JP2020003717A5 - - Google Patents
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- JP2020003717A5 JP2020003717A5 JP2018124969A JP2018124969A JP2020003717A5 JP 2020003717 A5 JP2020003717 A5 JP 2020003717A5 JP 2018124969 A JP2018124969 A JP 2018124969A JP 2018124969 A JP2018124969 A JP 2018124969A JP 2020003717 A5 JP2020003717 A5 JP 2020003717A5
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- polyester resin
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- crystalline polyester
- charge image
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- 239000002245 particle Substances 0.000 claims description 71
- 229920005989 resin Polymers 0.000 claims description 43
- 239000011347 resin Substances 0.000 claims description 43
- 229920001225 Polyester resin Polymers 0.000 claims description 34
- 239000004645 polyester resin Substances 0.000 claims description 34
- 125000003504 2-oxazolinyl group Chemical group O1C(=NCC1)* 0.000 claims description 18
- 229920000642 polymer Polymers 0.000 claims description 18
- 239000000805 composite resin Substances 0.000 claims description 17
- 238000002844 melting Methods 0.000 claims description 15
- -1 styrene compound Chemical class 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 230000003068 static Effects 0.000 claims description 7
- 230000004931 aggregating Effects 0.000 claims description 6
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 description 17
- 239000006185 dispersion Substances 0.000 description 16
- 239000003086 colorant Substances 0.000 description 14
- 239000001993 wax Substances 0.000 description 10
- 239000004094 surface-active agent Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 5
- 238000004220 aggregation Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 239000003945 anionic surfactant Substances 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 150000004665 fatty acids Chemical class 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000004698 Polyethylene (PE) Substances 0.000 description 2
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 description 2
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- OCQDPIXQTSYZJL-UHFFFAOYSA-N 1,4-bis(butylamino)anthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C(NCCCC)=CC=C2NCCCC OCQDPIXQTSYZJL-UHFFFAOYSA-N 0.000 description 1
- FKKAGFLIPSSCHT-UHFFFAOYSA-N 1-dodecoxydodecane;sulfuric acid Chemical compound OS(O)(=O)=O.CCCCCCCCCCCCOCCCCCCCCCCCC FKKAGFLIPSSCHT-UHFFFAOYSA-N 0.000 description 1
- DZNJMLVCIZGWSC-UHFFFAOYSA-N 3',6'-bis(diethylamino)spiro[2-benzofuran-3,9'-xanthene]-1-one Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC=C(N(CC)CC)C=C1OC1=CC(N(CC)CC)=CC=C21 DZNJMLVCIZGWSC-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N Phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- PZTQVMXMKVTIRC-RZLHGTIFSA-L Pigment Rubine Chemical compound [Ca+2].[O-]S(=O)(=O)C1=CC(C)=CC=C1\N=N\C1=C(O)C(C([O-])=O)=CC2=CC=CC=C12 PZTQVMXMKVTIRC-RZLHGTIFSA-L 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- NRCMAYZCPIVABH-UHFFFAOYSA-N Quinacridone Chemical compound N1C2=CC=CC=C2C(=O)C2=C1C=C1C(=O)C3=CC=CC=C3NC1=C2 NRCMAYZCPIVABH-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000004203 carnauba wax Substances 0.000 description 1
- 235000013869 carnauba wax Nutrition 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 230000001112 coagulant Effects 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- MOTZDAYCYVMXPC-UHFFFAOYSA-M dodecyl sulfate Chemical compound CCCCCCCCCCCCOS([O-])(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-M 0.000 description 1
- 229940043264 dodecyl sulfate Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 235000010187 litholrubine BK Nutrition 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012170 montan wax Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000001737 promoting Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- VQOIVBPFDDLTSX-UHFFFAOYSA-M sodium;3-dodecylbenzenesulfonate Chemical class [Na+].CCCCCCCCCCCCC1=CC=CC(S([O-])(=O)=O)=C1 VQOIVBPFDDLTSX-UHFFFAOYSA-M 0.000 description 1
- HWLCXJRHGUPXJZ-RTLSQWIOSA-K sodium;iron(2+);(1E)-1-oxidoiminonaphthalen-2-one;(1Z)-1-oxidoiminonaphthalen-2-one Chemical compound [Na+].[Fe+2].C1=CC=C2C(=N/[O-])\C(=O)C=CC2=C1.C1=CC=C2C(=N/[O-])\C(=O)C=CC2=C1.C1=CC=C2C(=N/[O-])/C(=O)C=CC2=C1 HWLCXJRHGUPXJZ-RTLSQWIOSA-K 0.000 description 1
- 229940086735 succinate Drugs 0.000 description 1
Description
本発明者はこのような課題を解決するため、凝集前の樹脂粒子Ｘをオキサゾリン基含有重合体と混合及び加熱し、更に凝集後の融着温度を所定範囲とすることで、低温定着性に優れ、且つ、帯電性能維持率に優れる静電荷像現像用トナーが得られることを見出した。
本発明は、複合樹脂Ａ及び結晶性ポリエステル樹脂Ｃを同一又は異なる樹脂粒子中に含む樹脂粒子Ｘと、オキサゾリン基含有重合体とを混合し、結晶性ポリエステル樹脂Ｃの融点以上の温度で加熱し、架橋樹脂粒子ＸＣを得る工程、
前記架橋樹脂粒子ＸＣを水系媒体中で凝集させて凝集粒子を得る工程、及び、
得られた前記凝集粒子を、前記結晶性ポリエステル樹脂Ｃの融点よりも１０℃低い温度以上の温度で融着させる工程を含み、
前記複合樹脂Ａが、アルコール成分及びカルボン酸成分の重縮合物であるポリエステル樹脂セグメントと、スチレン系化合物を含む原料モノマーの付加重合物であるビニル系樹脂セグメントとを含み、
前記オキサゾリン基含有重合体の添加量が、前記複合樹脂Ａ及び前記結晶性ポリエステル樹脂Ｃ中の酸基のモル数に対する前記オキサゾリン基含有重合体のオキサゾリン基のモル数（Ｏｘｚ当量）として、０．０２当量以上である、静電荷像現像用トナーの製造方法に関する。
In order to solve such a problem, the present inventor mixes and heats the resin particles X before aggregation with an oxazoline group-containing polymer, and further sets the fusion temperature after aggregation within a predetermined range to achieve low temperature fixability. It has been found that a toner for static charge image development, which is excellent and has an excellent charge performance retention rate, can be obtained.
In the present invention, the resin particles X containing the composite resin A and the crystalline polyester resin C in the same or different resin particles are mixed with the oxazoline group-containing polymer and heated at a temperature equal to or higher than the melting point of the crystalline polyester resin C. , Step to obtain crosslinked resin particles XC,
A step of aggregating the crosslinked resin particles XC in an aqueous medium to obtain agglomerated particles, and
The resulting the aggregated particles, comprising the step of fusing at 10 ° C. lower temperature or higher than the melting point of the crystalline polyester resin C,
The composite resin A contains a polyester resin segment which is a polycondensate of an alcohol component and a carboxylic acid component, and a vinyl resin segment which is an addition polymer of a raw material monomer containing a styrene compound.
The amount of the oxazoline group-containing polymer added is 0, as the number of moles of oxazoline groups (Oxz equivalent) of the oxazoline group-containing polymer relative to the number of moles of acid groups in the composite resin A and the crystalline polyester resin C. The present invention relates to a method for producing a toner for developing an electrostatic charge image, which is equal to or more than 02 equivalents.
［静電荷像現像用トナーの製造方法］
本発明の静電荷像現像用トナー（以下、単に「トナー」ともいう）の製造方法は、
複合樹脂Ａ及び結晶性ポリエステル樹脂Ｃを同一又は異なる樹脂粒子中に含む樹脂粒子Ｘと、オキサゾリン基含有重合体とを混合し、結晶性ポリエステル樹脂Ｃの融点以上の温度で加熱し、架橋樹脂粒子ＸＣを得る工程、
架橋樹脂粒子ＸＣを水系媒体中で凝集させて凝集粒子を得る工程、及び、
得られた凝集粒子を、結晶性ポリエステル樹脂Ｃの融点よりも１０℃低い温度以上の温度で融着させる工程を含む。
そして、複合樹脂Ａは、アルコール成分及びカルボン酸成分の重縮合物であるポリエステル樹脂セグメントと、スチレン系化合物を含む原料モノマーの付加重合物であるビニル系樹脂セグメントとを含む。
更に、オキサゾリン基含有重合体の添加量が、複合樹脂Ａ及び結晶性ポリエステル樹脂Ｃ中の酸基のモル数に対するオキサゾリン基含有重合体のオキサゾリン基のモル数（Ｏｘｚ当量）として、０．０２当量以上である。
以上の方法により、低温定着性に優れ、且つ、帯電性能維持率に優れるトナーが得られる。
[Manufacturing method of toner for static charge image development]
The method for producing a toner for developing an electrostatic charge image of the present invention (hereinafter, also simply referred to as "toner") is
The resin particles X containing the composite resin A and the crystalline polyester resin C in the same or different resin particles are mixed with the oxazoline group-containing polymer and heated at a temperature equal to or higher than the melting point of the crystalline polyester resin C to obtain the crosslinked resin particles. The process of obtaining XC,
A step of aggregating the crosslinked resin particles XC in an aqueous medium to obtain agglomerated particles, and
The step of fusing the obtained agglomerated particles at a temperature equal to or higher than 10 ° C. lower than the melting point of the crystalline polyester resin C is included.
The composite resin A contains a polyester resin segment which is a polycondensate of an alcohol component and a carboxylic acid component, and a vinyl resin segment which is an addition polymer of a raw material monomer containing a styrene compound.
Further, the amount of the oxazoline group-containing polymer added is 0.02 equivalent as the number of moles of oxazoline groups (Oxz equivalent) of the oxazoline group-containing polymer with respect to the number of moles of acid groups in the composite resin A and the crystalline polyester resin C. That is all.
By the above method, a toner having excellent low-temperature fixability and an excellent charge performance retention rate can be obtained.
本発明の一実施態様に係るトナーの製造方法は、例えば
複合樹脂Ａ及び結晶性ポリエステル樹脂Ｃを同一又は異なる樹脂粒子中に含む樹脂粒子Ｘと、オキサゾリン基含有重合体とを混合し、前記結晶性ポリエステル樹脂Ｃの融点以上の温度で加熱し、架橋樹脂粒子ＸＣを得る工程（以下、「工程（１）」ともいう）、
前記架橋樹脂粒子ＸＣを水系媒体中で凝集させて凝集粒子１を得る工程（以下、「工程（２）」ともいう）、
非晶性ポリエステル系樹脂Ｂを含む樹脂粒子Ｙを凝集粒子１に付着させて凝集粒子２を得る工程（以下、「工程（３）」ともいう）、及び、
得られた凝集粒子２を、結晶性ポリエステル樹脂Ｃの融点よりも１０℃低い温度以上の温度で融着させる工程（以下、「工程（４）」ともいう）を含む。
以下、当該実施態様を例にとり、本発明について説明する。
In the method for producing a toner according to an embodiment of the present invention, for example, resin particles X containing a composite resin A and a crystalline polyester resin C in the same or different resin particles are mixed with an oxazoline group-containing polymer, and the crystals are described. A step of obtaining crosslinked resin particles XC by heating at a temperature equal to or higher than the melting point of the sex polyester resin C (hereinafter, also referred to as “step (1)”).
A step of aggregating the crosslinked resin particles XC in an aqueous medium to obtain agglomerated particles 1 (hereinafter, also referred to as “step (2)”).
A step of adhering resin particles Y containing an amorphous polyester resin B to agglomerated particles 1 to obtain agglomerated particles 2 (hereinafter, also referred to as “step (3)”), and
The step (hereinafter, also referred to as “step (4)”) of fusing the obtained agglomerated particles 2 at a temperature equal to or higher than 10 ° C. lower than the melting point of the crystalline polyester resin C is included.
Hereinafter, the present invention will be described by taking the embodiment as an example.
〔混合条件〕
工程（１）では、複合樹脂Ａ及び結晶性ポリエステル樹脂Ｃを同一又は異なる樹脂粒子中に含む樹脂粒子Ｘと、オキサゾリン基含有重合体とを混合し、結晶性ポリエステル樹脂Ｃの融点以上の温度で加熱し、架橋樹脂粒子ＸＣを得る。結晶性ポリエステル樹脂Ｃの融点以上の温度で加熱することで、オキサゾリン基含有重合体と結晶性ポリエステル樹脂Ｃとの反応が促進され、帯電性能維持率を向上させることができる。
工程（１）の温度は、好ましくは結晶性ポリエステル樹脂Ｃの融点よりも５℃高い温度以上、より好ましくは結晶性ポリエステル樹脂Ｃの融点よりも１０℃高い温度以上、更に好ましくは結晶性ポリエステル樹脂Ｃの融点よりも１５℃高い温度以上であり、そして、好ましくは複合樹脂Ａの軟化点よりも１０℃高い温度以下、より好ましくは複合樹脂Ａの軟化点よりも５℃高い温度以下、更に好ましくは複合樹脂Ａの軟化点以下である。
工程（１）の加熱時間は、好ましくは０．５時間以上、より好ましくは１時間以上、更に好ましくは２時間以上であり、そして、好ましくは６時間以下、より好ましくは５時間以下、更に好ましくは４時間以下である。
ここで加熱時間とは、結晶性ポリエステル樹脂Ｃの融点以上の温度とする時間である。
なお、工程（１）において、混合方法は、公知の方法により行うことができる。
[Mixed conditions]
In the step (1), the resin particles X containing the composite resin A and the crystalline polyester resin C in the same or different resin particles are mixed with the oxazoline group-containing polymer, and at a temperature equal to or higher than the melting point of the crystalline polyester resin C. heating, Ru obtain crosslinked resin particles XC. By heating at a temperature equal to or higher than the melting point of the crystalline polyester resin C, the reaction between the oxazoline group-containing polymer and the crystalline polyester resin C is promoted, and the charge performance retention rate can be improved.
The temperature of the step (1) is preferably 5 ° C. or higher than the melting point of the crystalline polyester resin C, more preferably 10 ° C. or higher than the melting point of the crystalline polyester resin C, and further preferably the crystalline polyester resin. The temperature is 15 ° C. higher than the melting point of C, and preferably 10 ° C. or lower than the softening point of the composite resin A, more preferably 5 ° C. or higher than the softening point of the composite resin A, further preferably. Is less than or equal to the softening point of the composite resin A.
The heating time of the step (1) is preferably 0.5 hours or more, more preferably 1 hour or more, further preferably 2 hours or more, and preferably 6 hours or less, more preferably 5 hours or less, still more preferably. Is less than 4 hours.
Here, the heating time is a time at which the temperature is equal to or higher than the melting point of the crystalline polyester resin C.
In the step (1), the mixing method can be performed by a known method.
＜工程（２）＞
工程（２）では、架橋樹脂粒子ＸＣを水系媒体中で凝集させて凝集粒子１を得る。
<Process (2)>
In the step (2), the crosslinked resin particles XC are agglomerated in an aqueous medium to obtain agglomerated particles 1.
〔離型剤〕
工程（２）では、架橋樹脂粒子ＸＣと共に、離型剤を含む離型剤粒子を凝集させてもよい。
離型剤としては、例えば、ポリプロピレンワックス、ポリエチレンワックス、ポリプロピレンポリエチレン共重合体ワックス；マイクロクリスタリンワックス、パラフィンワックス、フィッシャートロプシュワックス、サゾールワックス等の炭化水素系ワックス又はそれらの酸化物；カルナウバワックス、モンタンワックス又はそれらの脱酸ワックス、脂肪酸エステルワックス等のエステル系ワックス；脂肪酸アミド類、脂肪酸類、高級アルコール類、脂肪酸金属塩が挙げられる。これらは１種又は２種以上を用いてもよい。
〔Release agent〕
In the step (2), the release agent particles containing the release agent may be aggregated together with the crosslinked resin particles XC.
Examples of the release agent include polypropylene wax, polyethylene wax, polypropylene-polyethylene copolymer wax; hydrocarbon waxes such as microcrystallin wax, paraffin wax, Fishertropch wax, and sazole wax, or oxides thereof; carnauba wax. , Montan wax or ester waxes such as deoxidizing waxes and fatty acid ester waxes; fatty acid amides, fatty acids, higher alcohols, fatty acid metal salts and the like. These may be used alone or in combination of two or more.
（離型剤粒子の分散液）
離型剤は、離型剤粒子の分散液として、架橋樹脂粒子ＸＣと混合し、凝集させることで、凝集粒子１に含有させることが好ましい。
離型剤粒子の分散液は、界面活性剤を用いて得ることも可能であるが、離型剤と後述する樹脂粒子Ｚとを混合して得ることが好ましい。離型剤と樹脂粒子Ｚを用いて離型剤粒子を調製することで、樹脂粒子Ｚにより離型剤粒子が安定化され、界面活性剤を使用しなくても離型剤を水系媒体中に分散させることが可能となる。離型剤粒子の分散液中では、離型剤粒子の表面に樹脂粒子Ｚが多数付着した構造を有していると考えられる。
(Dispersion of release agent particles)
The release agent is preferably contained in the agglomerated particles 1 by mixing with the crosslinked resin particles XC and aggregating the release agent particles as a dispersion liquid.
The dispersion liquid of the release agent particles can be obtained by using a surfactant, but it is preferably obtained by mixing the release agent and the resin particles Z described later. By preparing the release agent particles using the release agent and the resin particles Z, the release agent particles are stabilized by the resin particles Z, and the release agent can be placed in the aqueous medium without using a surfactant. It becomes possible to disperse. It is considered that the dispersion liquid of the release agent particles has a structure in which a large number of resin particles Z are adhered to the surface of the release agent particles.
〔着色剤〕
工程（２）では、架橋樹脂粒子ＸＣと共に、着色剤を含む着色剤粒子を凝集させてもよい。
着色剤としては、トナー用着色剤として用いられている染料、顔料等のすべてを使用することができる。
着色剤としては、例えば、カーボンブラック、フタロシアニンブルー、パーマネントブラウンＦＧ、ブリリアントファーストスカーレット、ピグメントグリーンＢ、ローダミン−Ｂベース、ソルベントレッド４９、ソルベントレッド１４６、ソルベントブルー３５、キナクリドン、カーミン６Ｂ、ジスアゾエローが挙げられる。トナーは、黒トナー、黒以外のカラートナーのいずれであってもよい。
[Colorant]
In the step (2), the colorant particles containing the colorant may be aggregated together with the crosslinked resin particles XC.
As the colorant, all of the dyes, pigments and the like used as the colorant for toner can be used.
Examples of the colorants include carbon black, phthalocyanine blue, permanent brown FG, brilliant first scarlet, pigment green B, rhodamine-B base, solvent red 49, solvent red 146, solvent blue 35, quinacridone, carmine 6B, and disazoero. Be done. The toner may be either black toner or color toner other than black.
（着色剤粒子の分散液）
着色剤は、着色剤粒子の分散液として、架橋樹脂粒子ＸＣと混合し、凝集させることで、凝集粒子１に含有させることが好ましい。
着色剤粒子の分散液は、着色剤と水系媒体とを、ホモジナイザー、超音波分散機等の分散機を用いて分散して得ることが好ましい。当該分散は、着色剤の分散安定性を向上させる観点から、界面活性剤の存在下で行うことが好ましい。当該界面活性剤としては、例えば、非イオン性界面活性剤、アニオン性界面活性剤、カチオン性界面活性剤が挙げられ、着色剤粒子の分散安定性を向上させる観点から、好ましくはアニオン性界面活性剤である。アニオン性界面活性剤としては、例えば、ドデシルベンゼンスルホン酸塩、ドデシル硫酸塩、ラウリルエーテル硫酸塩、アルケニルコハク酸塩が挙げられる。これらの中でも、ドデシルベンゼンスルホン酸塩が好ましい。
(Dispersion of colorant particles)
The colorant is preferably contained in the agglomerated particles 1 by mixing with the crosslinked resin particles XC and aggregating the colorant as a dispersion liquid of the colorant particles.
The dispersant of the colorant particles is preferably obtained by dispersing the colorant and an aqueous medium using a disperser such as a homogenizer or an ultrasonic disperser. The dispersion is preferably carried out in the presence of a surfactant from the viewpoint of improving the dispersion stability of the colorant. Examples of the surfactant include nonionic surfactants, anionic surfactants, and cationic surfactants, and from the viewpoint of improving the dispersion stability of the colorant particles, anionic surfactants are preferable. It is an agent. Examples of the anionic surfactant include dodecylbenzene sulfonate, dodecyl sulfate, lauryl ether sulfate, and alkenyl succinate. Of these, dodecylbenzene sulfonate is preferred.
〔界面活性剤〕
工程（２）では、混合分散液を調製した後に架橋樹脂粒子ＸＣを凝集させることが好ましい。
混合分散液を調製する際、架橋樹脂粒子ＸＣ及び必要に応じて添加される離型剤粒子等の任意成分の分散安定性を向上させる観点から、界面活性剤の存在下で行ってもよい。界面活性剤としては、例えば、アルキルベンゼンスルホン酸塩、アルキルエーテル硫酸塩等のアニオン性界面活性剤；ポリオキシエチレンアルキルエーテル、ポリオキシエチレンアルケニルエーテル類等の非イオン性界面活性剤が挙げられる。
界面活性剤を使用する場合、その使用量は、架橋樹脂粒子ＸＣ １００質量部に対して、好ましくは０．１質量部以上、より好ましくは０．５質量部以上であり、そして、好ましくは１０質量部以下、より好ましくは５質量部以下、更に好ましくは３質量部以下である。
[Surfactant]
In the step (2), it is preferable to agglomerate the crosslinked resin particles XC after preparing the mixed dispersion liquid.
When preparing the mixed dispersion liquid, it may be carried out in the presence of a surfactant from the viewpoint of improving the dispersion stability of arbitrary components such as the crosslinked resin particles XC and the release agent particles added as needed. Examples of the surfactant include anionic surfactants such as alkylbenzene sulfonates and alkyl ether sulfates; and nonionic surfactants such as polyoxyethylene alkyl ethers and polyoxyethylene alkenyl ethers.
When a surfactant is used, the amount used is preferably 0.1 part by mass or more, more preferably 0.5 part by mass or more, and preferably 10 parts by mass with respect to 100 parts by mass of the crosslinked resin particles XC. It is less than or equal to parts by mass, more preferably 5 parts by mass or less, and even more preferably 3 parts by mass or less.
前述の架橋樹脂粒子ＸＣの分散液、及び任意成分の混合は、常法により行われる。当該混合により得られた混合分散液に、凝集を効率的に行う観点から、凝集剤を添加することが好ましい。 The dispersion liquid of the crosslinked resin particles XC and the optional components described above are mixed by a conventional method. From the viewpoint of efficient aggregation, it is preferable to add a flocculant to the mixed dispersion obtained by the mixing.
凝集剤を用いて、例えば、０℃以上４０℃以下の架橋樹脂粒子ＸＣを含む混合分散液に、架橋樹脂粒子ＸＣ １００質量部に対し５質量部以上５０質量部以下の凝集剤を添加し、架橋樹脂粒子ＸＣを水系媒体中で凝集させて、凝集粒子１を得る。更に、凝集を促進させる観点から、凝集剤を添加した後に分散液の温度を上げることが好ましい。 Using a coagulant, for example, the mixed dispersion containing 0 ℃ least 40 ° C. below the crosslinked resin particles XC, was added 5 parts by mass or more 50 parts by weight of the flocculant to the crosslinked resin particles XC 100 parts by weight, The crosslinked resin particles XC are agglomerated in an aqueous medium to obtain agglomerated particles 1. Further, from the viewpoint of promoting aggregation, it is preferable to raise the temperature of the dispersion after adding the flocculant.
Claims (7)
前記架橋樹脂粒子ＸＣを水系媒体中で凝集させて凝集粒子を得る工程、及び、
得られた前記凝集粒子を、前記結晶性ポリエステル樹脂Ｃの融点よりも１０℃低い温度以上の温度で融着させる工程を含み、
前記複合樹脂Ａが、アルコール成分及びカルボン酸成分の重縮合物であるポリエステル樹脂セグメントと、スチレン系化合物を含む原料モノマーの付加重合物であるビニル系樹脂セグメントとを含み、
前記オキサゾリン基含有重合体の添加量が、前記複合樹脂Ａ及び前記結晶性ポリエステル樹脂Ｃ中の酸基のモル数に対する前記オキサゾリン基含有重合体のオキサゾリン基のモル数（Ｏｘｚ当量）として、０．０２当量以上である、静電荷像現像用トナーの製造方法。 The resin particles X containing the composite resin A and the crystalline polyester resin C in the same or different resin particles are mixed with the oxazoline group-containing polymer and heated at a temperature equal to or higher than the melting point of the crystalline polyester resin C to form a crosslinked resin. The process of obtaining particle XC,
A step of aggregating the crosslinked resin particles XC in an aqueous medium to obtain agglomerated particles, and
The step of fusing the obtained agglomerated particles at a temperature equal to or higher than 10 ° C. lower than the melting point of the crystalline polyester resin C is included.
The composite resin A contains a polyester resin segment which is a polycondensate of an alcohol component and a carboxylic acid component, and a vinyl resin segment which is an addition polymer of a raw material monomer containing a styrene compound.
The amount of the oxazoline group-containing polymer added is 0, as the number of moles of oxazoline groups (Oxz equivalent) of the oxazoline group-containing polymer relative to the number of moles of acid groups in the composite resin A and the crystalline polyester resin C. A method for producing a toner for developing an electrostatic charge image, which is 02 equivalents or more.
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