CN106634040A - Preparation method of red pigment - Google Patents
Preparation method of red pigment Download PDFInfo
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- CN106634040A CN106634040A CN201610751330.3A CN201610751330A CN106634040A CN 106634040 A CN106634040 A CN 106634040A CN 201610751330 A CN201610751330 A CN 201610751330A CN 106634040 A CN106634040 A CN 106634040A
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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
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a preparation method of a red pigment. The red pigment is prepared by 1, filling 2000 parts of water in a heavy nitrogen bucket, pouring 2B acid, ammonia water, 230 parts of hydrochloric acid, and sodium nitrite solution for future use; 2) filling 1500 parts of water in a dissolving bucket, pouring 2, 3 acid, and sodium hydroxide solution; stirring for 20 minutes and dissolving clearly; filling the mixture in a coupling bucket; 3, adding water, potassium hydroxide, and maleic rosin in a rosin bucket; dissolving and putting in the coupling bucket; 4, adding water to the coupling bucket and adjusting volume to 3000 parts of water; putting the solution prepared in step 1 to the coupling bucket; meanwhile, controlling pH value=9.0-10.0 by 5%-10% of sodium hydroxide solution convection, keeping heavy nitrogen free from too heavy, and stirring for 20 minutes; adding 15 parts of Solsperse 20000, adding calcium chloride water solution; stirring and adding 12-hydroxy oil acid; raising temperature to 50 DEG C; adding strontium chloride solution in the coupling bucket, filter-pressing and rinsing the solution for 2 hours, and acquiring a finished product. The finished product is fresh in color, high in transparency, strong in coloring force, low in oil absorption, and high in gloss.
Description
Technical field
The invention belongs to pigment production processing technique field, specifically a kind of preparation method of red pigment.
Background technology
Pigment is the powdered substance for colouring.Do not dissolve in the media such as water, grease, resin, organic solvent, but energy
Equably disperse in these media and colour can medium, so as to have certain covering power.
Also increasingly stronger to the cry of environmental protection with national policy and the improvement of people's living standards, all trades and professions are all
First place is mentioned in environmental protection.Ink market also and then makes the transition, and originally benzene kind solvent ink gradually fades out market, alkoxide environment-friendly type oil
Ink is more and more prosperous.And then some are delayed to be applied to the organic pigment of this kind of ink, particularly laked azo class organic pigment,
P.R.48:2（Sun-proof bright red BBC）, the Shortcomings in terms of adaptability, viscosity, transparency and gloss, not color development, viscosity is too high,
Transparency and gloss are inadequate.
The content of the invention
The present invention is not enough for prior art, there is provided a kind of preparation method of red pigment, is made using the preparation method
Pigment have bright-colored, transparency is high, strong coloring force, low oil absorption ferric, the characteristic of high glaze.
In order to solve above-mentioned technical problem, the present invention is addressed by following technical proposals：A kind of system of red pigment
Preparation Method, comprises the following steps：Following number is mass fraction, and 1, discharge water in diazonium bucket 2000 parts, 30 DEG C of temperature is adjusted,
Pour 150 parts of 2B acid into, pour 80 parts of 20% ammoniacal liquor into, stirring is fully dissolved, after the dissolving completely of PH=8.5～9,5-10 is put in minute
Enter 230 parts of 30% hydrochloric acid, then the volume for being cooled to -3 ~ 0 DEG C, adjusting volume to 4000 parts of water on the rocks, adds in 10-15 minutes
The sodium nitrite in aqueous solution of 160 part of 30% mass fraction, continues to react 40 minutes, and terminal PH=1,0 ~ 5 DEG C of storage temperature is standby；
2, discharge water in dissolving bucket 1500 parts, 35-40 DEG C is warming up to, pour the sodium hydrate aqueous solution that 2,3 218 parts of acid are put into 30% into
180 parts, stir 20 minutes, molten net, in being put into coupling bucket, adjustment temperature is 15 DEG C, add water the body that adjustment volume is 2000 parts of water
Product；3,100 parts of water are added in rosin bucket, 7.5 parts of potassium hydroxide are added, boiling is warming up to, 15 parts of maleic rosins are added, change
Clearly, 15 DEG C are cooled to, in being put into coupling bucket；4, add water the volume adjusted to 3000 parts of water of volume in coupling bucket, controls temperature 8-
10 DEG C, obtained solution in step 1 is put at 10 ~ 15 minutes in coupling bucket, while with the sodium hydroxide solution pair of 5%-10%
Stream control PH=9.0-10.0, terminal PH is in 9.2-9.5 for control, and temperature 7-10 DEG C, diazonium is not overweight, stirs 20 minutes, adds 15
Part Solsperse20000, is cooled to 0-3 DEG C, and 450 parts of mass fractions of addition are 33.33% calcium chloride water within 5-8 minutes
Solution, stirs 60 minutes, adds 15 parts of 12- hydroxy oleates, is warming up to 50 DEG C, and 26.4 parts of strontium chlorides are dissolved in 100 parts of water simultaneously
During coupling bucket is added within 3-5 minutes, 80 DEG C are continuously heating to, are incubated 15 minutes, be cooled to 60 DEG C, adjust PH=6.0, stirring
10 minutes, press filtration rinsed 2 hours, the amount of obtaining：357 parts.Pigment prepared by the present invention improves the dispersion in environment-friendly ink
Property and stability, and reduce viscosity, improve gloss, and have good surface-active to the solvent in environment-friendly ink system, and
There is plasticization to its resin, viscosity can be reduced.
The present invention compared with prior art, has the advantages that：Improved using red pigment obtained in this kind of method
Dispersiveness and stability in environment-friendly ink, and viscosity is reduced, gloss is improved, and to the solvent in environment-friendly ink system
There is good surface-active, and have plasticization to its resin, viscosity can be reduced.
Specific embodiment
The present invention is described in further detail with reference to specific embodiment：Embodiment 1, a kind of system of red pigment
Preparation Method, comprises the following steps：Following number is mass fraction, and 1, discharge water in diazonium bucket 2000 parts, 30 DEG C of temperature is adjusted,
Pour 150 parts of 2B acid into, pour 80 parts of 20% ammoniacal liquor into, stirring fully dissolving after PH=8.5 dissolvings completely, is put into 30% salt in 5 minutes
230 parts of acid, then the volume for being cooled to -3 DEG C, adjusting volume to 4000 parts of water on the rocks, at 10 minutes 160 part of 30% mass was added
The sodium nitrite in aqueous solution of fraction, continues to react 40 minutes, and terminal PH=1,0 DEG C of storage temperature is standby；2, put in dissolving bucket
1500 parts of water, is warming up to 35 DEG C, pours 180 parts of the sodium hydrate aqueous solution that 2,3 218 parts of acid are put into 30% into, stirs 20 minutes, molten
Only, in being put into coupling bucket, adjustment temperature is 15 DEG C, and add water the volume that adjustment volume is 2000 parts of water；3, add in rosin bucket
100 parts of water, add 7.5 parts of potassium hydroxide, are warming up to boiling, add 15 parts of maleic rosins, change clearly, are cooled to 15 DEG C, are put into idol
In closing bucket；4, add water the volume adjusted to 3000 parts of water of volume in coupling bucket, controls 8 DEG C of temperature, will make in step 1 at 10 minutes
Solution be put into coupling bucket, while with 5% sodium hydroxide solution convection current control PH=9.0, control terminal PH 9.2, temperature 7
DEG C, diazonium is not overweight, stirs 20 minutes, adds 15 parts of Solsperse20000, is cooled to 0 DEG C, and 450 parts were added in 5 minutes
Mass fraction is 33.33% calcium chloride water, is stirred 60 minutes, adds 15 parts of 12- hydroxy oleates, is warming up to 50 DEG C, will
26.4 parts of strontium chlorides are dissolved in 100 parts of water and were added in 3 minutes in coupling bucket, are continuously heating to 80 DEG C, are incubated 15 minutes,
60 DEG C are cooled to, PH=6.0 is adjusted, are stirred 10 minutes, press filtration, rinse 2 hours, the amount of obtaining：357 parts.
A kind of embodiment 2, preparation method of red pigment, comprises the following steps：Following number is mass fraction, and 1,
Discharge water in diazonium bucket 2000 parts, adjust 30 DEG C of temperature, pour 150 parts of 2B acid into, pour 80 parts of 20% ammoniacal liquor, stirring fully dissolving, PH into
After=9 dissolvings completely, 230 parts of 30% hydrochloric acid is put into 10 minutes, it is then on the rocks to be cooled to 0 DEG C, volume is adjusted to 4000 parts of water
Volume, the sodium nitrite in aqueous solution of 160 part of 30% mass fraction was added at 15 minutes, continued to react 40 minutes, and terminal PH=1 is protected
5 DEG C of temperature is deposited, it is standby；2, discharge water in dissolving bucket 1500 parts, 40 DEG C are warming up to, pour the hydrogen-oxygen that 2,3 218 parts of acid are put into 30% into
Change 180 parts of sodium water solution, stir 20 minutes, molten net, in being put into coupling bucket, adjustment temperature is 15 DEG C, the adjustment volume that adds water is
The volume of 2000 parts of water；3,100 parts of water are added in rosin bucket, 7.5 parts of potassium hydroxide are added, boiling is warming up to, add 15 parts
Maleic rosin, changes clearly, is cooled to 15 DEG C, in being put into coupling bucket；4, add water the volume adjusted to 3000 parts of water of volume in coupling bucket,
10 DEG C of temperature of control, was put into obtained solution in step 1 at 15 minutes in coupling bucket, while with 10% sodium hydroxide solution
Convection current control PH=10.0, terminal PH is 9.5 for control, 10 DEG C of temperature, and diazonium is not overweight, stirs 20 minutes, adds 15 parts
Solsperse20000, is cooled to 3 DEG C, and 450 parts of mass fractions of addition are 33.33% calcium chloride water in 8 minutes, are stirred
Mix 60 minutes, add 15 parts of 12- hydroxy oleates, be warming up to 50 DEG C, 26.4 parts of strontium chlorides are dissolved in 100 parts of water and in 5 minutes
In being inside added to coupling bucket, 80 DEG C are continuously heating to, are incubated 15 minutes, be cooled to 60 DEG C, adjust PH=6.0, stirred 10 minutes, pressure
Filter, rinses 2 hours, the amount of obtaining：357 parts.
A kind of embodiment 3, preparation method of red pigment, comprises the following steps：Following number is mass fraction, and 1,
Discharge water in diazonium bucket 2000 parts, adjust 30 DEG C of temperature, pour 150 parts of 2B acid into, pour 80 parts of 20% ammoniacal liquor, stirring fully dissolving, PH into
After=8.7 dissolvings completely, 230 parts of 30% hydrochloric acid is put into 8 minutes, then on the rocks to be cooled to -2 DEG C, adjustment volume is to 4000 parts of water
Volume, add the sodium nitrite in aqueous solution of 160 part of 30% mass fraction in 10-15 minutes, continue to react 40 minutes, terminal PH
=1,3 DEG C of storage temperature is standby；2, discharge water in dissolving bucket 1500 parts, 38 DEG C are warming up to, pour 2,3 218 parts of acid into and be put into 30%
180 parts of sodium hydrate aqueous solution, stir 20 minutes, molten net, in being put into coupling bucket, adjustment temperature is 15 DEG C, and add water adjusting body
Product is the volume of 2000 parts of water；3,100 parts of water are added in rosin bucket, 7.5 parts of potassium hydroxide are added, boiling is warming up to, add
15 parts of maleic rosins, change clearly, are cooled to 15 DEG C, in being put into coupling bucket；4, add water in coupling bucket and adjust to 3000 parts of water of volume
Volume, controls 9 DEG C of temperature, is put into obtained solution in step 1 at 13 minutes in coupling bucket, while molten with 8% NaOH
Liquid convection current control PH=9.5, terminal PH is 9.3 for control, 9 DEG C of temperature, and diazonium is not overweight, stirs 20 minutes, adds 15 parts
Solsperse20000, is cooled to 1 DEG C, and 450 parts of mass fractions of addition are 33.33% calcium chloride water in 7 minutes, are stirred
Mix 60 minutes, add 15 parts of 12- hydroxy oleates, be warming up to 50 DEG C, 26.4 parts of strontium chlorides are dissolved in 100 parts of water and in 4 minutes
In being inside added to coupling bucket, 80 DEG C are continuously heating to, are incubated 15 minutes, be cooled to 60 DEG C, adjust PH=6.0, stirred 10 minutes, pressure
Filter, rinses 2 hours, the amount of obtaining：357 parts.
Solsperse20000 the and 12- hydroxy oleates used using pigment obtained in the various embodiments described above and its ratio
Example, is screened through meticulous, and repeatedly experiment carries out application authorization, is just established.It is gorgeous that Solsperse20000 improves sun-proof
Red BBC pigment, the dispersiveness and stability in environment-friendly ink, and viscosity is reduced, improve gloss, 12- hydroxy oleates, to environmental protection
Solvent in ink system has good surface-active, and has plasticization to its resin, can reduce viscosity.The face so as to made by
Material has bright-colored, transparency height, strong coloring force, low oil absorption ferric, the characteristic of high glaze.
Claims (1)
1. a kind of preparation method of red pigment, it is characterised in that：Comprise the following steps：Following number is mass fraction, and 1,
Discharge water in diazonium bucket 2000 parts, adjust 30 DEG C of temperature, pour 150 parts of 2B acid into, pour 80 parts of 20% ammoniacal liquor into, stirring is fully dissolved,
After the dissolving completely of PH=8.5～9,230 parts of 30% hydrochloric acid is put into 5-10 minutes, then on the rocks to be cooled to -3 ~ 0 DEG C, adjusting body
The volume of product to 4000 parts of water, the sodium nitrite in aqueous solution of 160 part of 30% mass fraction is added in 10-15 minutes, continues to react
40 minutes, terminal PH=1,0 ~ 5 DEG C of storage temperature was standby；2, discharge water in dissolving bucket 1500 parts, 35-40 DEG C is warming up to, pour into
2,3 218 parts of acid are put into 30% 180 parts of sodium hydrate aqueous solution, stir 20 minutes, molten net, in being put into coupling bucket, adjust temperature
For 15 DEG C, add water the volume that adjustment volume is 2000 parts of water；3,100 parts of water are added in rosin bucket, add 7.5 parts of hydroxides
Potassium, is warming up to boiling, adds 15 parts of maleic rosins, changes clearly, is cooled to 15 DEG C, in being put into coupling bucket；4, add water tune in coupling bucket
The whole volume to 3000 parts of water of volume, controls temperature 8-10 DEG C, and obtained solution in step 1 is put into coupling at 10 ~ 15 minutes
In bucket, while with the sodium hydroxide solution convection current control PH=9.0-10.0 of 5%-10%, controlling terminal PH in 9.2-9.5, temperature 7-
10 DEG C, diazonium is not overweight, stirs 20 minutes, adds 15 parts of Solsperse20000, is cooled to 0-3 DEG C, adds within 5-8 minutes
Enter the calcium chloride water that 450 parts of mass fractions are 33.33%, stir 60 minutes, add 15 parts of 12- hydroxy oleates, be warming up to 50
DEG C, 26.4 parts of strontium chlorides are dissolved in 100 parts of water and are added within 3-5 minutes in coupling bucket, 80 DEG C are continuously heating to, insulation
15 minutes, 60 DEG C are cooled to, adjust PH=6.0, stirred 10 minutes, press filtration, rinse 2 hours, the amount of obtaining：357 parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610751330.3A CN106634040A (en) | 2016-08-30 | 2016-08-30 | Preparation method of red pigment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610751330.3A CN106634040A (en) | 2016-08-30 | 2016-08-30 | Preparation method of red pigment |
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| CN106634040A true CN106634040A (en) | 2017-05-10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762360A (en) * | 2019-01-16 | 2019-05-17 | 杭州映山花颜料化工有限公司 | A kind of azo dyes automatic production process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1119196A (en) * | 1994-07-20 | 1996-03-27 | 拜尔公司 | Azo dyestuffs with a chlorotrazine group |
| EP0881267A1 (en) * | 1996-10-11 | 1998-12-02 | Kabushiki Kaisha Ueno Seiyaku Oyo Kenkyujo | Azo compounds and process for preparing the same |
| CN1760283A (en) * | 2005-09-30 | 2006-04-19 | 河南黄河旋风股份有限公司 | Method for preparing Nano red organic pigment |
| CN102732052A (en) * | 2012-05-29 | 2012-10-17 | 吴江市屯村颜料厂 | Preparation method for 3120 light fast brilliant red BBC |
| CN103044948A (en) * | 2013-01-06 | 2013-04-17 | 上虞市东海化工有限公司 | Preparation method of red pigment |
| CN103254661A (en) * | 2013-05-14 | 2013-08-21 | 嘉兴科隆化工有限公司 | Industrialized production method of transference-resistant blue light red pigment for PU (Poly Urethane) |
| CN103387754A (en) * | 2013-08-09 | 2013-11-13 | 嘉兴科隆化工有限公司 | Method for producing pigment red 48:2 with excellent heat resistance and migration resistance |
| CN103937333A (en) * | 2014-04-18 | 2014-07-23 | 广州艾科化学有限公司 | Mill base for foaming waterborne polyurethane |
| CN105062222A (en) * | 2015-07-24 | 2015-11-18 | 吴江市屯村颜料厂 | Pigment fast brilliant red BBC dispersion and preparation method therefor |
-
2016
- 2016-08-30 CN CN201610751330.3A patent/CN106634040A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1119196A (en) * | 1994-07-20 | 1996-03-27 | 拜尔公司 | Azo dyestuffs with a chlorotrazine group |
| EP0881267A1 (en) * | 1996-10-11 | 1998-12-02 | Kabushiki Kaisha Ueno Seiyaku Oyo Kenkyujo | Azo compounds and process for preparing the same |
| CN1760283A (en) * | 2005-09-30 | 2006-04-19 | 河南黄河旋风股份有限公司 | Method for preparing Nano red organic pigment |
| CN102732052A (en) * | 2012-05-29 | 2012-10-17 | 吴江市屯村颜料厂 | Preparation method for 3120 light fast brilliant red BBC |
| CN103044948A (en) * | 2013-01-06 | 2013-04-17 | 上虞市东海化工有限公司 | Preparation method of red pigment |
| CN103254661A (en) * | 2013-05-14 | 2013-08-21 | 嘉兴科隆化工有限公司 | Industrialized production method of transference-resistant blue light red pigment for PU (Poly Urethane) |
| CN103387754A (en) * | 2013-08-09 | 2013-11-13 | 嘉兴科隆化工有限公司 | Method for producing pigment red 48:2 with excellent heat resistance and migration resistance |
| CN103937333A (en) * | 2014-04-18 | 2014-07-23 | 广州艾科化学有限公司 | Mill base for foaming waterborne polyurethane |
| CN105062222A (en) * | 2015-07-24 | 2015-11-18 | 吴江市屯村颜料厂 | Pigment fast brilliant red BBC dispersion and preparation method therefor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762360A (en) * | 2019-01-16 | 2019-05-17 | 杭州映山花颜料化工有限公司 | A kind of azo dyes automatic production process |
| CN109762360B (en) * | 2019-01-16 | 2020-07-21 | 杭州映山花颜料化工有限公司 | Automatic production process of azo dye |
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Application publication date: 20170510 |
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