CN106243774A - C.I. the preparation method of the red 57:1 of aqueous pigment - Google Patents

C.I. the preparation method of the red 57:1 of aqueous pigment Download PDF

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Publication number
CN106243774A
CN106243774A CN201610610715.8A CN201610610715A CN106243774A CN 106243774 A CN106243774 A CN 106243774A CN 201610610715 A CN201610610715 A CN 201610610715A CN 106243774 A CN106243774 A CN 106243774A
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China
Prior art keywords
weight portions
adds
solution
minutes
red
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Pending
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CN201610610715.8A
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Chinese (zh)
Inventor
山长坡
黄志强
孔祥新
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Shandong Sunshine Pigment Co Ltd
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Shandong Sunshine Pigment Co Ltd
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Priority to CN201610610715.8A priority Critical patent/CN106243774A/en
Publication of CN106243774A publication Critical patent/CN106243774A/en
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/006—Preparation of organic pigments
    • C09B67/0065—Preparation of organic pigments of organic pigments with only non-macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B29/00—Monoazo dyes prepared by diazotising and coupling
    • C09B29/0003—Monoazo dyes prepared by diazotising and coupling from diazotized anilines
    • C09B29/0007—Monoazo dyes prepared by diazotising and coupling from diazotized anilines containing acid groups, e.g. CO2H, SO3H, PO3H2, OSO3H, OPO2H2; Salts thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B29/00—Monoazo dyes prepared by diazotising and coupling
    • C09B29/10—Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group
    • C09B29/103—Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group of the naphthalene series
    • C09B29/106—Hydroxy carboxylic acids of the naphthalene series

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Paper (AREA)

Abstract

The invention discloses the preparation method of a kind of red 57:1 of C.I. aqueous pigment.The preparation method is that the preparation first carrying out diazo liquid, coupling solution, the diazo liquid prepared is put in coupling solution and carry out coupling, then carry out post processing, during post processing, add Sr2+、Al3+And Mg2+, and maleic anhydride of styrene dispersant, then through filter pressing, be dried, after mixed and standardization, inspection the red 57:1 of finished pigment.The preparation method of the red 57:1 of C.I. aqueous pigment of the present invention, the alkali resistance of pigment prepared is good, and storage is stable, in aqueous acrylamide acid system standing time length do not have anti-thick, the phenomenon such as become viscous, in water-based system, application is freely.

Description

C.I. the preparation method of the red 57:1 of aqueous pigment
Technical field
The present invention relates to method for preparing pigment, particularly relate to the preparation method of a kind of red 57:1 of C.I. aqueous pigment.
Background technology
C.I. the red 57:1 of organic pigment is to make containing double [2-(3-carboxyl-2-hydroxyl naphthyl azo base)-5-toluenesulfonic acid] calcium Red pigment for required composition.This C.I. paratonere 57:1 is by by the diazol of 4-aminotoluene-3-sulfonic acid and 3-hydroxyl Base-2-naphthoic acid coupling obtains AZOpigments, then its color lakeization is come with inorganic calcium compound further by this AZOpigments Preparation.But the pigment prepared in this way is poor due to alkali resistance, and bin stability is bad, at aqueous acrylamide acid system Middle standing time length easily occur anti-thick, the phenomenon such as become viscous, high degree limit its application in water-based system.
Summary of the invention
It is an object of the invention to, in place of overcoming the deficiencies in the prior art, it is provided that a kind of red 57:1's of C.I. aqueous pigment Preparation method, mainly solves the red problem storing instability in water-based system of 57 serial pigments that prior art exists.
The preparation method of the red 57:1 of C.I. aqueous pigment of the present invention, it is characterised in that realized by following steps:
Prepared by a, diazo liquid: put into appropriate water purification in diazonium tank, adds the 4B acid of 380～400 weight portions, pulls an oar 20 points Clock, adds the liquid caustic soda of 260～300 weight portions, and the molten clear rear ice block cooling that adds, to less than 20 DEG C, adds 700～720 weight portions Hydrochloric acid, after stirring 15 minutes, continues on the rocks to be cooled to-2 DEG C, adds the sodium nitrite solution of 450～500 weight portions, potassium iodide The micro-indigo plant of reagent paper, is sufficiently stirred for 45 minutes, adds the calcium chloride solution of 300～320 weight portions of cooling, continues stirring 15 minutes, Diazo liquid volume 80000～90000 parts, pH≤1.5, temperature≤5 DEG C, standby；
Prepared by b, coupling solution: put into appropriate water purification in material tank, adds the 2 of 400～430 weight portions, and 3-is sour, pulls an oar 10 points Clock, adds the liquid caustic soda of 800～850 weight portions, changes clear, adds appropriate bottom water in coupling tank, will change clear 2,3-acid in material tank Solution is put in coupling tank, and addition ice block cooling is to 1～3 DEG C, standby；
C, coupling: in the coupling solution that diazo liquid step a prepared is prepared with putting into step b for 10 to 15 minutes, pH be 10.5～ 11, temperature is 8 DEG C；
D, post processing: adding the magnesium chloride solution of 80～100 weight portions in the product that step c obtains, pH value is 10.5, continues to fill Divide stirring 60 minutes, be warming up to add when 53 DEG C the strontium nitrate solution of 150～180 weight portions, be continuously heating to 85～90 DEG C, then It is incubated 5～10 minutes, on the rocks is cooled to 53 DEG C, add the aluminum trichloride solution of 100～120 weight portions, and the liquid after diluted stream Aqueous slkali, keeps pH 7.5～8, adds the maleic anhydride of styrene dispersant of 20 weight portions, after stirring 15 minutes, and dnockout, pressure Filter, dry, pulverize, after inspection the red 57:1 of finished pigment.
Water soluble acrylic acid binder is mainly by ionic bond, hydrogen bond, anchoring group and pigment with the combination of pigment molecule Surface combines.The carboxyl of ionic bond, amide groups can be formed if water soluble acrylic acid binder has both contained, and have again and can form hydrogen The hydroxyl of key, therefore the combination ratio of red 57:1 precious with pigment is stronger.Present invention introduces many kinds of metal ions, formed more complicated Crystalline structure, relies on space entropic effect to give pigment particles stability in application system.It is simultaneously introduced macromolecule dispersing agent, In the middle of pigment and aqueous acrylamide acid system, play sterically hindered and barrier action, improve storage property the most accordingly.
As preferably, the liquid caustic soda concentration in described step a is 33%, and the concentration of hydrochloric acid is 31%, and the content of 4B acid is 98%, the concentration of sodium nitrite solution is 35%.
As preferably, the liquid caustic soda concentration in described step b is 33%, and the content of 2,3-acid is 98%.
As preferably, in described step d, magnesium chloride solution, strontium nitrate solution, the concentration of aluminum trichloride solution are 30%, Concentration of lye after dilution is 10%.
Therefore, the present invention use simultaneously various metals organic compound face class and, it is possible to solve paratonere 57:1 resistance to storage Sustainability problem, increases its stability.
Beneficial effects of the present invention: the preparation method of the red 57:1 of C.I. aqueous pigment of the present invention, prepares Alkali resistance of pigment is good, and storage is stable, in aqueous acrylamide acid system standing time length do not have anti-thick, the phenomenon such as become viscous, In water-based system, application is freely.
Detailed description of the invention
In conjunction with embodiment, technical scheme is further illustrated.
Embodiment 1: the preparation method of the red 57:1 of a kind of treasured, is realized by following steps:
Prepared by a, diazo liquid: put into appropriate water purification in diazonium tank, adds the 4B acid of 380 weight portions, pulls an oar 20 minutes, add The liquid caustic soda of 300 weight portions, the molten clear rear ice block cooling that adds, to less than 20 DEG C, adds the hydrochloric acid of 720 weight portions, stirs 15 minutes After, continue on the rocks to be cooled to-2 DEG C, add, the sodium nitrite solution of 460 weight portions, the micro-indigo plant of potassium iodide starch paper, be sufficiently stirred for 45 Minute, add the calcium chloride solution of 260 weight portions of cooling, continue to stir 15 minutes, diazo liquid volume 80000～90000 parts, PH≤1.5, temperature≤5 DEG C, standby；
Prepared by b, coupling solution: put into appropriate water purification in material tank, adds the 2 of 395 weight portions, and 3-is sour, pulls an oar 10 minutes, adds Entering the liquid caustic soda of 810 weight portions, change clear, add appropriate bottom water, will change clear 2 in material tank in coupling tank, 3-acid solution puts into idol Closing in tank, addition ice block cooling is to 1～3 DEG C, standby；
C, coupling: in the coupling solution that diazo liquid step a prepared is prepared with putting into step b for 10 to 15 minutes, pH be 10.5～ 11, temperature is 8 DEG C；
D, post processing: add the magnesium chloride solution of 80 weight portions in the product that step c obtains, pH value is 10.5, continues fully to stir Mix 60 minutes, be warming up to add when 53 DEG C the strontium nitrate solution of 150 weight portions, be continuously heating to 85～90 DEG C, then be incubated 5～10 Minute, on the rocks it is cooled to 53 DEG C, adds the aluminum trichloride solution of 100 weight portions, and the liquid caustic soda solution after diluted stream, keep pH to exist 7.5～8, add the maleic anhydride of styrene dispersant of 20 weight portions, after stirring 15 minutes, dnockout, filter pressing, dry, pulverize, inspection After testing the red 57:1 of finished pigment.
The alkali resistance of pigment prepared by above method is good, and storage is stable, when placing in aqueous acrylamide acid system Between long do not have anti-thick, the phenomenon such as become viscous, in water-based system, application is freely.

Claims (5)

  1. The preparation method of the red 57:1 of 1.C.I. aqueous pigment, it is characterised in that realized by following steps:
    Prepared by a, diazo liquid: put into appropriate water purification in diazonium tank, adds the 4B acid of 380～400 weight portions, pulls an oar 20 points Clock, adds the liquid caustic soda of 260～300 weight portions, and the molten clear rear ice block cooling that adds, to less than 20 DEG C, adds 700～720 weight portions Hydrochloric acid, after stirring 15 minutes, continues on the rocks to be cooled to-2 DEG C, adds the sodium nitrite solution of 450～500 weight portions, potassium iodide The micro-indigo plant of reagent paper, is sufficiently stirred for 45 minutes, adds the calcium chloride solution of 300～320 weight portions of cooling, continues stirring 15 minutes, Diazo liquid volume 80000～90000 parts, pH≤1.5, temperature≤5 DEG C, standby；
    Prepared by b, coupling solution: put into appropriate water purification in material tank, adds the 2 of 400～430 weight portions, and 3-is sour, pulls an oar 10 points Clock, adds the liquid caustic soda of 800～850 weight portions, changes clear, adds appropriate bottom water in coupling tank, will change clear 2,3-acid in material tank Solution is put in coupling tank, and addition ice block cooling is to 1～3 DEG C, standby；
    C, coupling: in the coupling solution that diazo liquid step a prepared is prepared with putting into step b for 10 to 15 minutes, pH be 10.5～ 11, temperature is 8 DEG C；
    D, post processing: adding the magnesium chloride solution of 80～100 weight portions in the product that step c obtains, pH value is 10.5, continues to fill Divide stirring 60 minutes, be warming up to add when 53 DEG C the strontium nitrate solution of 150～180 weight portions, be continuously heating to 85～90 DEG C, then It is incubated 5～10 minutes, on the rocks is cooled to 53 DEG C, add the aluminum trichloride solution of 100～120 weight portions, and the liquid after diluted stream Aqueous slkali, keeps pH 7.5～8, adds the maleic anhydride of styrene dispersant of 20 weight portions, after stirring 15 minutes, and dnockout, pressure Filter, dry, pulverize, after inspection the red 57:1 of finished pigment.
  2. The preparation method of the red 57:1 of C.I. aqueous pigment the most according to claim 1, it is characterised in that described step a In liquid caustic soda concentration be 33%, the concentration of hydrochloric acid is 31%, 4B acid content be 98%, the concentration of sodium nitrite solution is 35%.
  3. The preparation method of the red 57:1 of C.I. aqueous pigment the most according to claim 1, it is characterised in that described step b In liquid caustic soda concentration be 33%, 2,3-acid content be 98%.
  4. The preparation method of the red 57:1 of C.I. aqueous pigment the most according to claim 1, it is characterised in that described step d Middle magnesium chloride solution, strontium nitrate solution, the concentration of aluminum trichloride solution are 30%, and the concentration of lye after dilution is 10%, benzene EMA acid anhydride dispersant concentration is 30%.
  5. The preparation method of the red 57:1 of C.I. aqueous pigment the most according to claim 1, it is characterised in that a kind of precious red 57:1 Preparation method, realized by following steps:
    Prepared by a, diazo liquid: put into appropriate water purification in diazonium tank, adds the 4B acid of 380 weight portions, pulls an oar 20 minutes, add The liquid caustic soda of 300 weight portions, the molten clear rear ice block cooling that adds, to less than 20 DEG C, adds the hydrochloric acid of 720 weight portions, stirs 15 minutes After, continue on the rocks to be cooled to-2 DEG C, add, the sodium nitrite solution of 460 weight portions, the micro-indigo plant of potassium iodide starch paper, be sufficiently stirred for 45 Minute, add the calcium chloride solution of 260 weight portions of cooling, continue to stir 15 minutes, diazo liquid volume 80000～90000 parts, PH≤1.5, temperature≤5 DEG C, standby；
    Prepared by b, coupling solution: put into appropriate water purification in material tank, adds the 2 of 395 weight portions, and 3-is sour, pulls an oar 10 minutes, adds Entering the liquid caustic soda of 810 weight portions, change clear, add appropriate bottom water, will change clear 2 in material tank in coupling tank, 3-acid solution puts into idol Closing in tank, addition ice block cooling is to 1～3 DEG C, standby；
    C, coupling: in the coupling solution that diazo liquid step a prepared is prepared with putting into step b for 10 to 15 minutes, pH be 10.5～ 11, temperature is 8 DEG C；
    D, post processing: add the magnesium chloride solution of 80 weight portions in the product that step c obtains, pH value is 10.5, continues fully to stir Mix 60 minutes, be warming up to add when 53 DEG C the strontium nitrate solution of 150 weight portions, be continuously heating to 85～90 DEG C, then be incubated 5～10 Minute, on the rocks it is cooled to 53 DEG C, adds the aluminum trichloride solution of 100 weight portions, and the liquid caustic soda solution after diluted stream, keep pH to exist 7.5～8, add the maleic anhydride of styrene dispersant of 20 weight portions, after stirring 15 minutes, dnockout, filter pressing, dry, pulverize, inspection After testing the red 57:1 of finished pigment.
CN201610610715.8A 2016-07-29 2016-07-29 C.I. the preparation method of the red 57:1 of aqueous pigment Pending CN106243774A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108864752A (en) * 2018-08-10 2018-11-23 天津城建大学 A kind of water-dispersion type paratonere 57:1 modified pigment and preparation method thereof
CN111718610A (en) * 2020-07-24 2020-09-29 蓬莱新光颜料化工有限公司 Flame-retardant pigment and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101544847A (en) * 2008-03-28 2009-09-30 东洋油墨制造株式会社 Producing process for microfined organic pigment, microfined organic pigment and microfined organic pigment coloring composition
CN101851433A (en) * 2010-05-20 2010-10-06 杭州新晨颜料有限公司 Method for preparing pigment carmine 57:1
JP2014208744A (en) * 2013-03-29 2014-11-06 日本化薬株式会社 Colored dispersion, ink composition, inkjet recording method, and colored matter
CN105315725A (en) * 2014-06-30 2016-02-10 佳能株式会社 Production process for self-dispersible pigment, self-dispersible pigment, ink, ink cartridge and ink jet recording method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101544847A (en) * 2008-03-28 2009-09-30 东洋油墨制造株式会社 Producing process for microfined organic pigment, microfined organic pigment and microfined organic pigment coloring composition
CN101851433A (en) * 2010-05-20 2010-10-06 杭州新晨颜料有限公司 Method for preparing pigment carmine 57:1
JP2014208744A (en) * 2013-03-29 2014-11-06 日本化薬株式会社 Colored dispersion, ink composition, inkjet recording method, and colored matter
CN105315725A (en) * 2014-06-30 2016-02-10 佳能株式会社 Production process for self-dispersible pigment, self-dispersible pigment, ink, ink cartridge and ink jet recording method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
周煜等: "苯乙烯-马来酸酐(SMA)共聚物对颜料的分散及其在喷墨印花中的应用", 《印染助剂》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108864752A (en) * 2018-08-10 2018-11-23 天津城建大学 A kind of water-dispersion type paratonere 57:1 modified pigment and preparation method thereof
CN108864752B (en) * 2018-08-10 2020-04-28 天津城建大学 Water-dispersible pigment red 57:1 modified pigment and preparation method thereof
CN111718610A (en) * 2020-07-24 2020-09-29 蓬莱新光颜料化工有限公司 Flame-retardant pigment and preparation method thereof

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