CN1763013A - 8-amidoquinaldine production method - Google Patents
8-amidoquinaldine production method Download PDFInfo
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- CN1763013A CN1763013A CN 200510094326 CN200510094326A CN1763013A CN 1763013 A CN1763013 A CN 1763013A CN 200510094326 CN200510094326 CN 200510094326 CN 200510094326 A CN200510094326 A CN 200510094326A CN 1763013 A CN1763013 A CN 1763013A
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- amidoquinaldine
- production method
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- hydrogen
- 1mpa
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Abstract
The present invention relates to the synthesis of chemical material. The production process of 8-amino quinaldine includes the steps of: dispersing 8-nitro-2-methyl-quinoline in benzene solvent, pumping into hydrogenation reactor for displacement reaction under the action of Pd/C catalyst, replacement with nitrogen and hydrogen after finishing reaction, press filtering, recovering Pd/C catalyst, and cooling the filtrate to crystallization to obtain 8-amino quinaldine in high yield and high purity. The 8-amino quinaldine product is used in producing pigment yellow-138 with bright color and high strength in lower production cost.
Description
Technical field
The present invention relates to a kind of synthesis technique of industrial chemicals.
Background technology
The 8-amidoquinaldine is a kind of dyestuff intermediate that is applied to high-grade pigment dyestuff industry, because prior art adopts Sodium Sulphide or iron powder reducing to make, its production cost height, the three wastes are big, and of poor quality, industrial applicibility is little, causes domestic dependence on import, make that derived product pigment yellow 13 8 coloured light of producing are not bright-coloured, and the production cost height.
Summary of the invention
The object of the invention is to invent a kind of 8-amidoquinaldine production method of producing, do not have the three wastes, can producing bright pigment yellow 13 8 of being easy to.
The present invention is finished by following steps:
A. with 8-nitro-2-methyl-quinoline and equal-volume benzene kind solvent, add in the Scattered Kettle, stir into the homodisperse thing;
B. above-mentioned dispersion thing is pumped in the hydrogenation still;
C. add palladium carbon catalyst;
D. closed reactor carries out replacement(metathesis)reaction;
E. after question response finishes, use the 0.5MPa nitrogen replacement, emptying;
F. use 1MPa nitrogen, emptying for the second time;
G. use the 0.5MPa hydrogen exchange, for the third time emptying;
H. add 1MPa hydrogen again, the 1MPa 5 minutes of keep-uping pressure is warming up to 100 ℃ ± 5 ℃, opens reactor, stirs 30 minutes, feeds hydrogen; Hydrogenation temperature is controlled at 100～120 ℃, and hydrogenation finished in about 4 hours;
I. be cooled to 80 ℃, palladium carbon catalyst is reclaimed in press filtration;
J. the filtrate crystallisation by cooling is separated out finished product, i.e. the 8-amidoquinaldine
Pass through above-mentioned steps; can obtain yield height, 8-amidoquinaldine that purity is high; reaction process is easy to control; production process does not have the three wastes; environmental protection capital construction less investment; remarkable benefit, and can provide safeguard by derived product pigment yellow 13 8 bright in luster for producing, that intensity is high, and save the production cost of pigment yellow 13 8.
In order to guarantee safety in production, among the present invention, in step c, elder generation adds in the reactor after the palladium charcoal is scattered in water again.
Benzene kind solvent in step a can be dimethylbenzene or toluene.
The tool present embodiment
One, get the raw materials ready:
8-nitro-2-methyl-quinoline 99% 100KG
Solvent (dimethylbenzene or toluene) 1000KG
Palladium charcoal (Pa/c) 1.5KG
20 bottles of hydrogen
2 bottles of nitrogen
(pa/c) uses the 20KG water-dispersion with the palladium charcoal, and be standby.
Two, operation steps:
A. 8-nitro-2-methyl-quinoline, solvent are added in the Scattered Kettle, stir into the homodisperse thing.
B. the dispersion thing with step a pumps in the hydrogenation still.
C. add palladium charcoal water dispersant.
D. closed reactor carries out replacement(metathesis)reaction.
E. after the reaction of steps d finishes, use the 0.5MPA nitrogen purge for the first time, remove oxygen.
F. use for the second time the 1MPA nitrogen purge, remove oxygen.Add 0.5MPA hydrogen for the third time, nitrogen is removed in emptying.
G. add 1MPA hydrogen the 4th time, pressure is not leaked in pressurize 5 minutes, is warming up to 100 ℃ ± 5 ℃, opens reactor, stirs 30 minutes, feeds hydrogen; Hydrogenation temperature is controlled at 100～120 ℃, and hydrogenation finished in about 4 hours;
I. be cooled to 80 ℃, palladium carbon catalyst is reclaimed in press filtration;
J. the filtrate crystallisation by cooling is separated out about 80KG 8-amidoquinaldine, and recovery rate is 95～98%.
The structural formula of 8-amidoquinaldine is:
Above-mentioned chemical reaction process equation is:
Claims (3)
1, the production method of 8-amidoquinaldine is characterized in that being finished by following steps:
A. with 8-nitro-2-methyl-quinoline and equal-volume benzene kind solvent, add in the Scattered Kettle, stir into the homodisperse thing;
B. above-mentioned dispersion thing is pumped in the hydrogenation still;
C. add palladium carbon catalyst;
D. closed reactor carries out replacement(metathesis)reaction;
E. after question response finishes, use the 0.5MPa nitrogen replacement, emptying;
F. use 1MPa nitrogen, emptying for the second time;
G. use the 0.5MPa hydrogen exchange, for the third time emptying;
H. add 1MPa hydrogen again, the 1MPa 5 minutes of keep-uping pressure is warming up to 100 ℃ ± 5 ℃, opens reactor, stirs 30 minutes, feeds hydrogen; Hydrogenation temperature is controlled at 100～120 ℃, and hydrogenation finished in about 4 hours;
I. be cooled to 80 ℃, palladium carbon catalyst is reclaimed in press filtration;
J. the filtrate crystallisation by cooling is separated out finished product, i.e. the 8-amidoquinaldine.
2,, it is characterized in that in step c elder generation adds in the reactor after the palladium charcoal is scattered in water again according to the production method of the described 8-amidoquinaldine of claim 1.
3,, it is characterized in that benzene kind solvent is dimethylbenzene or toluene among the step a according to the production method of the described 8-amidoquinaldine of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510094326A CN100577647C (en) | 2005-09-08 | 2005-09-08 | 8-amidoquinaldine production method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510094326A CN100577647C (en) | 2005-09-08 | 2005-09-08 | 8-amidoquinaldine production method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1763013A true CN1763013A (en) | 2006-04-26 |
| CN100577647C CN100577647C (en) | 2010-01-06 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200510094326A Expired - Fee Related CN100577647C (en) | 2005-09-08 | 2005-09-08 | 8-amidoquinaldine production method |
Country Status (1)
| Country | Link |
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| CN (1) | CN100577647C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602723B (en) * | 2009-07-10 | 2011-06-08 | 湖南大学 | Preparation method of 2-methyl-8-aminoquinoline |
| WO2013098837A2 (en) | 2011-10-24 | 2013-07-04 | Keki Hormusji Gharda | A bis-quinaldine compound and a process for preparing the same |
| KR20140034963A (en) * | 2012-09-10 | 2014-03-21 | 엘지디스플레이 주식회사 | High transmissional yellow dye for lcd and synthetic method thereof |
-
2005
- 2005-09-08 CN CN200510094326A patent/CN100577647C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602723B (en) * | 2009-07-10 | 2011-06-08 | 湖南大学 | Preparation method of 2-methyl-8-aminoquinoline |
| WO2013098837A2 (en) | 2011-10-24 | 2013-07-04 | Keki Hormusji Gharda | A bis-quinaldine compound and a process for preparing the same |
| US9062000B2 (en) | 2011-10-24 | 2015-06-23 | Keki Hormusji Gharda | Bis-quinaldine compound and a process for preparing the same |
| KR20140034963A (en) * | 2012-09-10 | 2014-03-21 | 엘지디스플레이 주식회사 | High transmissional yellow dye for lcd and synthetic method thereof |
| CN103665919A (en) * | 2012-09-10 | 2014-03-26 | 乐金显示有限公司 | High transmissional yellow dye for LCD and synthetic method thereof |
| KR101988046B1 (en) * | 2012-09-10 | 2019-06-11 | 엘지디스플레이 주식회사 | High transmissional yellow dye for lcd and synthetic method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100577647C (en) | 2010-01-06 |
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