CN103045020B - Pigment color paste special for black neutral ink and preparation method of paste - Google Patents

Pigment color paste special for black neutral ink and preparation method of paste Download PDF

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Publication number
CN103045020B
CN103045020B CN201310016253.3A CN201310016253A CN103045020B CN 103045020 B CN103045020 B CN 103045020B CN 201310016253 A CN201310016253 A CN 201310016253A CN 103045020 B CN103045020 B CN 103045020B
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mill base
carbon black
add
writing ink
neutral writing
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CN103045020A (en
Inventor
刘守军
张瑞东
刁红亮
吴瑞娟
李月月
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Taiyuan yingkeao pen and ink technology Co.,Ltd.
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Shanxi Yingkeao Chemical Industry Technology Co Ltd
Taiyuan University of Technology
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Abstract

The invention discloses a pigment color paste special for black neutral ink. The pigment color paste comprises the following components in parts by weight: 20-30 parts of color black, 36-63 parts of deionized water, 0.5-1 parts of lubricating agent, 0.05-0.2 parts of emulsifying agent, 1-2 parts of dispersing agents, 5-10 parts of polyvinylpyrrolidone, 0.5-1 part of wetting dispersant and 10-20 parts of polyethylene glycol. The pigment color paste has the characteristics that rheology features are easy to modulate, stability is high and lubricating property is good.

Description

A kind of black Neutral writing ink sole pigment mill base and preparation method thereof
Technical field
The present invention relates to a kind of black Neutral writing ink sole pigment mill base and preparation method thereof.
Background technology
Neutral writing ink is a kind of water color ink that neutral ballpoint pen uses of specializing in, its maximum feature is to have very high stability, oilness and special rheological, and main manifestations is to have ultramicro-pigment size distribution, can stablize and use lubricating auxiliary agent and possess certain shear-thinning rheological characteristics.
The production of Neutral writing ink mainly realizes in the mode that adds other functional agent directly to modulate in water-based pigment colour paste.Because there not being Neutral writing ink special-used colour starch product to come out, the conventional two class mill base product modulation of Neutral writing ink.One class is water-borne coatings and water color ink mill base, for example patent " a kind of water-base inorganic pigment color paste and preparation method thereof (application number: CN200510097165.6) " and patent " inorganic pigment color paste and preparation method thereof (application number: CN200910030199.1) ".The feature of such mill base is to use in a large number tensio-active agent or macromolecule resin and pigment particle size thicker, with the Neutral writing ink of its modulation not only size distribution be difficult to reach requirement and because existing of excess surface active agent is difficult to realize the regulation and control of rheological characteristics.Another kind of is ink-jet printing ink mill base, for example patent " for the nano grade inorganic dispersible pigment color paste (application number: CN200410000322.2) of ink-jet printing ink " and patent a kind of preparation method of cationic water-based pigment colour paste " (application number: 200610096924.1) ".The feature of such mill base is that surfactant content is low and realized the Ultramicro Dispersion of pigment, but owing to not adding lubricating auxiliary agent at mill base preparatory phase, is difficult to realize the compatibility of Neutral writing ink oilness and stability.Ben is that patent " a kind of water-based pigment colour paste and preparation method thereof (application number: CN201010248740.9) " also belongs to this type of situation.
Summary of the invention
The object of this invention is to provide a kind ofly for modulating water-based pigment colour paste of black Neutral writing ink and preparation method thereof, reach modulated black Neutral writing ink and there is rheological characteristics and be easy to regulation and control, the high and good feature of lubricity of stability.
The present invention is by choose reasonable and use tensio-active agent, the Ultramicro Dispersion of pigment and the microemulsified of lubricating auxiliary agent are realized with multistage grinding technics, prepared mill base has compatible good with various auxiliary agents for rheological characteristics and is easy to the feature of controlling, can be exclusively used in modulation high quality Neutral writing ink, the Neutral writing ink stability of modulating is high, lubricity is excellent and can be according to different demands regulation and control rheological characteristicss.
The present invention is for modulating the water-based pigment colour paste of black Neutral writing ink, and its formulation weight umber consists of:
Colour carbon black as above is colour carbon black C111 or colour carbon black C311.
Lubricant as above is alkylphosphonic acid carboxylic acid ester compound, is Hostaphat MDAH(Clariant chemical industry (China) company limited), Hostaphat1306(Clariant chemical industry (China) company limited), one in S1 type alkyl phosphate (Li Hong chemical plant, Dandong).
Emulsifying agent as above is nonionogenic tenside, is polyoxyethylene nonylphenol ether, one or more in polyoxyethylene octylphenol ether, ten Polyglycerine monoleates, glyceryl monostearate.
Dispersion agent as above is aniorfic surfactant, is Dispersogen SNW(Clariant chemical industry (China) company limited) or Dispersogen1728(Clariant chemical industry (China) company limited).
Polyvinylpyrrolidone as above (molecular formula [C 19h 31n 3o 3] n) be PVP-K15(relative molecular weight 8 × 10 3), PVP-K30(relative molecular weight 4 × 104) in one or both.
Wetting dispersing agent is amphoterics amine multipolymer as mentioned above, trade(brand)name DUOEEN TDO(Akzo Nobel surface chemistry trade Co., Ltd).
Polyoxyethylene glycol as above, molecular formula is HO (CH 2cH 2o) nh (n=4-450), its average molecular mass is 2 × 10 2.
Preparation method of the present invention comprises the steps:
1) lubricant added in polyoxyethylene glycol and be heated to 60 ± 5 DEG C, adding emulsifier for mixing to homogeneous transparent, under constant temperature, adding the hot water of 60 ± 5 DEG C of 10-15 weight parts, stirring and be cooled to room temperature afterwards, forming transparent or semitransparent lubricant microemulsion;
2) polyvinylpyrrolidone is dissolved in the deionized water of equivalent, forms the polyvinylpyrrolidone aqueous solution;
3) in remaining deionized water, add dispersion agent and wetting dispersing agent, and fully stirring and dissolving forms clear solution, after add colour carbon black to stir, and soak 1-1.5h and form carbon black slurry;
4) in the carbon black slurry forming, add the polyvinylpyrrolidone aqueous solution and lubricant microemulsion, mix rear use basket-type grinder and grind 1.5-2h;
5) discharging when the thick mill base basket grinding being formed is afterwards placed in nanometer sand mill and is ground to pigment particle size D90≤350nm, is mill base finished product.
The present invention compared with prior art tool has the following advantages:
1. by choose reasonable and use tensio-active agent, in ensureing stability of pigment paste, significantly reduced the content of the tensio-active agent of mill base, made it possess good compatibility and rheology modulability;
2. utilize micro emulsion principle in mill base, to add lubricating auxiliary agent, when effective guarantee mill base is stable, also improved the lubricated writing quality of mill base modulation ink;
3. choose reasonable tensio-active agent be used in conjunction with multistage grinding technics, has efficiently realized the Ultramicro Dispersion of charcoal blacks, prepared mill base pigment particle size is distributed and reached the technical requirements of preparing Neutral writing ink.
Embodiment
Embodiment 1(mill base 1)
Paste formula:
Preparation process:
1) Hostaphat MDAH added in polyoxyethylene glycol and be heated to 60 DEG C, add polyoxyethylene nonylphenol ether to be stirred to homogeneous transparent, under constant temperature, add 60 DEG C of hot water of 15 weight part, stir and be cooled to room temperature afterwards, form transparent or semitransparent Hostaphat MDAH microemulsion; 2) polyvinylpyrrolidone PVP-K30 and PVP-K15 are dissolved in the deionized water of equivalent, form the polyvinylpyrrolidone aqueous solution; 3) in remaining deionized water, add Dispersogen SNW and DUOEEN TDO and fully stirring and dissolving form clear solution, after add colour carbon black C111 to stir and soak 1h and form carbon black slurry; 4) in the carbon black slurry forming, add the polyvinylpyrrolidone aqueous solution and Hostaphat MDAH microemulsion, mix rear use basket-type grinder and grind 1.5h; 5) discharging when the thick mill base basket grinding being formed is afterwards placed in nanometer sand mill and is ground to pigment particle size D90≤350nm, is mill base finished product.
Embodiment 2(mill base 2)
Paste formula:
Preparation process:
1) Hostaphat1306 added in polyoxyethylene glycol and be heated to 63 DEG C, add polyoxyethylene octylphenol ether to be stirred to homogeneous transparent, under constant temperature, add 60 DEG C of hot water of 15 weight part, stir and be cooled to room temperature afterwards, form transparent or semitransparent Hostaphat1306 microemulsion; 2) polyvinylpyrrolidone PVP-K30 and PVP-K15 are dissolved in the deionized water of equivalent, form the polyvinylpyrrolidone aqueous solution; 3) in remaining deionized water, add Dispersogen1728 and DUOEEN TDO and fully stirring and dissolving form clear solution, after add colour carbon black C111 to stir and soak 1.5h and form carbon black slurry; 4) in the carbon black slurry forming, add the polyvinylpyrrolidone aqueous solution and Hostaphat1306 microemulsion, mix rear use basket-type grinder and grind 2h; 5) discharging when the thick mill base basket grinding being formed is afterwards placed in nanometer sand mill and is ground to pigment particle size D90≤350nm, is mill base finished product.
Embodiment 3(mill base 3)
Paste formula:
Preparation process:
1) S1 type alkyl phosphate added in polyoxyethylene glycol and be heated to 65 DEG C, add polyoxyethylene nonylphenol ether and ten Polyglycerine monoleates to be stirred to homogeneous transparent, under constant temperature, add 65 DEG C of hot water of 12 weight part, stir and be cooled to room temperature afterwards, form transparent or semitransparent S1 type alkyl phosphate; 2) polyvinylpyrrolidone PVP-K30 is dissolved in the deionized water of equivalent, forms the polyvinylpyrrolidone aqueous solution; 3) in remaining deionized water, add Dispersogen SNW and DUOEEN TDO and fully stirring and dissolving form clear solution, after add colour carbon black C311 to stir and soak 1h and form carbon black slurry; 4) in the carbon black slurry forming, add the polyvinylpyrrolidone aqueous solution and S1 type alkylphosphonic acid carboxylic acid ester microemulsion, mix rear use basket-type grinder and grind 1.5h; 5) discharging when the thick mill base basket grinding being formed is afterwards placed in nanometer sand mill and is ground to pigment particle size D90≤350nm, is mill base finished product.
Embodiment 4(mill base 4)
Paste formula:
Preparation process:
1) S1 type alkyl phosphate added in polyoxyethylene glycol and be heated to 65 DEG C, add polyoxyethylene nonylphenol ether and glyceryl monostearate to be stirred to homogeneous transparent, under constant temperature, add 65 DEG C of hot water of 15 weight part, stir and be cooled to room temperature afterwards, form transparent or semitransparent S1 type alkyl phosphate; 2) polyvinylpyrrolidone PVP-K30 is dissolved in the deionized water of equivalent, forms the polyvinylpyrrolidone aqueous solution; 3) in remaining deionized water, add Dispersogen1728 and DUOEEN TDO and fully stirring and dissolving form clear solution, after add colour carbon black C311 to stir and soak 1h and form carbon black slurry; 4) in the carbon black slurry forming, add the polyvinylpyrrolidone aqueous solution and S1 type alkylphosphonic acid carboxylic acid ester microemulsion, mix rear use basket-type grinder and grind about 2h; 5) discharging when the thick mill base basket grinding being formed is afterwards placed in nanometer sand mill and is ground to pigment particle size D90≤350nm, is mill base finished product.
Embodiment 5(mill base 5)
Paste formula:
Preparation process:
1) S1 type alkyl phosphate added in polyoxyethylene glycol and be heated to 65 DEG C, add polyoxyethylene nonylphenol ether and ten Polyglycerine monoleates to be stirred to homogeneous transparent, under constant temperature, add 65 DEG C of hot water of 15 weight part, stir and be cooled to room temperature afterwards, form transparent or semitransparent S1 type alkyl phosphate; 2) polyvinylpyrrolidone PVP-K30 is dissolved in the deionized water of equivalent, forms the polyvinylpyrrolidone aqueous solution; 3) in remaining deionized water, add Dispersogen SNW and DUOEEN TDO and fully stirring and dissolving form clear solution, after add colour carbon black C311 to stir and soak 1.5h and form carbon black slurry; 4) in the carbon black slurry forming, add the polyvinylpyrrolidone aqueous solution and S1 type alkylphosphonic acid carboxylic acid ester microemulsion, mix rear use basket-type grinder and grind about 2h; 5) discharging when the thick mill base basket grinding being formed is afterwards placed in nanometer sand mill and is ground to pigment particle size D90≤350nm, is mill base finished product.
The application 1 of embodiment 1-5
According to Neutral writing ink modulation formula, get a certain amount of mill base, under whipped state, add respectively successively a certain amount of pH adjusting agent, wetting Agent for Printing Inks, defoamer, sanitas, inhibiter, thickening material, after stirring, filter de-bubble, obtain Neutral writing ink product.
Obtain Neutral writing ink 1, Neutral writing ink 3, Neutral writing ink 5, Neutral writing ink 7 and Neutral writing ink 9 with mill base 1, mill base 2, mill base 3, mill base 4 and mill base 5 according to following formula modulation respectively.
PH adjusting agent in above-mentioned formula is that the 50% trolamine aqueous solution, wetting Agent for Printing Inks are that glycol ether, defoamer are Surfynol DF – 66(US Air chemistry Products Co., Ltd), sanitas is that BIT, inhibiter are that benzotriazole, thickening material are T251(Shenzhen Hai Run Chemical Co., Ltd.).
The Neutral writing ink main performance index of modulating in table 1.
The application 2 of embodiment 1-5
According to Neutral writing ink modulation formula, get a certain amount of mill base, under whipped state, add respectively successively a certain amount of pH adjusting agent, wetting Agent for Printing Inks, defoamer, sanitas, inhibiter, thickening material, after stirring, filter de-bubble and obtain Neutral writing ink product.
Obtain Neutral writing ink 2, Neutral writing ink 4, Neutral writing ink 6, Neutral writing ink 8 and Neutral writing ink 10 with mill base 1, mill base 2, mill base 3, mill base 4 and mill base 5 according to following formula modulation respectively.
PH adjusting agent in above-mentioned formula is that the 50% trolamine aqueous solution, wetting Agent for Printing Inks are that propylene glycol and 1-Methoxy-2-propyl acetate mixed solution (1:1), defoamer are Surfynol DF – 66(US Air chemistry Products Co., Ltd), sanitas is that BIT, inhibiter are that benzotriazole, thickening material are T255(Shenzhen Hai Run Chemical Co., Ltd.).
The Neutral writing ink main performance index of modulating in table 1.

Claims (4)

1. a black Neutral writing ink sole pigment mill base, is characterized in that formulation weight umber consists of:
Described lubricant is the one in Hostaphat MDAH, Hostaphat1306, S1 type alkyl phosphate;
Described emulsifying agent is polyoxyethylene nonylphenol ether, one or more in polyoxyethylene octylphenol ether, ten Polyglycerine monoleates, glyceryl monostearate;
Described dispersion agent is Dispersogen SNW or Dispersogen1728;
Described wetting agent is DUOEEN TDO;
And preparation by the following method:
1) lubricant added in polyoxyethylene glycol and be heated to 60 ± 5 DEG C, adding emulsifier for mixing to homogeneous transparent, under constant temperature, adding the hot water of 60 ± 5 DEG C of 10-15 weight parts, stirring and be cooled to room temperature afterwards, forming transparent or semitransparent lubricant microemulsion;
2) polyvinylpyrrolidone is dissolved in the deionized water of equivalent, forms the polyvinylpyrrolidone aqueous solution;
3) in remaining deionized water, add dispersion agent and wetting agent, and fully stirring and dissolving forms clear solution, after add colour carbon black to stir, and soak 1-1.5h and form carbon black slurry;
4) in the carbon black slurry forming, add the polyvinylpyrrolidone aqueous solution and lubricant microemulsion, mix rear use basket-type grinder and grind 1.5-2h;
5) discharging when the thick mill base basket grinding being formed is afterwards placed in nanometer sand mill and is ground to pigment particle size D90≤350nm, is mill base finished product.
2. a kind of black Neutral writing ink sole pigment mill base as claimed in claim 1, is characterized in that described colour carbon black is colour carbon black C111 or colour carbon black C311.
3. a kind of black Neutral writing ink sole pigment mill base as claimed in claim 1, is characterized in that described polyvinylpyrrolidone is one or both in PVP-K15, PVP-K30.
4. a kind of black Neutral writing ink sole pigment mill base as claimed in claim 1, is characterized in that the molecular formula of described polyoxyethylene glycol is HO (CH 2cH 2o) nh, wherein n=4-450, its average molecular mass is 2 × 10 2.
CN201310016253.3A 2013-01-16 2013-01-16 Pigment color paste special for black neutral ink and preparation method of paste Active CN103045020B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106833136A (en) * 2017-02-10 2017-06-13 岳阳凯门水性助剂有限公司 A kind of dispersant and dispersible pigment color paste
WO2019193597A1 (en) * 2018-04-03 2019-10-10 M/S Koel Colours Pvt. Ltd. An anti-dust and easily dispersible pigment
CN108587249B (en) * 2018-04-16 2019-04-30 深圳市祥盛兴科技有限公司 A kind of preparation method of Neutral writing ink colour carbon black
CN112410915B (en) * 2019-08-23 2022-08-12 中国石油化工股份有限公司 Coloring paste suitable for dry acrylic fibers and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0717085A1 (en) * 1994-12-15 1996-06-19 Bayer Corporation Phosphoric acid monoesters useful for surface treatment of pigments for waterborne coatings
CN102372949A (en) * 2010-08-09 2012-03-14 曾炽涛 Aqueous pigment slurry and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0717085A1 (en) * 1994-12-15 1996-06-19 Bayer Corporation Phosphoric acid monoesters useful for surface treatment of pigments for waterborne coatings
CN102372949A (en) * 2010-08-09 2012-03-14 曾炽涛 Aqueous pigment slurry and preparation method thereof

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