CN102311658B - Preparation method of pigment used for water-based ink - Google Patents

Preparation method of pigment used for water-based ink Download PDF

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Publication number
CN102311658B
CN102311658B CN2010102190110A CN201010219011A CN102311658B CN 102311658 B CN102311658 B CN 102311658B CN 2010102190110 A CN2010102190110 A CN 2010102190110A CN 201010219011 A CN201010219011 A CN 201010219011A CN 102311658 B CN102311658 B CN 102311658B
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CN102311658A (en
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王健
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Longkou United Chemical Co.,Ltd.
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LONGKOU UNION CHEMICAL CO Ltd
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Abstract

The invention discloses a preparation method of a pigment used for water-based ink, which comprises the following steps: stirring 50-200 parts of water and 22 parts of sodium hydroxide, adding 22-24 parts of tobias acid and 0.1-2 parts of 2, 6 acid, dissolving, filtering, adding 28.4 parts of hydrochloric acid at the temperature of -3 to 2 DEG C, stirring, adding 30.4 parts of sodium nitrite solution, stirring at the temperature of 0-5 DEG C, adding 56 parts of calcium chloride solution, and stirring to obtain a solution I; stirring 200-720 parts of water and 24.5 parts of sodium hydroxide, adding 16 parts of 2-naphthol to dissolve at the temperature of 20-60 DEG C and filter, and adding 0.1-5.6 parts of rosin solution and 0.1-4 parts of turkey red oil solution into a filtrate at the temperature of 20-60 DEG C to obtain a solution II; adding the solution II into the solution I at the temperature of 0-5 DEG C to couple for 20 minutes, stirring for 30-60 minutes at the temperature of 10-15 DEG C, raising the temperature to 65-90 DEG C to transform completely, stirring for 10-30 minutes, filtering by pressing, washing filter cakes by water, and removing moisture in the filter cakes to obtain the pigment used for water-based ink. The viscosity stability of ink prepared from the pigment used for water-based ink disclosed by the invention is high, and after the treatment of 48 hours at the temperature of 50 DEG C, the viscosity is still basically unchanged.

Description

The preparation method of pigment used for water-based ink
Technical field
The present invention relates to the preparation method of pigment used for water-based ink.
Background technology
At society, the speed of printing press is more and more faster, requires printing ink high strength low viscosity; And common azo lake class pigment, viscosity stability is poor, causes print quality unstable.
Summary of the invention
The preparation method who the purpose of this invention is to provide the pigment used for water-based ink that a kind of ink viscosity stability of preparing is high.
The preparation method of pigment used for water-based ink provided by the present invention, comprise the steps:
50~200 weight parts waters and 22 weight part caustic soda, stir, and adds 22~24 weight part TOBIAS ACID 97MIN.& 98MIN. and 0.1~2 weight part 2,6 acid are dissolved, and filter, and filtrate is cooled to-3~0 ℃, add 28.4 weight part hydrochloric acid, stir, add 30.4 weight part sodium nitrite solutions, 0~5 ℃ of temperature, stir, add 56 weight part calcium chloride solutions, stir, obtain solution I;
200~720 weight parts waters and 24.5 weight part caustic soda, stir, and adds 20~60 ℃ of 16 weight part beta naphthals to dissolve beta naphthal, filter, in filtrate, add 0.1~5.6 weight part rosin solution and the Turkey red oil solution of 0.1~4 weight part, cool to 20~35 ℃, obtain solution II;
Solution II joined in 0~5 ℃ of solution I coupling 20 minutes, and 10~15 ℃ of temperature, stirred 30~60 minutes, was warmed up to 65~90 ℃ and transformed fully, stirred 10~30 minutes, and press filtration, filter cake is washed, and removes the moisture in filter cake, obtains pigment used for water-based ink;
In described caustic soda, the quality percentage composition of sodium hydroxide is 20%; In described hydrochloric acid, the quality percentage composition of HCl is 30%;
The quality percentage composition of described sodium nitrite solution Sodium Nitrite is 25%; In described calcium chloride solution, the quality percentage composition of calcium chloride is 27%; Described rosin solution is that 15 weight parts waters and 5.6 weight part rosin heatings are transparent to solution; Described Turkey red oil solution is that 10 weight parts waters and the intensification of 2 weight part turkey red oils are dissolved turkey red oil.
The ink viscosity stability that pigment used for water-based ink of the present invention is made is high, processes 48 hours for 50 ℃, and viscosity is still substantially unchanged.
Embodiment
Raw materials used in following embodiment:
Caustic soda: the quality percentage composition of sodium hydroxide is 20%;
The quality percentage composition of hydrochloric acid: HCl is 30%;
Sodium nitrite solution: the quality percentage composition of Sodium Nitrite is 25%;
Calcium chloride solution: the quality percentage composition of calcium chloride is 27%;
Beta naphthal: purity 98%;
Rosin solution: 15 weight parts waters and 5.6 weight part rosin heatings to 95 are ℃ transparent to solution;
Turkey red oil solution: 10 weight parts waters and 2 weight part turkey red oils heat up turkey red oil are dissolved;
TOBIAS ACID 97MIN.& 98MIN.: purity 100%.
Embodiment 1,
It is transparent that 50 weight parts waters, 22 weight part caustic soda, stirring add 24 weight part 100% TOBIAS ACID 97MIN.& 98MIN. and 0.1 weight part 6-Hydroxy-2-naphthoic acid to dissolve, pH12, filter, filtrate joins diazotization tank, lowers the temperature-3 ℃, add fast 28.4 weight part hydrochloric acid, stirred 10 minutes, and added 30.4 weight part sodium nitrite solutions, 0 ℃ of stirring of temperature 30 minutes, add 56 weight part calcium chloride solutions, stirred 10 minutes, and joined in the large tank of coupling, 0 ℃ of temperature is treated coupling;
200 weight parts waters, 24.5 weight part caustic soda, the 20 ℃ of stirrings that heat up add the beta naphthal of 16 weight parts transparent to beta naphthal, filter, filtrate joins in diazotization tank, add 0.1 weight part rosin solution and the Turkey red oil solution of 0.1 weight part, cool to 35 ℃, then join in the large tank of coupling;
Coupling 20 minutes, pH8,10 ℃ of temperature, stirred 30 minutes, heat up 65 ℃, stirred pH8 30 minutes, cool to below 50 ℃, press filtration, water are flushed to below water outlet conductivity 200us/cm, and filter cake has rinsed the recession press filtration, on filter cake, baking oven dries moisture content 50% left and right or oven dry, and you are dark red to obtain pigment used for water-based ink-lithol.
Lithol that pigment scarlet 33g (100%), add 27.5g Joncry 61 resin liquid, water 38.5g (filter cake is removed the moisture contained in filter cake), defoamer 1g, be weighed in the stainless steel cup of 400ml, the steel ball of additional 300g 4mm, ground 1 hour in the upper vibration of Red Devil (Red Devil), obtains the heavy colour slurry; Then by Joncryl 89: heavy colour slurry=3: 2 is in harmonious proportion to obtain printing ink, starches by heavy colour: white Nippon=be in harmonious proportion at 2: 50 water down slurry; By printing ink with RDS7# rod blade coating on double gummed paper and enamelled paper, with the RDS14# rod, will water down the slurry blade coating on enamelled paper, the China ink layer is dry rear by Macbeth color-eye 2180 spectrophotometer test ink and to water down paste colors poor.
DL-0.5Da-0.4Db-0.3, DE0.707; Color strength is 100%; Watering down mill base is 105%.
Heavy colour slurry and printing ink, by Zahn cup 3# tested viscosity, are then obturaged heavy colour slurry and printing ink, put into 50 ℃ of baking ovens through 48 hours, take out, lower the temperature 25 ℃ the time and use again Zahn cup 3# tested viscosity.
Viscosity is substantially between 15 seconds to 17 seconds, and stability is between 15 seconds to 16 seconds, and basic do not have to change
Embodiment 2,
It is transparent that 200 weight parts waters, 22 weight part caustic soda, stirring add 23 weight part 100% TOBIAS ACID 97MIN.& 98MIN. and 1 weight part 6-Hydroxy-2-naphthoic acid to dissolve, pH12, filter, filtrate joins diazotization tank, lowers the temperature 0 ℃, add fast 28.4 weight part hydrochloric acid, stirred 10 minutes, and added 30.4 weight part sodium nitrite solutions, 5 ℃ of stirrings of temperature 30 minutes, add 56 weight part calcium chloride solutions, stirred 10 minutes, and joined in the large tank of coupling, 5 ℃ of temperature are treated coupling;
720 weight parts waters, 24.5 weight part caustic soda, the 60 ℃ of stirrings that heat up add the beta naphthal of 16 weight parts transparent to beta naphthal, filter, filtrate joins in diazotization tank, add 5.6 weight part rosin solutions and the Turkey red oil solution of 4 weight parts, cool to 20 ℃, then join in the large tank of coupling;
Coupling 20 minutes, pH8,15 ℃ of temperature, stirred 60 minutes, heat up 90 ℃, stirred pH8 10 minutes, cool to below 50 ℃, press filtration, water are flushed to below water outlet conductivity 200us/cm, and filter cake has rinsed the recession press filtration, on filter cake, baking oven dries moisture content 50% left and right or oven dry, and you are dark red to obtain pigment used for water-based ink-lithol.
Lithol that pigment scarlet 33g (100%), add 27.5g Joncry 61 resin liquid, water 38.5g (filter cake is removed the moisture contained in filter cake), defoamer 1g, be weighed in the stainless steel cup of 400ml, the steel ball of additional 300g 4mm, ground 1 hour in the upper vibration of Red Devil (RedDevil), obtains the heavy colour slurry; Then by Joncryl 89: heavy colour slurry=3: 2 is in harmonious proportion to obtain printing ink, starches by heavy colour: white Nippon=be in harmonious proportion at 2: 50 water down slurry; By printing ink with RDS7# rod blade coating on double gummed paper and enamelled paper, with the RDS14# rod, will water down the slurry blade coating on enamelled paper, the China ink layer is dry rear by Macbeth color-eye 2180 spectrophotometer test ink and to water down paste colors poor.
DL-0.9Da-0.8Db-0.5, DE1.3; Color strength is 103%; Watering down mill base is 110%.
Heavy colour slurry and printing ink, by Zahn cup3# tested viscosity, are then obturaged heavy colour slurry and printing ink, put into 50 ℃ of baking ovens through 48 hours, take out, lower the temperature 25 ℃ the time and use again Zahn cup3# tested viscosity.
Viscosity is substantially between 15 seconds to 17 seconds, and stability is between 15 seconds to 16 seconds, and basic do not have to change
Embodiment 3,
It is transparent that 100 weight parts waters, 22 weight part caustic soda, stirring add 22 weight part 100% TOBIAS ACID 97MIN.& 98MIN. and 2 weight part 6-Hydroxy-2-naphthoic acids to dissolve, pH12, filter, filtrate joins diazotization tank, lowers the temperature 0 ℃, add fast 28.4 weight part hydrochloric acid, stirred 10 minutes, and added 30.4 weight part sodium nitrite solutions, 5 ℃ of stirrings of temperature 30 minutes, add 56 weight part calcium chloride solutions, stirred 10 minutes, and joined in the large tank of coupling, 5 ℃ of temperature are treated coupling;
300 weight parts waters, 24.5 weight part caustic soda, the 60 ℃ of stirrings that heat up add the beta naphthal of 16 weight parts transparent to beta naphthal, filter, filtrate joins in diazotization tank, add 3.0 weight part rosin solutions and the Turkey red oil solution of 2.0 weight parts, cool to 20 ℃, then join in the large tank of coupling;
Coupling 20 minutes, pH8,15 ℃ of temperature, stirred 60 minutes, heat up 75 ℃, stirred pH8 30 minutes, cool to below 50 ℃, press filtration, water are flushed to below water outlet conductivity 200us/cm, and filter cake has rinsed the recession press filtration, on filter cake, baking oven dries moisture content 50% left and right or oven dry, and you are dark red to obtain pigment used for water-based ink-lithol.
Lithol that pigment scarlet 33g (100%), add 27.5g Joncry 61 resin liquid, water 38.5g (filter cake is removed the moisture contained in filter cake), defoamer 1g, be weighed in the stainless steel cup of 400ml, the steel ball of additional 300g 4mm, ground 1 hour in the upper vibration of Red Devil (RedDevil), obtains the heavy colour slurry; Then by Joncryl 89: heavy colour slurry=3: 2 is in harmonious proportion to obtain printing ink, starches by heavy colour: white Nippon=be in harmonious proportion at 2: 50 water down slurry; By printing ink with RDS7# rod blade coating on double gummed paper and enamelled paper, with the RDS14# rod, will water down the slurry blade coating on enamelled paper, the China ink layer is dry rear by Macbeth color-eye 2180 spectrophotometer test ink and to water down paste colors poor.
DL-1.2Da-1.3Db-1.0, DE2.03; Color strength is 104%; Watering down mill base is 115%.
Heavy colour slurry and printing ink, by Zahn cup3# tested viscosity, are then obturaged heavy colour slurry and printing ink, put into 50 ℃ of baking ovens through 48 hours, take out, lower the temperature 25 ℃ the time and use again Zahn cup3# tested viscosity.
Viscosity is substantially between 15 seconds to 17 seconds, and stability is between 15 seconds to 16 seconds, and basic do not have to change
Above embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention, all should fall in the definite protection domain of claims of the present invention.

Claims (1)

1. the preparation method of pigment used for water-based ink, comprise the steps:
50~200 weight parts waters and 22 weight part caustic soda, stir, and adds 22~24 weight part TOBIAS ACID 97MIN.& 98MIN. and 0.1~2 weight part 2,6 acid are dissolved, and filter, and filtrate is cooled to-3~0 ℃, add 28.4 weight part hydrochloric acid, stir, add 30.4 weight part sodium nitrite solutions, 0~5 ℃ of temperature, stir, add 56 weight part calcium chloride solutions, stir, obtain solution I;
200~720 weight parts waters and 24.5 weight part caustic soda, stir, and adds 16 weight part beta naphthals, 20~60 ℃ dissolve beta naphthal, filter, and in filtrate, add 0.1~5.6 weight part rosin solution and the Turkey red oil solution of 0.1~4 weight part, cool to 20~35 ℃, obtain solution II;
Solution II joined in 0~5 ℃ of solution I coupling 20 minutes, and 10~15 ℃ of temperature, stirred 30~60 minutes, was warmed up to 65~90 ℃ and transformed fully, stirred 10~30 minutes, and press filtration, filter cake is washed, and removes the moisture in filter cake, obtains pigment used for water-based ink;
In described caustic soda, the quality percentage composition of sodium hydroxide is 20%; In described hydrochloric acid, the quality percentage composition of HCl is 30%;
The quality percentage composition of described sodium nitrite solution Sodium Nitrite is 25%; In described calcium chloride solution, the quality percentage composition of calcium chloride is 27%; Described rosin solution is that 15 weight parts waters and 5.6 weight part rosin heatings are transparent to solution; Described Turkey red oil solution is 10 weight parts waters and 2 weight part turkey red oils, heats up turkey red oil is dissolved.
CN2010102190110A 2010-07-07 2010-07-07 Preparation method of pigment used for water-based ink Active CN102311658B (en)

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CN104098923B (en) * 2014-07-25 2016-04-06 嘉兴科隆化工有限公司 A kind of machine side separates out industrialized preparing process and the machine side precipitation detection method thereof of few red

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5614013A (en) * 1993-10-20 1997-03-25 Ciba-Geigy Corporation Pigment compositions
CN101161735A (en) * 2006-10-12 2008-04-16 株式会社御牧工程 Penetration inhibitor, penetration inhibiting method, and solvent inkjet ink

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JPH1046086A (en) * 1996-08-01 1998-02-17 Sanyo Shikiso Kk Azolake pigment composition
DE10049200A1 (en) * 2000-10-05 2002-04-11 Clariant Gmbh Process for the production of azo colorants
US6610133B2 (en) * 2000-12-20 2003-08-26 Basf Corporation Dispersions for use in ink jet inks

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5614013A (en) * 1993-10-20 1997-03-25 Ciba-Geigy Corporation Pigment compositions
CN101161735A (en) * 2006-10-12 2008-04-16 株式会社御牧工程 Penetration inhibitor, penetration inhibiting method, and solvent inkjet ink

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* Cited by examiner, † Cited by third party
Title
JP特开平10-46086A 1998.02.17

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Address after: 265705 No.1 Cong street, zhuyouguan Town, Longkou City, Yantai City, Shandong Province

Patentee after: Longkou United Chemical Co.,Ltd.

Address before: 265705 No.1 Cong street, zhuyouguan Town, Longkou City, Yantai City, Shandong Province

Patentee before: LONGKOU UNION CHEMICAL Co.,Ltd.