CN1746227A - Production of paint red 254 - Google Patents
Production of paint red 254 Download PDFInfo
- Publication number
- CN1746227A CN1746227A CN 200510094325 CN200510094325A CN1746227A CN 1746227 A CN1746227 A CN 1746227A CN 200510094325 CN200510094325 CN 200510094325 CN 200510094325 A CN200510094325 A CN 200510094325A CN 1746227 A CN1746227 A CN 1746227A
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- CN
- China
- Prior art keywords
- amyl alcohol
- pigment red
- tertiary amyl
- production method
- sodium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Production of pigment red 254 is prepared by adding chlorphenterzine into tert-amyl sodium solution, agitating, dissolving, lowering temperature to 80 Deg C., dripping into mixed liquid of disproester succinate and tert-amyl, keeping temperature at 110-130 Deg C. for 2-5hrs, distilling, collecting tert-amyl, adding into water, agitating, extracting, filtering, washing, drying, and taking out solid to obtain pigment red 254. It achieves simple process, more yield and high strength.
Description
Technical field
The present invention relates to be used for the production technique that DPP is the Pigment red 254 of high-grade pigment dyestuff.
Background technology
Pigment red 254 is that DPP is the raw materials for production of high-grade pigment dyestuff, and annual about 1500 tons of at present domestic market demand to Pigment red 254 mainly is a dependence on import, not only causes the production cost height, and does not have autonomy.
Summary of the invention
The object of the invention is to invent a kind of production method that can satisfy the Pigment red 254 of market demand.
Production method of the present invention is: add in sodium tert-amyl alcohol solution 6-chlorophenyl nitrile, stirring and dissolving, be cooled to 80 ℃ of mixed solutions that drip diisopropyl ester amber acid and tertiary amyl alcohol, drip the back and be incubated 2～5 hours down, distillation at 110～130 ℃, after collecting tertiary amyl alcohol, add entry and stir suction filtration, washing, oven dry, get solid, promptly get Pigment red 254.
The present invention has adopted the diisopropyl ester amber acid condensation, and production technique is controlled easily, and the product yield height can reach 93%, and product is bright-coloured, and the intensity height has not only been filled up domestic blank, and has satisfied market demand.
Above-mentioned sodium tert-amyl alcohol solution be 2: 1.5～1.7: 1 to the weight ratio of 6-chlorophenyl nitrile, diisopropyl ester amber acid, tertiary amyl alcohol.
Sodium tert-amyl alcohol solution is to use N by tertiary amyl alcohol and sodium under 95 ℃ of conditions
2Displace the H of generation
2, heat again to 100～105 ℃, be incubated stand-by after 8 hours.
During preparation sodium tert-amyl alcohol solution, the weight ratio of tertiary amyl alcohol and sodium is 10: 1.
Specific embodiment
One, prepares pure sodium solution
Get the raw materials ready: tertiary amyl alcohol 100kg, sodium 10kg
With above-mentioned mixing of materials, be heated to 95 ℃, stir the H2 that displaces generation with N2, heat again to 100～105 ℃, be incubated 8 hours, it is stand-by to finish.
Two, condensation reaction
Chemical equation
1, get the raw materials ready:
To 6-chlorophenyl nitrile 20kg
Diisopropyl ester amber acid 16kg
Tertiary amyl alcohol 10kg
2, operation steps:
Above-mentioned pure sodium solution is cooled to 40 ℃, adding is to 6-chlorophenyl nitrile, and the stirring heating dissolving is cooled to 80 ℃ and drips diisopropyl ester amber acid and tertiary amyl alcohol, temperature is controlled at 110～130 ℃, finish 130 ℃ of insulations 2～5 hours, protect and finish distillation, behind the collection tertiary amyl alcohol, add entry and stir suction filtration, wash three times, oven dry gets 24 kilograms of Pigment reds 254.Yield: 93%.
Pigment red 254 molecular structural formulas:
Claims (4)
1, the production method of Pigment red 254, it is characterized in that adding in sodium tert-amyl alcohol solution to 6-chlorophenyl nitrile, stirring and dissolving is cooled to 80 ℃ of mixed solutions that drip diisopropyl ester amber acid and tertiary amyl alcohol, drip the back and be incubated 2～5 hours down at 110～130 ℃, distillation behind the collection tertiary amyl alcohol, adds entry and stirs suction filtration, washing, solid is got in oven dry, promptly gets Pigment red 254.
2,, it is characterized in that above-mentioned sodium tert-amyl alcohol solution and be 2: 1.5～1.7: 1 the weight ratio of 6-chlorophenyl nitrile, diisopropyl ester amber acid, tertiary amyl alcohol according to the production method of the described Pigment red 254 of claim 1.
3,, it is characterized in that sodium tert-amyl alcohol solution is to use N by tertiary amyl alcohol and sodium under 95 ℃ of conditions according to the production method of claim 1 or 2 described Pigment reds 254
2Displace the H of generation
2, heat again to 100～105 ℃, be incubated stand-by after 8 hours.
4, according to the production method of the described Pigment red 254 of claim 3, the weight ratio that it is characterized in that tertiary amyl alcohol and sodium is 10: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510094325 CN1746227A (en) | 2005-09-08 | 2005-09-08 | Production of paint red 254 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510094325 CN1746227A (en) | 2005-09-08 | 2005-09-08 | Production of paint red 254 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1746227A true CN1746227A (en) | 2006-03-15 |
Family
ID=36165957
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510094325 Pending CN1746227A (en) | 2005-09-08 | 2005-09-08 | Production of paint red 254 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1746227A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831197A (en) * | 2010-05-17 | 2010-09-15 | 南通市争妍颜料化工有限公司 | Production process for pigment red 254 variety HL with high covering power |
| CN102001915A (en) * | 2010-10-19 | 2011-04-06 | 常州吉恩化工有限公司 | Manufacturing method of granular sodium tert-pentoxide |
| CN101624476B (en) * | 2009-08-10 | 2012-11-14 | 南通市争妍颜料化工有限公司 | Production process of pigment red HT |
| CN102964865A (en) * | 2012-11-23 | 2013-03-13 | 江苏双乐化工颜料有限公司 | Preparation method of pigment red 254 |
-
2005
- 2005-09-08 CN CN 200510094325 patent/CN1746227A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624476B (en) * | 2009-08-10 | 2012-11-14 | 南通市争妍颜料化工有限公司 | Production process of pigment red HT |
| CN101831197A (en) * | 2010-05-17 | 2010-09-15 | 南通市争妍颜料化工有限公司 | Production process for pigment red 254 variety HL with high covering power |
| CN102001915A (en) * | 2010-10-19 | 2011-04-06 | 常州吉恩化工有限公司 | Manufacturing method of granular sodium tert-pentoxide |
| CN102001915B (en) * | 2010-10-19 | 2013-11-06 | 常州吉恩化工有限公司 | Manufacturing method of granular sodium tert-pentoxide |
| CN102964865A (en) * | 2012-11-23 | 2013-03-13 | 江苏双乐化工颜料有限公司 | Preparation method of pigment red 254 |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |