CN105295424A - Preparation method of pigment yellow 168 - Google Patents
Preparation method of pigment yellow 168 Download PDFInfo
- Publication number
- CN105295424A CN105295424A CN201510661830.3A CN201510661830A CN105295424A CN 105295424 A CN105295424 A CN 105295424A CN 201510661830 A CN201510661830 A CN 201510661830A CN 105295424 A CN105295424 A CN 105295424A
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- Prior art keywords
- pigment yellow
- preparation
- solution
- degrees celsius
- fully
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- 239000000049 pigment Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000005859 coupling reaction Methods 0.000 claims abstract description 15
- 230000008878 coupling Effects 0.000 claims abstract description 6
- 238000010168 coupling process Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 235000010288 sodium nitrite Nutrition 0.000 claims description 9
- VZLLZDZTQPBHAZ-UHFFFAOYSA-N 2-nitroaniline-4-sulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1[N+]([O-])=O VZLLZDZTQPBHAZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012954 diazonium Substances 0.000 claims description 5
- 150000001989 diazonium salts Chemical class 0.000 claims description 5
- CJLSDBRIXZFCKV-UHFFFAOYSA-N 4-chloro-3-oxo-n-phenylbutanamide Chemical group ClCC(=O)CC(=O)NC1=CC=CC=C1 CJLSDBRIXZFCKV-UHFFFAOYSA-N 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 2
- 125000000664 diazo group Chemical group [N-]=[N+]=[*] 0.000 abstract 2
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 238000006193 diazotization reaction Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 230000036632 reaction speed Effects 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Paints Or Removers (AREA)
Abstract
The invention relates to a preparation method of pigment yellow 168, and belongs to the field of chemical engineering. The method mainly comprises the following steps of diazo salt preparation, diazotization, coupling, precipitation, filtering, drying and the like. The preparation method of the pigment yellow 168 provided by the invention has the advantages in the coupling stage, an ice bath mode is used for controlling the temperature; the temperature of the existing coupling reaction is generally controlled at 5 to 10 DEG C; the inventor of the invention discovers that at 0 to 2 DEG C, the reaction speed is the highest; the product color is bright, so that too dark color of a final product due to the diazo salt caused by too long coupling reaction time is avoided.
Description
Technical field
The present invention relates to a kind of preparation method of Pigment Yellow 73 168, belong to chemical field.
Background technology
Pigment Yellow 73 168 is mainly used in the painted of coating and plastics, has good resistance to migration energy in plasticity PVC.In existing Pigment Yellow 73 manufacturing process, in the coupled reaction stage, because diazonium salt is easily hydrolyzed, cause product performance unstable, therefore, coupled reaction becomes this pigment dyestuff production technique always most important ring.In general, coupled reaction more abundant, then product quality is higher.And existing coupled reaction, as required, be generally selected in 5 to 10 degrees Celsius, or 15 to 20 degrees Celsius are carried out, and the product obtained like this, its luminance shortage, the look power that also just result in Pigment Yellow 73 168 is lower.
Summary of the invention
The present invention wants technical solution problem to be: the shortcoming overcoming above-mentioned technology, provides a kind of preparation method that can carry out the Pigment Yellow 73 168 of coupled reaction fast.
In order to solve the problems of the technologies described above, the technical scheme that the present invention proposes is: a kind of preparation method of Pigment Yellow 73 168, comprises the following steps:
(1) by 2-nitro-4-sulfo aniline, be dissolved in hydrochloric acid;
(2) solution is cooled to lower than 5 degrees Celsius with ice bath;
(3) add Sodium Nitrite and fully stir, forming diazonium salt solution;
(4) after the mixing of sodium hydroxide solution, water and adjacent chloracetyl Acetanilide also fully being stirred, adding acetum and also stir, to forming suspended particles, keeping stirring;
(5) solution of step (3) is added in the solution of step (4) carries out coupling, and fully stir, simultaneously with ice bath cooling, make mixeding liquid temperature lower than 2 degrees Celsius;
(6) add calcium oxide, and be heated to 30 to 45 degrees Celsius; Be incubated 20 minutes; It is made fully to be precipitated as color lake;
(7) Pigment Yellow 73 168 is namely obtained after filtration, washing, drying; After grinding, namely obtain described Pigment Yellow 73 168 powder.
Such scheme further improves and is: in step (4), and the acetum concentration used is 15.5%.
Such scheme further improves and is: in described step (3), uses urea to destroy excessive Sodium Nitrite.
Such scheme further improves and is: in described step (1), and concentration of hydrochloric acid is 40%.
Such scheme further improves and is: at the 2-nitro-4-sulfo aniline of described step (1), be 1.6:1 to 1.8:1 with the mass ratio of the Sodium Nitrite in step (3).
The preparation method of Pigment Yellow 73 168 provided by the invention, in the coupling stage with ice bath mode control temperature, existing coupled reaction temperature general control is at 5 to 10 degrees Celsius, the present inventor then finds, 0 to 2 degrees Celsius time, speed of response is the quickest, and product colour is bright.Thus avoid, because of coupled reaction overlong time, causing diazonium salt, cause the finished product color excessively dark.
Embodiment
Embodiment
The preparation method of the Pigment Yellow 73 168 that the present embodiment provides, comprises the following steps:
(1) by 2-nitro-4-sulfo aniline, be dissolved in hydrochloric acid;
(2) solution is cooled to lower than 5 degrees Celsius with ice bath;
(3) add Sodium Nitrite and fully stir, forming diazonium salt solution;
(4) after the mixing of sodium hydroxide solution, water and adjacent chloracetyl Acetanilide also fully being stirred, adding acetum and also stir, to forming suspended particles, keeping stirring;
(5) solution of step (3) is added in the solution of step (4) carries out coupling, and fully stir, simultaneously with ice bath cooling, make mixeding liquid temperature lower than 2 degrees Celsius;
(6) add calcium oxide, and be heated to 30 to 45 degrees Celsius; Be incubated 20 minutes; It is made fully to be precipitated as color lake
(7) Pigment Yellow 73 168 is namely obtained after filtration, washing, drying; After grinding, namely obtain described Pigment Yellow 73 168 powder.
In step (4), the acetum concentration used is 15.5%.
In step (3), urea is used to destroy excessive Sodium Nitrite.
In step (1), concentration of hydrochloric acid is 40%.
In the 2-nitro-4-sulfo aniline of step (1), be 1.6:1 to 1.8:1 with the mass ratio of the Sodium Nitrite in step (3).
The Pigment Yellow 73 168 obtained in the present embodiment, brightness significantly improves, and improves the shortcoming that this pigment colour power is weak greatly.
The present invention is not limited to the concrete technical scheme of above-described embodiment, and in addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacing and being formed, and are the protection domain of application claims.
Claims (5)
1. a preparation method for Pigment Yellow 73 168, is characterized in that, comprises the following steps:
(1) by 2-nitro-4-sulfo aniline, be dissolved in hydrochloric acid;
(2) solution is cooled to lower than 5 degrees Celsius with ice bath;
(3) add Sodium Nitrite and fully stir, forming diazonium salt solution;
(4) after the mixing of sodium hydroxide solution, water and adjacent chloracetyl Acetanilide also fully being stirred, adding acetum and also stir, to forming suspended particles, then keeping stirring;
(5) solution of step (3) is added in the solution of step (4) carries out coupling, and fully stir, simultaneously with ice bath cooling, make mixeding liquid temperature lower than 2 degrees Celsius;
(6) add calcium oxide, and be heated to 30 to 45 degrees Celsius; Be incubated 20 minutes, make it fully be precipitated as color lake;
(7) Pigment Yellow 73 168 is namely obtained after filtration, washing, drying; After grinding, namely obtain described Pigment Yellow 73 168 powder.
2. the preparation method of Pigment Yellow 73 168 as claimed in claim 1, it is characterized in that: in described step (4), the acetum concentration used is 15.5%.
3. the preparation method of Pigment Yellow 73 168 as claimed in claim 1, is characterized in that: in described step (3), uses urea to destroy excessive Sodium Nitrite.
4. the preparation method of Pigment Yellow 73 168 as claimed in claim 1, it is characterized in that: in described step (1), concentration of hydrochloric acid is 40%.
5. the preparation method of Pigment Yellow 73 168 as claimed in claim 1, is characterized in that: at the 2-nitro-4-sulfo aniline of described step (1), be 1.6:1 to 1.8:1 with the mass ratio of the Sodium Nitrite in step (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510661830.3A CN105295424A (en) | 2015-10-15 | 2015-10-15 | Preparation method of pigment yellow 168 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510661830.3A CN105295424A (en) | 2015-10-15 | 2015-10-15 | Preparation method of pigment yellow 168 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105295424A true CN105295424A (en) | 2016-02-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510661830.3A Pending CN105295424A (en) | 2015-10-15 | 2015-10-15 | Preparation method of pigment yellow 168 |
Country Status (1)
| Country | Link |
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| CN (1) | CN105295424A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4304711A (en) * | 1978-03-18 | 1981-12-08 | Ciba-Geigy Corporation | Pigment compositions |
| US4523953A (en) * | 1982-12-06 | 1985-06-18 | Montedison S.P.A. | Photostable yellow composite pigments and process for their preparation |
| JP2004170825A (en) * | 2002-11-22 | 2004-06-17 | Canon Inc | Yellow toner |
-
2015
- 2015-10-15 CN CN201510661830.3A patent/CN105295424A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4304711A (en) * | 1978-03-18 | 1981-12-08 | Ciba-Geigy Corporation | Pigment compositions |
| US4523953A (en) * | 1982-12-06 | 1985-06-18 | Montedison S.P.A. | Photostable yellow composite pigments and process for their preparation |
| JP2004170825A (en) * | 2002-11-22 | 2004-06-17 | Canon Inc | Yellow toner |
Non-Patent Citations (2)
| Title |
|---|
| 秦云: "重氮化与偶合反应的理论研究", 《保山师专学报》 * |
| 马飞飞: "由双乙烯酮衍生的乙酰基乙酰芳胺类色淀颜料", 《乙醛醋酸化工》 * |
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Application publication date: 20160203 |