限于Cinquasia品红(DuPont),Levanyl黑A-SF(Miles,Bayer),Sunsperse炭黑LHD 9303,Sunsperse蓝BHD 6000和Sunsperse黄YHD 6001,购自Sun Chemicals;Normandy品红RD-2400,永久黄YE0305,永久紫VT2645,Argyle绿XP-111-S,立索复红调色剂,Royal艳红RD-8192,艳绿调色剂GR 0991,和Ortho橙OR 2673,都购自Paul Uhlich;苏丹橙G,联甲苯胺红,和E.D.甲苯胺红,购自Aldrich;苏丹III,苏丹II,和苏丹IV,都购自Matheson,Coleman,Bell;用于Thermoplast NSD PS PA购自Ugine Kuhlman,加拿大的猩红;Bon红C,购自Dominion Color Co.;Lumogen黄D0790,Suco-Gelb L1250,Suco-黄D1355,Paliogen紫5100,Paliogen橙3040,Paliogen黄152,Neopen黄,Paliogen红3871K,Paliogen红3340,Paliogen黄1560,Paliogen紫5890,Paliogen蓝6470,立索猩红4440,立索坚牢猩红L4300,立索猩红D3700,立索坚牢黄0991K,Paliotol黄1840,Heliogen绿L8730,Heliogen蓝L6900,L7202,D6840,D7080,Neopen蓝,Sudan蓝OS,苏丹橙220,和Fanal粉红D4830,都购自BASF;Cinquasia品红,购自DuPont;Novoperm黄FG1,购自Hoechst;Hostaperm粉红E,和PV坚牢蓝B2G01,都购自American Hoechst;Irgalite蓝BCA,和Oracet粉红RF,都购自Ciba-Geigy。也可以采用着色剂的混合物。
当存在时,着色剂可以在调色剂组合物中以任何所需或有效的数量存在,如调色剂组合物的约1%-约25wt%,例如约2%-约15%,和作为进一步的例子约5%-约12wt%,基于调色剂组合物的总重量。然而,数量可以在这些范围以外。
磺化聚酯树脂可包含磺化(SO4 -或SO3 -)基团,该基团可以在受控条件下聚集/聚结成约3.5-约6.5的调色剂尺寸粒子并且例如在凝结剂存在下pH可以为约5.5。磺化聚酯树脂可以在温水中如约70℃分散,并可导致亚微米粒子。磺化聚酯树脂可以是选自如下的聚合物:磺化聚酯如聚(1,2-亚丙基-钠代5-磺基间苯二甲酸酯),聚(亚新戊基-钠代5-磺基间苯二甲酸酯),聚(二亚乙基-钠代5-磺基间苯二甲酸酯),共聚(1,2-亚丙基-钠代5-磺基间苯二甲酸酯)-共聚-(1,2-亚丙基-对苯二甲酸酯-邻苯二甲酸酯),共聚(1,2-亚丙基-二亚乙基钠代5-磺基间苯二甲酸酯)-共聚-(1,2-亚丙基-二亚乙基-对苯二甲酸酯-邻苯二甲酸酯),共聚(亚乙基-亚新戊基-钠代5-磺基间苯二甲酸酯)-共聚-(亚乙基-亚新戊基-对苯二甲酸酯-邻苯二甲酸酯),和共聚(丙氧基化双酚A)-共聚-(丙氧基化双酚A-钠代5-磺基间苯二甲酸酯)。磺化聚酯树脂可以选自线性、支化和结晶的。树脂粒子的尺寸可以为约0.05-约1微米。
可以选择各种二元酸或二元酸酯以形成本公开内容的磺化聚酯树脂,如选自如下的那些:富马酸、丙二酸、衣康酸、2-甲基衣康酸、马来酸、马来酸酐、己二酸、琥珀酸、辛二酸、2-乙基琥珀酸、戊二酸、十二烷基琥珀酸、2-甲基己二酸、庚二酸、壬二酸、癸二酸、对苯二甲酸、间苯二甲酸、邻苯二甲酸、1,2-环己烷二酸、1,3-环己烷二酸、1,4-环己烷二酸、其中烷基包含约2-约22个碳原子的二烷基酯,并可以是丙二酸酯、琥珀酸酯、富马酸酯、衣康酸酯、对苯二甲酸酯、间苯二甲酸酯、邻苯二甲酸酯、环己烷二酸酯及其混合物的酯。二元酸可任选地选择的数量为35mol%-约0.45mol%,基于约100mol%树脂。在实施方案中,二元酸可以选自富马酸、丙二酸、衣康酸、2-甲基衣康酸、马来酸和马来酸酐。
在实施方案中,磺化有机二元酸或二元酸酯的例子包括选自如下的那些:钠代5-磺基间苯二甲酸,钾代5-磺基间苯二甲酸,钠代2-磺基对苯二甲酸,钾代2-磺基对苯二甲酸,5-磺基间苯二甲酸二甲酯钠盐、5-磺基间苯二甲酸二甲酯钾盐及其混合物。二元酸可以任选地存在的数量为1mol%-约10mol%,基于约100mol%树脂。
可用于制备磺化聚酯树脂的有机二元醇的例子包括但不限于二元醇或二醇,如碳链长度为例如约1-约25个碳原子的亚烷基二醇,和作为进一步的例子,乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-丁二醇、1,3-丁二醇、1,4-丁二醇、1,2-戊二醇、1,3-戊二醇、1,4-戊二醇、1,5-戊二醇、己二醇、庚二醇、二甘醇、二丙二醇、环己烷二醇、2,2-二甲基丙二醇、1,2-丙二醇、新戊二醇、辛二醇、环己烷二甲醇、及其混合物。包括二元醇或二醇的有机二元醇可以各种有效数量采用,例如树脂的约45-约55mol%。
磺化聚酯树脂由凝胶渗透色谱和使用聚苯乙烯作为标准物测量的数均分子量(Mn)为约1,500-约50,000克每摩尔,和重均分子量(Mw)为约6,000克每摩尔-约150,000克每摩尔且多分散性为约2-约12。
磺化聚酯树脂可以在调色剂组合物中采用任何所需或有效的数量存在,如约75-约95wt%,例如约80-约90wt%,基于调色剂组合物的总重量。然而,数量可以在这此范围以外。
凝结剂,如金属盐可有助于聚集和聚结磺化聚酯树脂。凝结剂可以是水溶性金属盐,如单价、二价或多价盐,选自如下金属的氯化物、硫酸盐、硝酸盐、溴化物、碘化物、氟化物、乙酰乙酸盐、磺基硅酸盐和乙酸盐:铝、镁、锌、钠、锂、铷、铯、铍、钡、锶、铜、锰、铬、铁、氧钒基和钾。凝结剂的非限制性例子包括氯化铝、硫酸锌、硫酸镁、硫酸钾-铝、氯化钠、溴化钠、碘化钠、氟化钠、乙酸钠、乙酰乙酸钠、氯化锂、溴化锂、碘化锂、氟化锂、乙酸锂、乙酰乙酸锂、氯化钾、溴化钾、碘化钾、氟化钾、乙酸钾、乙酰乙酸钾、溴化铷、氯化铷、碘化铷、氟化铷、乙酸铷、乙酰乙酸铷、溴化铯、氯化铯、碘化铯、氟化铯、乙酸铯、乙酰乙酸铯、溴化铍、氯化铍、碘化铍、氟化铍、乙酸铍、乙酰乙酸铍、溴化镁、氯化镁、碘化镁、氟化镁、乙酸镁、乙酰乙酸镁、溴化钙、溴化钡、氯化钡、碘化钡、氟化钡、乙酸钡、乙酰乙酸钡、溴化锶、氯化锶、碘化锶、氟化锶、乙酸锶、乙酰乙酸锶、溴化锌、氯化锌、碘化锌、氟化锌、乙酸锌、乙酰乙酸锌、溴化铜、氯化铜、碘化铜、氟化铜、乙酸铜、乙酰乙酸铜、溴化锰、氯化锰、碘化锰、氟化锰、乙酸锰、乙酰乙酸锰、溴化铬、氯化铬、碘化铬、氟化铬、乙酸铬、乙酰乙酸铬、溴化铁、氯化铁、碘化铁、氟化铁、乙酸铁、乙酰乙酸铁、溴化氧钒、氯化氧钒、碘化氧钒、氟化氧钒、乙酸氧钒、和乙酰乙酸氧钒。凝结剂可以在酸性溶液(例如1摩尔硝酸溶液)中加入混合物,并且在此加入步骤期间混合物的粘度可增加。
在实施方案中,可以以两部分加入凝结剂。第一部分可以在约20℃-约35℃,例如约23℃-约30℃,还例如约23℃-约25℃,和作为进一步的例子约25℃-约28℃的温度下加入。在加入第一部分之后,为保证凝结剂用尽可以将温度增加到约50℃并且pH可以为约5.5。温度的此增加可移动平衡,由此强制锌离子到着色的磺化聚酯树脂粒子表面上。此外,温度的此增加可对粒度的增长具有最小的影响。可以在增加温度之后加入凝结剂的第二部分。获得的磺化聚酯调色剂粒子的尺寸为约1-约5微米,例如约2-约4微米,和作为进一步的例子约2-约3微米。
其后,可以施加热量和搅拌以诱导微米尺寸粒子的聚集和形成。聚集温度可以为约40℃-约62℃,例如约45℃-约58℃。完成聚集的温度可控制核调色剂粒子的尺寸。
在实施方案中,磺化聚酯调色剂粒子可任选地包含蜡。蜡可包括以体积直径表示的尺寸为约0.1-约0.5微米,例如约0.2-约0.4微米的亚微米蜡粒子。蜡可以在与磺化聚酯调色剂粒子中存在的离子表面活性剂具有相同电荷极性的离子表面活性剂中分散。蜡的非限制性例子包括购自Allied Chemical and Petrolite Corporation的聚丙烯和聚乙烯,购自Michaelman Inc.和the Daniels ProductsCompany的蜡乳液,购自Eastman Chemical Products,Inc.的EPOLENE N-15TM,VISCOL 550-PTM,购自Sanyo Kasei K.K.的低重均分子量聚丙烯和相似材料。选择的市售聚乙烯的分子量(Mw)可以为约700-约2,500,而市售聚丙烯的分子量可以为约4,000-约7,000。官能化蜡如胺和酰胺的例子包括例如购自Micro Powder Inc.的AQUA SUPERSLIP 6550TM,SUPERSLIP 6530TM,氟化蜡,例如购自Micro Powder Inc.的POLYFLUO 190TM,POLYFLUO 200TM,POLYFLUO523XFTM,AQUA POLYFLUO 411TM,AQUA POLYSILK 19TM,POLYSILK14TM,混合氟化酰胺蜡,例如也购自Micro Powder Inc.的MICROSPERSION 19TM,酰亚胺,酯,季胺,羧酸或丙烯酸类聚合物乳液,例如JONCRYL 74TM,89TM,130TM,537TM,538TM,都购自SCJohnson Wax,购自Allied Chemical and Petrolite Corporation和S C Johnson Wax的氯化聚丙烯和聚乙烯。蜡的峰值熔融温度(Tm)可以为约70℃-约110℃并且开始熔化热为约50℃-约100℃。
在公开的方法中,可以将聚金属卤化物聚集剂加入到核调色剂粒子中。在实施方案中,当调色剂粒子的pH为约3-约6,例如约5-约6,例如约5.4时,可以将聚金属卤化物加入到调色剂粒子中。聚金属卤化物,不象凝结剂,可自身粘附到核调色剂粒子的表面。聚金属卤化物可以选自聚氯化铝(PAC)和聚磺基硅酸铝(PASS)。
然后可以将包括核调色剂粒子和聚金属卤化物的混合物的pH从约5.4降低到例如约4。由于pH驱动离子的电荷,依赖于pH聚金属卤化物可以是活性的或非活性的。例如,在低pH下聚金属卤化物是活性的并诱导正电荷。结果是,调色剂粒子的表面可以是带阳离子电荷的。聚金属卤化物可以采用任何所需或有效的数量存在,如约0.1%-约30wt%,例如约10%-约20wt%,相对于调色剂组合物的重量。然而,数量可以在这些范围以外。
公开的方法进一步包括将阴离子胶乳加入到包括聚金属卤化物的混合物中,该聚金属卤化物粘附到核调色剂粒子的表面。阴离子胶乳可包括乙烯基聚合物树脂粒子,该粒子可以是阴离子的。乙烯基聚合物树脂的非限制性例子包括聚(苯乙烯/丁二烯),聚(对甲基苯乙烯/丁二烯),聚(间甲基苯乙烯/丁二烯),聚(α-甲基苯乙烯/丁二烯),聚(甲基丙烯酸甲酯/丁二烯),聚(甲基丙烯酸乙酯/丁二烯),聚(甲基丙烯酸丙酯/丁二烯),聚(甲基丙烯酸丁酯/丁二烯),聚(丙烯酸甲酯/丁二烯),聚(丙烯酸乙酯/丁二烯),聚(丙烯酸丙酯/丁二烯),聚(丙烯酸丁酯/丁二烯),聚(苯乙烯/异戊二烯),聚(对甲基苯乙烯/异戊二烯),聚(间甲基苯乙烯/异戊二烯),聚(α-甲基苯乙烯/异戊二烯),聚(甲基丙烯酸甲酯/异戊二烯),聚(甲基丙烯酸乙酯/异戊二烯),聚(甲基丙烯酸丙酯/异戊二烯),聚(甲基丙烯酸丁酯/异戊二烯),聚(丙烯酸甲酯/异戊二烯),聚(丙烯酸乙酯/异戊二烯),聚(丙烯酸丙酯/异戊二烯),聚(丙烯酸丁酯-异戊二烯),聚(苯乙烯/丙烯酸正丁酯/丙烯酸),聚(苯乙烯/甲基丙烯酸正丁酯/丙烯酸),聚(苯乙烯/甲基丙烯酸正丁酯/丙烯酸β-羧基乙酯),聚(苯乙烯/丙烯酸正丁酯/丙烯酸β-羧基乙酯)聚(苯乙烯/丁二烯/甲基丙烯酸),聚(苯乙烯/丙烯酸正丁酯/苯乙烯磺酸钠盐/丙烯酸)及其混合物。
乙烯基聚合物树脂粒子,如苯乙烯丙烯酸酯乳液聚集粒子可包含羧酸基团,该羧酸基团可以受控地聚结到调色剂粒子的表面上。乙烯基聚合物粒子的羧酸基团可以选自丙烯酸、甲基丙烯酸、衣康酸、丙烯酸β-羧基乙酯、富马酸、马来酸和肉桂酸,并且其中羧酸存在的数量可以为约0.1-约10wt%。乙烯基聚合物粒子可以采用任何所需或有效的数量存在,如约10-约40wt%,例如约15-约30wt%的数量,相对于调色剂粒子,以在调色剂粒子上形成涂层。然而,数量可以在这些范围以外。
在加入阴离子胶乳之后,可以将混合物的pH进一步从约4降低到约3.8,例如约3.3,随后搅拌。在实施方案中,可以在小于约3的pH下使乙烯基聚合物树脂粘附到核调色剂粒子的表面上。不限于任何特定的理论,相信如果将pH提高到例如约6,则乙烯基聚合物树脂将不熔凝到调色剂粒子的表面上。相反地,如果将调色剂粒子的pH降低以适应乙烯基聚合物树脂粒子的pH,例如至约2.5,则相信调色剂粒子的聚集/聚结是不能控制的,例如由于锌离子的产生。
可以加热核调色剂粒子混合物。例如,可以提高温度以熔凝包括乙烯基聚合物粒子的阴离子胶乳到核调色剂粒子的表面上,由此形成涂覆的调色剂粒子。可以将温度提高到约50℃-约65℃,例如约53℃-约63℃,和作为进一步的例子约56℃-约58℃。
可以将涂覆的调色剂粒子搅拌约5-约7小时,然后可以洗涤。滤液可以是透明的,表示没有报废。可以使涂覆的调色剂粒子干燥,经历充电,和熔凝。
获得的涂覆调色剂粒子可包括核和壳,该核包括磺化聚酯树脂而该壳包括乙烯基聚合物,如苯乙烯丙烯酸酯羧酸。此壳可允许获得的涂覆调色剂粒子保留它们的电荷。
以体积平均直径计,涂覆的调色剂粒子的粒度可以为约1微米-约25微米,例如约2-约15微米。粒度分布(GSD)可以为约1.1-约1.33,例如约1.11-约1.28。尺寸和尺寸分布可以由库乐尔特颗粒计数器测量,而不需要采取常规粉碎和分级方法。
在实施方案中,可任选地加入表面活性剂,如阴离子和/或非离子表面活性剂。表面活性剂可控制粒度和粒度分布(GSD)。离子表面活性剂的例子包括但不限于阴离子表面活性剂,如十二烷基硫酸钠、十二烷基苯磺酸钠、十二烷基萘硫酸钠、二烷基苯烷基硫酸盐和磺酸盐、abitic acid、NEOGEN R、和购自Kao的NEOGEN SC、购自Dow Chemical Co.的DOWFAX等,以及其混合物。阴离子表面活性剂可以采用任何所需或有效的数量使用,如用于制备共聚物树脂的单体的约0.01%-约10wt%,例如约0.1%-约5%,尽管数量可以在这些范围以外。
合适非离子表面活性剂的例子包括聚乙烯醇、聚丙烯酸、鲸蜡醇糖(methalose)、甲基纤维素、乙基纤维素、丙基纤维素、羟乙基纤维素、羧甲基纤维素、聚氧乙烯鲸蜡基醚、聚氧乙烯月桂基醚、聚氧乙烯辛基醚、聚氧乙烯辛基苯基醚、聚氧乙烯油基醚、聚氧乙烯脱水山梨醇单月桂酸酯、聚氧乙烯硬脂基醚、聚氧乙烯壬基苯基醚、二烷基苯氧基聚(亚乙基氧)乙醇(从Rhone-Poulenc作为IGEPALCA-210,IGEPAL CA-520,IGEPAL CA-720,IGEPAL CO-890,IGEPALCO-720,IGEPAL CO-290,ANTAROX 890和ANTAROX 897购得)等,以及其混合物。非离子表面活性剂可以采用任何所需或有效的数量存在,例如用于制备共聚物树脂的单体的约0.01%-约10wt%,和作为进一步的例子约0.1%-约5%,尽管数量可以在这些范围以外。
调色剂组合物任选地也可包括电荷控制添加剂,如卤化烷基吡啶鎓,该卤化烷基吡啶鎓包括氯化氯化鲸蜡基吡啶鎓和如在美国专利4,298,672中公开的其它物质,硫酸盐和硫酸氢盐,该硫酸盐和硫酸氢盐包括如在美国专利4,560,635中公开的二硬脂基二甲基铵甲基硫酸盐,和如在美国专利4,937,157;4,560,635中公开的二硬脂基二甲基硫酸氢铵,3,5-二叔丁基水杨酸锌化合物,如购自OrientChemical Company,日本的Bontron E-84,或如在美国专利4,656,112中公开的锌化合物,3,5-二叔丁基水杨酸铝化合物如购自OrientChemical Company,日本的Bontron E-88,或如在美国专利4,845,003中公开的铝化合物,如在美国专利3,944,493;4,007,293;4,079,014;4,394,430;4,464,452;4,480,021;和4,560,635中公开的电荷控制添加剂等,以及其混合物。
任选的电荷控制添加剂可以在调色剂组合物中采用任何所需或有效的数量存在,如约0.1%-约10wt%,例如约1%-约5wt%,相对于调色剂组合物的总重量。然而,数量可以在此范围以外。
调色剂组合物也可任选地包括外部表面添加剂,该外部表面添加剂包括助流添加剂,该添加剂通常可以在其调色剂表面上存在。外部表面添加剂的非限制性例子包括金属氧化物如二氧化钛、氧化锡、其混合物等,胶态二氧化硅,如AEROSIL,金属盐和脂肪酸的金属盐,包括硬脂酸锌、氧化铝、氧化铈、及其混合物。几种上述添加剂说明于美国专利3,590,000和3,800,588中。此外,外部表面添加剂可以是美国专利6,004,714;6,190,815和6,214,507的涂覆二氧化硅。外部表面添加剂可以在聚集工艺期间加入或共混到形成的调色剂粒子上。
任选的外部表面添加剂可以采用任何所需或有效的数量存在,例如约0.1%-约5wt%,作为进一步的例子约0.1%-约1wt%,相对于调色剂组合物的总重量。然而,数量可以在此范围以外。
聚结的粒子与未聚结的聚集体的不同之处主要在于形态;未聚结的粒子具有更大的表面积,如具有“葡萄簇”形状,而聚结的粒子的表面积降低,如具有“马铃薯”形状或甚至球形形状。可以通过调节聚结工艺期间的条件,如温度、聚结时间等控制粒子形态。
适于制备公开的调色剂粒子的乳液聚集工艺说明于许多专利中,如美国专利5,278,020;5,290,654;5,308,734;5,344,738;5,346,797;5,348,832;5,364,729;5,366,841;5,370,963;5,376,172;5,403,693;5,418,108;5,405,728;5,482,812;5,496,676;5,501,935;5,527,658;5,585,215;5,593,807;5,604,076;5,622,806;5,648,193;5,650,255;5,650,256;5,658,704;5,660,965;5,723,253;5,744,520;5,763,133;5,766,818;5,747,215;5,804,349;5,827,633;5,853,944;5,840,462;5,863,698;5,869,215;5,902,710;5,910,387;5,916,725;5,919,595;5,922,501;5,925,488;5,945,245;5,977,210;6,017,671;6,020,101;6,045,240;6,132,924;6,143,457;和6,210,853。可以选择这些专利的组分和方法用于本公开内容的实施方案中。
实施例1
磺化聚酯乳液(A):(SPE)
通过缩聚反应制备包含3.75摩尔磺化的磺化聚酯树脂。通过碾磨将树脂研磨成粉末。将100gm树脂粉末加入到反应器中的10升水中并以500rpm的速度采用节距叶片涡轮机搅拌。将反应器的温度升高到85℃和允许搅拌1小时以消散树脂成包括在水中悬浮的约25nm磺化聚酯(SPE)树脂粒子的乳液。然后将反应器冷却到约23℃-约25℃并排出乳液。乳液包括11wt%树脂和89wt%水。
乙烯基聚合物乳液B的制备:
由苯乙烯丙烯酸丁酯和丙烯酸β羧基乙酯(βCEA)的乳液聚合产生的包括聚合物粒子的胶乳乳液制备如下。28.9克DOWFAX 2A1TM(阴离子乳化剂-55%活性成分)和25.8kg去离子水的表面活性剂溶液通过在不锈钢保持罐中混合5分钟而制备。然后在将混合物转移入反应器之前,将保持罐采用氮气吹扫5分钟。然后将反应器采用氮净连续吹扫,同时在100rpm下搅拌。然后将反应器加热到80℃。
单独地,将407g过硫酸铵引发剂溶于2.0kg去离子水。同样,单独地采用如下方式制备单体乳液A。混合21kg苯乙烯、6.11kgDOWFAXTM(阴离子活性剂)和12.9kg去离子水以形成乳液。然后在80℃下将5%上述乳液缓慢加入包含含水表面活性剂相的反应器以形成晶种,其中“晶种”表示例如在加入引发剂溶液之前加入反应器的初始乳液胶乳,同时由氮气吹扫。然后将以上引发剂溶液缓慢加入反应器,形成约5-约12nm胶乳“晶种”粒子。在10分钟之后,使用计量泵将剩余的乳液计量加入。
一旦将所有的以上单体乳液加入主反应器,将温度在80℃下保持另外2小时以完成反应。然后将反应器内容物冷却到约25℃。获得的分离产物包括在包含以上表面活性剂的含水相中悬浮的40wt%亚微米的0.2微米直径的苯乙烯/丙烯酸丁酯/βCEA树脂粒子。由凝胶渗透色谱测量的树脂胶乳的分子性能是Mw为36,000,Mn为10.8,由差示扫描量热计测量的中点Tg为53.8℃,其中中点Tg定义为在聚合物的开始和污损Tg之间的中间点。
调色剂制备
将400g包含11%固体的以上SPE乳液(A)放入烧杯,向烧杯中加入5.8g包括48%固体的flexiverse青色颜料分散体(38%颜料和10%树脂)。将此放置在温度控制的热板上并采用顶式搅拌器搅拌。将1.4g乙酸锌(ZnAc)(3wt%固体)放入45g水中并振荡直到溶解。将此缓慢加入混合物,其后将内容物加热到50℃。测量的粒度是1.7微米及GSD为1.84。然后在50℃下向其中加入另一相似部分的ZnAc溶液并允许搅拌另外2小时,得到1.9微米的粒度与1.23的GSD。发现混合物的pH是5.4。向其中加入2.26g的PAC溶液,该溶液包含0.26g PAC(10%活性成分)和2.0g 0.1M的硝酸。然后将混合物的pH采用4%硝酸溶液进一步降低到4.0。发现粒度是2.3微米。向其中加入40gm乳液B(40%固体)并将pH进一步降低到3.4以活化PAC和搅拌过夜。现在发现粒度是3.0微米(图1)。然后将温度提高到55℃和允许反应器搅拌另外2hrs。发现粒度是3.6微米。将反应器内容物进一步搅拌另外4小时,得到6.0微米的粒度与1.28的GSD。允许小样品搅拌另外2hrs,在该时间观察上清液是透明的。发现粒度为6.7微米及GSD为1.28。将调色剂粒子采用DIW洗涤并过滤两次和冷冻干燥。从扫描电子显微照片计算的调色剂的粒子形状因子为125。Sysmex FPIA-2100也可用于计算圆形度,它总是小于或等于1.0。
实施例2
使用根据实施例1的方法制备第二调节剂,区别在于在此情况下颜料是REGAL 330炭黑,其中炭黑含量是6wt%。
Claims (10)
1.一种方法,包括:
混合磺化聚酯树脂、着色剂和凝结剂;
加热获得的磺化聚酯混合物;
加入聚金属卤化物和阴离子胶乳以形成涂覆的调色剂粒子;和
加热涂覆的调色剂粒子。
2.权利要求1的方法,其中将凝结剂的第一部分在约20℃-约35℃的温度下加入,然后将温度增加到约50℃和pH是约5.5。
3.权利要求2的方法,其中加入凝结剂的第二部分使得磺化聚酯调色剂粒子的粒度为约2-约3微米。
4.权利要求1的方法,其中聚金属卤化物选自聚氯化铝和聚磺基硅酸铝。
5.权利要求1的方法,其中涂覆的调色剂粒子是带负电的。
6.权利要求1的方法,其中加热涂覆的调色剂粒子使阴离子胶乳的乙烯基聚合物树脂熔凝到调色剂粒子的表面上。
7.一种方法,包括:
混合着色剂、磺化聚酯树脂和凝结剂以形成粒度为约1-约5微米的调色剂粒子;
加热获得的磺化聚酯调色剂粒子;
加入聚金属卤化物和包括乙烯基聚合物树脂的阴离子胶乳;和
通过加热将乙烯基聚合物树脂熔凝到调色剂粒子的表面上。
8.一种方法,包括:
混合磺化聚酯调色剂粒子与凝结剂以形成核调色剂粒子;和
加入聚金属卤化物到核调色剂粒子的表面上以形成涂覆的调色剂粒子。
9.一种方法,包括:
混合磺化聚酯树脂、着色剂和凝结剂的第一部分;
加热混合物;和
加入凝结剂的第二部分以形成磺化聚酯调色剂粒子。
10.一种方法,包括:
混合磺化聚酯树脂、着色剂、蜡和凝结剂;
加热获得的磺化聚酯调色剂粒子;加入聚金属卤化物和阴离子胶乳以形成涂覆的调色剂粒子;和加热涂覆的调色剂粒子。
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US11/094,404 US7799502B2 (en) | 2005-03-31 | 2005-03-31 | Toner processes |
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EP (1) | EP1708037B1 (zh) |
JP (1) | JP4908030B2 (zh) |
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Cited By (2)
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CN104155856A (zh) * | 2013-05-13 | 2014-11-19 | 富士施乐株式会社 | 静电图像显影用调色剂、静电图像显影剂、调色剂盒、处理盒、成像装置和成像方法 |
CN104155856B (zh) * | 2013-05-13 | 2019-08-16 | 富士施乐株式会社 | 调色剂、显影剂、调色剂盒、处理盒、成像装置和成像方法 |
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CN1841216B (zh) | 2011-11-16 |
DE602006001677D1 (de) | 2008-08-21 |
EP1708037B1 (en) | 2008-07-09 |
CA2541183C (en) | 2010-05-11 |
US7799502B2 (en) | 2010-09-21 |
JP2006285246A (ja) | 2006-10-19 |
BRPI0601046A (pt) | 2006-12-05 |
US20060222996A1 (en) | 2006-10-05 |
CA2541183A1 (en) | 2006-09-30 |
EP1708037A1 (en) | 2006-10-04 |
JP4908030B2 (ja) | 2012-04-04 |
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