CN108485306A - A kind of synthetic method of aniline black byestuffs - Google Patents
A kind of synthetic method of aniline black byestuffs Download PDFInfo
- Publication number
- CN108485306A CN108485306A CN201810271690.2A CN201810271690A CN108485306A CN 108485306 A CN108485306 A CN 108485306A CN 201810271690 A CN201810271690 A CN 201810271690A CN 108485306 A CN108485306 A CN 108485306A
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- CN
- China
- Prior art keywords
- black
- aniline
- polyaniline
- solvent
- ferric trichloride
- Prior art date
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Classifications
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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
- C09B17/00—Azine dyes
- C09B17/02—Azine dyes of the benzene series
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0683—Polycondensates containing six-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0694—Polycondensates containing six-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only two nitrogen atoms in the ring, e.g. polyquinoxalines
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention discloses a kind of synthetic methods of aniline black byestuffs, including in acid condition, and through ferric trichloride and potassium ferrate the step of oxidation polymerization prepares intermediate polyaniline is occurred for aniline；Under the action of catalyst polyethylene glycol, by polyaniline and nitrobenzene occur condensation reaction prepare target product solvent it is black 7 the step of.The present invention uses method of fractional steps synthetic black 7, reduces the production cycle, reduces quantity of three wastes, reduces energy consumption；Meanwhile the potent oxidant potassium ferrate of green is introduced, aniline has obtained high purity polyaniline through ferric trichloride potassium ferrate co-oxidation, the dosage of ferric trichloride is greatly reduced, and reduces the content of iron ion in waste water, environmentally protective；Since under the action of polyethylene glycol, polyaniline and nitrobenzene are condensed to yield solvent black 7, and the black 7 coloured light form and aspect of solvent are partially blue, more meet the demand of client.
Description
Technical field
The present invention relates to a kind of synthetic methods of aniline black byestuffs, and in particular to a kind of synthetic method of solvent black 7 belongs to
The manufacturing technology field of chemical dyestuff.
Background technology
Nigrosine series dyes are most ancient one of dye species, and the current many countries in west still use and open largely
Open up relevant research work.With eliminating for plastics leather industrial expansion and cancinogenic dye, both at home and abroad to aniline black byestuffs
Demand sharply increasing.
Solvent black 7 is foremost one kind in aniline black byestuffs, also known as oil-soluble nigrosine, be in current black dyes most
Black, most blue product can be used as tune blue-black.Nigrosine is superior solvent resistant, acidproof, alkaline-resisting, fast light, heat-resisting, not soluble in water,
And it is not reacted with DOP.No matter it is single use.Or as toning purposes, it is all PU mill bases, leather colouring, coating, oil
The first choice of the high blue phase black colorant environment such as ink, coloring resin.
Black 7 wide market of solvent, but the solvent of domestic production at present black 7 is using aniline, hydrochloric acid, iron chloride, nitrobenzene
With the technique of iron one kettle way oxidative condensation, the partially red phase of coloured light, production cycle length, high energy consumption, wastewater flow rate are big.It is based on this back of the body
Scape, the present invention provides a kind of synthetic methods of new aniline black byestuffs, it is intended to solve the problems, such as present on current techniques.
Invention content
The object of the present invention is to provide a kind of synthetic method of aniline black byestuffs, the method reduces iron ion in waste water
Content, reduce the three wastes, reduce energy consumption, shorten the production cycle, improve product coloured light, it is made more to meet the need of client
It asks.
Realizing the technical solution of the object of the invention is：A kind of synthetic method of aniline black byestuffs, including：
(1) in acid condition, through ferric trichloride and potassium ferrate oxidation-polymerization is occurred into for aniline and prepares intermediate polyphenyl
The step of amine,
(2) under the action of catalyst polyethylene glycol, condensation reaction is occurred into for polyaniline and nitrobenzene and prepares target product
Solvent it is black 7 the step of,
Further, in step (1), the acid condition is the hydrochloric acid using concentration 30w%, and input amount is aniline
0.5~0.625 times of quality, input method are to be added dropwise, and at 40 DEG C or more, time for adding controls in 2h dropping temperature.
Further, in step (1), ferric trichloride input amount is 0.05~0.0625 times of aniline quality.
Further, in step (1), potassium ferrate input amount is 0.025~0.03 times of aniline quality.
Further, in step (1), oxidation-polymeric reaction temperature is 120~130 DEG C.
Further, in step (2), the input amount of nitrobenzene is 1.2~1.5 times of aniline quality.
Further, in step (2), the input amount of polyethylene glycol is 0.05~0.08 times of aniline quality.
Further, in step (2), the input amount of DMAC is 2~2.5 times of aniline quality.
Further, in step (2), setting-up point is maintained at 180~200 DEG C.
Further, in step (2), after condensation reaction, be down to 70 DEG C be added DMAC black to solvent 7 carry out separation carry
It is pure.
Compared with prior art, it is an advantage of the invention that：
(1) method of fractional steps synthetic black 7 is used, reduces the production cycle, reduces quantity of three wastes, reduce energy consumption.
(2) the potent oxidant potassium ferrate of green is introduced, aniline is obtained through ferric trichloride-potassium ferrate co-oxidation
The dosage of ferric trichloride is greatly reduced in high purity polyaniline, reduces the content of iron ion in waste water, environmentally protective.
(3) under the action of polyethylene glycol, polyaniline and nitrobenzene are condensed to yield solvent black 7, and the black 7 coloured light form and aspect of solvent are inclined
Indigo plant more meets the demand of client.
Specific implementation mode
Specific embodiment is will be given below, for the present invention is described further.
Embodiment 1
(1) oxidation-polymerisation：The potassium ferrate of the aniline of 80g, the ferric trichloride of 5g and 2g is put into the four of 500ml
In mouth flask, after stirring evenly, it is warming up to 40~50 DEG C of hydrochloric acid 50g for starting that a concentration of 30w% is slowly added dropwise, rate of addition control
System is in 2h or so.It is added dropwise, is warming up to 120~130 DEG C, and keep the temperature at such a temperature, wait for that bottle wall condenses droplet, stop protecting
Temperature.
(2) condensation reaction：The polyethylene glycol of the nitrobenzene of 96g and 4g are put into above-mentioned reaction system, stirred evenly subsequent
It is continuous to be warming up to 180~200 DEG C, after keeping the temperature 4h, 70 DEG C are down to, reaction system is added in the DMAC of 160g, is dropped naturally while stirring
Temperature is down to room temperature, filters, hot water washing, dries, obtains the finished product solvent black 7 of 64g, the black 7 coloured light form and aspect of solvent obtained are inclined
It is blue.
Embodiment 2
(1) oxidation-polymerisation：The potassium ferrate of the aniline of 80g, the ferric trichloride of 4g and 2.4g is put into 500ml's
In four-hole boiling flask, after stirring evenly, it is warming up to 40~50 DEG C of hydrochloric acid 50g for starting that a concentration of 30w% is slowly added dropwise, rate of addition
Control is in 2h or so.It is added dropwise, is warming up to 120~130 DEG C, and keep the temperature at such a temperature, wait for that bottle wall condenses droplet, stop protecting
Temperature.
(2) condensation reaction：The polyethylene glycol of the nitrobenzene of 96g and 4g are put into above-mentioned reaction system, stirred evenly subsequent
It is continuous to be warming up to 180~200 DEG C, after keeping the temperature 4h, 70 DEG C are down to, reaction system is added in the DMAC of 160g, is dropped naturally while stirring
Temperature is down to room temperature, filters, hot water washing, dries, obtains the finished product solvent black 7 of 62.7g, the black 7 coloured light form and aspect of solvent obtained are inclined
It is blue.
Embodiment 3
(1) oxidation-polymerisation：The potassium ferrate of the aniline of 80g, the ferric trichloride of 4g and 2.4g is put into 500ml's
In four-hole boiling flask, after stirring evenly, it is warming up to 40~50 DEG C of hydrochloric acid 40g for starting that a concentration of 30w% is slowly added dropwise, rate of addition
Control is in 2h or so.It is added dropwise, is warming up to 120~130 DEG C, and keep the temperature at such a temperature, wait for that bottle wall condenses droplet, stop protecting
Temperature.
(2) condensation reaction：The polyethylene glycol of the nitrobenzene of 120g and 4g are put into above-mentioned reaction system, stirred evenly subsequent
It is continuous to be warming up to 180~200 DEG C, after keeping the temperature 4h, 70 DEG C are down to, reaction system is added in the DMAC of 160g, is dropped naturally while stirring
Temperature is down to room temperature, filters, hot water washing, dries, obtains the finished product solvent black 7 of 62.1g, the black 7 coloured light form and aspect of solvent obtained are inclined
It is blue.
Embodiment 4
(1) oxidation-polymerisation：The potassium ferrate of the aniline of 80g, the ferric trichloride of 4g and 2.4g is put into 500ml's
In four-hole boiling flask, after stirring evenly, it is warming up to 40~50 DEG C of hydrochloric acid 40g for starting that a concentration of 30w% is slowly added dropwise, rate of addition
Control is in 2h or so.It is added dropwise, is warming up to 120~130 DEG C, and keep the temperature at such a temperature, wait for that bottle wall condenses droplet, stop protecting
Temperature.
(2) condensation reaction：The polyethylene glycol of the nitrobenzene of 120g and 6.4g are put into above-mentioned reaction system, after stirring evenly
180~200 DEG C are continuously heating to, after keeping the temperature 4h, is down to 70 DEG C, reaction system is added in the DMAC of 160g, it is natural while stirring
Room temperature is down in cooling, is filtered, hot water washing, is dried, obtains the finished product solvent black 7 of 64.2g, the black 7 coloured light form and aspect of solvent obtained
It is partially blue.
Embodiment 5
(1) oxidation-polymerisation：The potassium ferrate of the aniline of 80g, the ferric trichloride of 4g and 2.4g is put into 500ml's
In four-hole boiling flask, after stirring evenly, it is warming up to 40~50 DEG C of hydrochloric acid 40g for starting that a concentration of 30w% is slowly added dropwise, rate of addition
Control is in 2h or so.It is added dropwise, is warming up to 120~130 DEG C, and keep the temperature at such a temperature, wait for that bottle wall condenses droplet, stop protecting
Temperature.
(2) condensation reaction：The polyethylene glycol of the nitrobenzene of 120g and 6.4g are put into above-mentioned reaction system, after stirring evenly
180~200 DEG C are continuously heating to, after keeping the temperature 4h, is down to 70 DEG C, reaction system is added in the DMAC of 200g, it is natural while stirring
Room temperature is down in cooling, is filtered, hot water washing, is dried, obtains the finished product solvent black 7 of 61.5g, the black 7 coloured light form and aspect of solvent obtained
It is partially blue.
Embodiment described above is only described the preferred embodiment of the present invention, not to the present invention's
Range is set, and without departing from the spirit of the invention, those of ordinary skill in the art are to technical scheme of the present invention
The modification and improvement done should all be fallen into the protection domain of claims of the present invention determination.
Claims (10)
1. the synthetic method of aniline black byestuffs, which is characterized in that including：
(1) in acid condition, through ferric trichloride and potassium ferrate oxidation-polymerization is occurred into for aniline and prepares intermediate polyaniline
Step,
(2) under the action of catalyst polyethylene glycol, condensation reaction is occurred into for polyaniline and nitrobenzene and prepares target product solvent
Black 7 the step of,
2. the method as described in claim 1, which is characterized in that in step (1), the acid condition is by using concentration
The hydrochloric acid of 30w%, which is added dropwise in reaction system, to be realized, dripping quantity is 0.5~0.625 times of aniline quality, and dropping temperature is 40
DEG C or more, time for adding controls in 2h.
3. the method as described in claim 1, which is characterized in that in step (1), ferric trichloride input amount is aniline quality
0.05~0.0625 times.
4. the method as described in claim 1, which is characterized in that in step (1), potassium ferrate input amount is aniline quality
0.025~0.03 times.
5. the method as described in claim 1, which is characterized in that in step (1), oxidation-polymeric reaction temperature is 120~130
℃。
6. the method as described in claim 1, which is characterized in that in step (2), the input amount of nitrobenzene is aniline quality
1.2~1.5 times.
7. the method as described in claim 1, which is characterized in that in step (2), the input amount of polyethylene glycol is aniline quality
0.05~0.08 times.
8. the method as described in claim 1, which is characterized in that in step (2), the input amount of DMAC be aniline quality 2~
2.5 again.
9. the method as described in claim 1, which is characterized in that in step (2), setting-up point is maintained at 180~200
℃。
10. the method as described in claim 1, which is characterized in that in step (2), after condensation reaction, be down to 70 DEG C of additions
DMAC black to solvent 7 carries out separating-purifying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810271690.2A CN108485306A (en) | 2018-03-29 | 2018-03-29 | A kind of synthetic method of aniline black byestuffs |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810271690.2A CN108485306A (en) | 2018-03-29 | 2018-03-29 | A kind of synthetic method of aniline black byestuffs |
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| Publication Number | Publication Date |
|---|---|
| CN108485306A true CN108485306A (en) | 2018-09-04 |
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ID=63316896
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810271690.2A Pending CN108485306A (en) | 2018-03-29 | 2018-03-29 | A kind of synthetic method of aniline black byestuffs |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10245497A (en) * | 1997-02-28 | 1998-09-14 | Kozo Horiuchi | Black pigment |
| JP2000072974A (en) * | 1998-09-01 | 2000-03-07 | Kozo Horiuchi | Preparation of aniline black |
| CN1358802A (en) * | 1999-12-21 | 2002-07-17 | 罗姆和哈斯公司 | Black dye formula capable of dissolving in alcohol |
| WO2002094941A1 (en) * | 2000-01-14 | 2002-11-28 | Tokyo Shikizai Industry Co., Ltd. | Process for producing black pigment |
| CN101817791A (en) * | 2009-02-27 | 2010-09-01 | 严纪一 | Method for directly producing water soluble aniline black |
| CN101845235A (en) * | 2009-12-15 | 2010-09-29 | 西北农林科技大学 | Method for preparing aniline black in dye industry |
| CN103044962A (en) * | 2012-12-26 | 2013-04-17 | 辽宁恒星精细化工有限公司 | Aniline black pigment producing method |
| CN103896864A (en) * | 2014-04-23 | 2014-07-02 | 青岛双桃精细化工（集团）有限公司 | Preparation method of nigrosine |
-
2018
- 2018-03-29 CN CN201810271690.2A patent/CN108485306A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10245497A (en) * | 1997-02-28 | 1998-09-14 | Kozo Horiuchi | Black pigment |
| JP2000072974A (en) * | 1998-09-01 | 2000-03-07 | Kozo Horiuchi | Preparation of aniline black |
| CN1358802A (en) * | 1999-12-21 | 2002-07-17 | 罗姆和哈斯公司 | Black dye formula capable of dissolving in alcohol |
| WO2002094941A1 (en) * | 2000-01-14 | 2002-11-28 | Tokyo Shikizai Industry Co., Ltd. | Process for producing black pigment |
| CN101817791A (en) * | 2009-02-27 | 2010-09-01 | 严纪一 | Method for directly producing water soluble aniline black |
| CN101845235A (en) * | 2009-12-15 | 2010-09-29 | 西北农林科技大学 | Method for preparing aniline black in dye industry |
| CN103044962A (en) * | 2012-12-26 | 2013-04-17 | 辽宁恒星精细化工有限公司 | Aniline black pigment producing method |
| CN103896864A (en) * | 2014-04-23 | 2014-07-02 | 青岛双桃精细化工（集团）有限公司 | Preparation method of nigrosine |
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Application publication date: 20180904 |