CN106008258A - Testing method for optimal treatment conditions for 3GL (4-chloro-2-nitroaniline) diazotization solid residues - Google Patents
Testing method for optimal treatment conditions for 3GL (4-chloro-2-nitroaniline) diazotization solid residues Download PDFInfo
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- CN106008258A CN106008258A CN201610456123.5A CN201610456123A CN106008258A CN 106008258 A CN106008258 A CN 106008258A CN 201610456123 A CN201610456123 A CN 201610456123A CN 106008258 A CN106008258 A CN 106008258A
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- diazotising
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C245/00—Compounds containing chains of at least two nitrogen atoms with at least one nitrogen-to-nitrogen multiple bond
- C07C245/20—Diazonium compounds
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Abstract
The invention relates to a testing method for optimal treatment conditions for 3GL (4-chloro-2-nitroaniline) diazotization solid residues. According to the testing method, the optimal treatment conditions for the 3GL diazotization solid residues are determined by changing a washing temperature and the number of stirring and washing times through an orthogonal test. The testing method has the advantages as follows: the conditions that the optimal washing temperature is 40 DEG C and the number of stirring and washing times is one are determined with the testing method, 3GL contains the fewest impurities and the fewest prepeaks at the moment, the diazotization solid residues can be reduced to 0.5% or lower, the impurities and the prepeaks in 3GL can be reduced effectively, and the diazotization solid residues can be reduced effectively.
Description
Technical field
The present invention relates to the solid Slag treatment method of 3GL diazotising, particularly to the test method of the solid slag optimal treatment condition of a kind of 3GL diazotising.
Background technology
P-chloro-o-nitroaniline, has another name called red base 3GL, by 2,5-dichloronitrobenzene prepares through ammonia ammonolysis, crystallization, sucking filtration, is dissolved in ethanol, ether, acetic acid, is slightly soluble in ligroin, can be used for producing organic pigment and the dyestuff such as bright red color lake, light yellow 10G color lake as azoic dyes color base.And existing preparation technology, prepared 3GL, the shortcomings such as impurity is many, the solid slag having 5%-10% not after having leading peak, and diazotising etc..
Therefore, the processing method of the solid slag of a kind of 3GL diazotising of research and development is needed badly.
Summary of the invention
The technical problem to be solved in the present invention is to provide the test method of the solid slag optimal treatment condition of a kind of 3GL diazotising, optimal washing temperature and washing times is determined by this test method, and then can effectively reduce the impurity in 3GL and forward, also it is effectively reduced the solid slag after diazotising simultaneously.
For solving above-mentioned technical problem, the technical scheme is that the test method of the solid slag optimal treatment condition of a kind of 3GL diazotising, its innovative point is: described test method passes through orthogonal test, changes washing temperature and stirring washing times, determines the optimal treatment condition of the solid slag of 3GL diazotising.
Further, described washing temperature is the one in 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C or 80 DEG C.
Further, described washing times is the one in 1 time, 2 times, 3 times or 4 times.
It is an advantage of the current invention that: the test method of the solid slag optimal treatment condition of 3GL diazotising of the present invention, determining that optimal washing temperature is 40 DEG C by this test method is 1 time with washing times, now, in 3GL, impurity is minimum, forward is minimum, after diazotising, solid slag can be reduced to less than 0.5%, and then can effectively reduce the impurity in 3GL and forward, is also effectively reduced the solid slag after diazotising simultaneously.
Detailed description of the invention
The following examples can make professional and technical personnel that the present invention is more fully understood, but the most therefore limits the present invention among described scope of embodiments.
Embodiment
1
The processing method of the solid slag of the present embodiment 3GL diazotising, selecting 3GL impurity content is 0.41, forward is 0.29 to be washed by stirring, effectively go the removal of impurity, washing temperature is 20 DEG C, washes 1 time, and after process, in 3GL, impurity content is 0.38, forward is 0.27, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
2
The present embodiment, relative to embodiment 1, changes washing times, changes into for 1 time washing 2 times by washing, and after process, in 3GL, impurity content is 0.27, and forward is 0.13, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
3
The present embodiment, relative to embodiment 1, changes washing times, changes into for 1 time washing 3 times by washing, and after process, in 3GL, impurity content is 0.20, and forward is 0.11, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
4
The present embodiment, relative to embodiment 1, changes washing times, changes into for 1 time washing 4 times by washing, and after process, in 3GL, impurity content is 0.20, and forward is 0.10, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
5
The present embodiment, relative to embodiment 1, changes washing temperature, washing temperature changes into 30 DEG C, and after process, in 3GL, impurity content is 0.36, and forward is 0.25, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
6
The present embodiment, relative to embodiment 1, changes washing temperature, washing temperature changes into 40 DEG C, and after process, in 3GL, impurity content is 0.24, and forward is 0.12, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
7
The present embodiment, relative to embodiment 1, changes washing temperature, washing temperature changes into 50 DEG C, and after process, in 3GL, impurity content is 0.20, and forward is 0.11, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
8
The present embodiment, relative to embodiment 1, changes washing temperature, washing temperature changes into 60 DEG C, and after process, in 3GL, impurity content is 0.25, and forward is 0.15, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
9
The present embodiment, relative to embodiment 1, changes washing temperature, washing temperature changes into 70 DEG C, and after process, in 3GL, impurity content is 0.24, and forward is 0.12, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
10
The present embodiment, relative to embodiment 1, changes washing temperature, washing temperature changes into 80 DEG C, and after process, in 3GL, impurity content is 0.22, and forward is 0.13, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
11
The present embodiment, relative to embodiment 2, changes washing temperature, washing temperature changes into 30 DEG C, and after process, in 3GL, impurity content is 0.27, and forward is 0.13, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
12
The present embodiment, relative to embodiment 2, changes washing temperature, washing temperature changes into 40 DEG C, and after process, in 3GL, impurity content is 0.25, and forward is 0.13, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
13
The present embodiment, relative to embodiment 2, changes washing temperature, washing temperature changes into 50 DEG C, and after process, in 3GL, impurity content is 0.24, and forward is 0.11, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
14
The present embodiment, relative to embodiment 2, changes washing temperature, washing temperature changes into 60 DEG C, and after process, in 3GL, impurity content is 0.22, and forward is 0.12, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
15
The present embodiment, relative to embodiment 2, changes washing temperature, washing temperature changes into 70 DEG C, and after process, in 3GL, impurity content is 0.23, and forward is 0.11, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
16
The present embodiment, relative to embodiment 2, changes washing temperature, washing temperature changes into 80 DEG C, and after process, in 3GL, impurity content is 0.22, and forward is 0.11, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
17
The present embodiment, relative to embodiment 3, changes washing temperature, washing temperature changes into 30 DEG C, and after process, in 3GL, impurity content is 0.23, and forward is 0.12, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
18
The present embodiment, relative to embodiment 3, changes washing temperature, washing temperature changes into 40 DEG C, and after process, in 3GL, impurity content is 0.23, and forward is 0.11, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
19
The present embodiment, relative to embodiment 3, changes washing temperature, washing temperature changes into 50 DEG C, and after process, in 3GL, impurity content is 0.20, and forward is 0.09, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
20
The present embodiment, relative to embodiment 3, changes washing temperature, washing temperature changes into 60 DEG C, and after process, in 3GL, impurity content is 0.21, and forward is 0.10, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
21
The present embodiment, relative to embodiment 3, changes washing temperature, washing temperature changes into 70 DEG C, and after process, in 3GL, impurity content is 0.19, and forward is 0.09, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
22
The present embodiment, relative to embodiment 3, changes washing temperature, washing temperature changes into 80 DEG C, and after process, in 3GL, impurity content is 0.19, and forward is 0.09, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
23
The present embodiment, relative to embodiment 4, changes washing temperature, washing temperature changes into 30 DEG C, and after process, in 3GL, impurity content is 0.22, and forward is 0.11, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
24
The present embodiment, relative to embodiment 4, changes washing temperature, washing temperature changes into 40 DEG C, and after process, in 3GL, impurity content is 0.21, and forward is 0.11, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
25
The present embodiment, relative to embodiment 4, changes washing temperature, washing temperature changes into 50 DEG C, and after process, in 3GL, impurity content is 0.20, and forward is 0.11, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
26
The present embodiment, relative to embodiment 4, changes washing temperature, washing temperature changes into 60 DEG C, and after process, in 3GL, impurity content is 0.19, and forward is 0.10, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
27
The present embodiment, relative to embodiment 4, changes washing temperature, washing temperature changes into 70 DEG C, and after process, in 3GL, impurity content is 0.19, and forward is 0.08, and after diazotising, solid slag can be reduced to 0.5%.
Embodiment
28
The present embodiment, relative to embodiment 4, changes washing temperature, washing temperature changes into 80 DEG C, and after process, in 3GL, impurity content is 0.19, and forward is 0.08, and after diazotising, solid slag can be reduced to 0.5%.
By the contrast of each embodiment, when washing temperature is 40 DEG C and washing times is 1 time, treatment conditions are optimal.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and description; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within scope of the claimed invention.Claimed scope is defined by appending claims and equivalent thereof.
Claims (3)
1. the test method of the solid slag optimal treatment condition of 3GL diazotising, it is characterised in that: described test method passes through orthogonal test, changes washing temperature and stirring washing times, determines the optimal treatment condition of the solid slag of 3GL diazotising.
The test method of the solid slag optimal treatment condition of 3GL diazotising the most according to claim 1, it is characterised in that: described washing temperature is the one in 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C or 80 DEG C.
The test method of the solid slag optimal treatment condition of 3GL diazotising the most according to claim 1, it is characterised in that: described washing times is the one in 1 time, 2 times, 3 times or 4 times.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610456123.5A CN106008258A (en) | 2016-06-22 | 2016-06-22 | Testing method for optimal treatment conditions for 3GL (4-chloro-2-nitroaniline) diazotization solid residues |
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| CN201610456123.5A CN106008258A (en) | 2016-06-22 | 2016-06-22 | Testing method for optimal treatment conditions for 3GL (4-chloro-2-nitroaniline) diazotization solid residues |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7825257B1 (en) * | 2007-10-23 | 2010-11-02 | Bausch & Lomb Incorporated | Synthesis of benzotriazole monomer |
| CN102675126A (en) * | 2012-05-24 | 2012-09-19 | 江苏隆昌化工有限公司 | Production method of o-nitro parachloroaniline |
| CN103408456A (en) * | 2013-08-15 | 2013-11-27 | 江苏隆昌化工有限公司 | Clean halogenated aromatic nitroaniline diazotization technology |
-
2016
- 2016-06-22 CN CN201610456123.5A patent/CN106008258A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7825257B1 (en) * | 2007-10-23 | 2010-11-02 | Bausch & Lomb Incorporated | Synthesis of benzotriazole monomer |
| CN102675126A (en) * | 2012-05-24 | 2012-09-19 | 江苏隆昌化工有限公司 | Production method of o-nitro parachloroaniline |
| CN103408456A (en) * | 2013-08-15 | 2013-11-27 | 江苏隆昌化工有限公司 | Clean halogenated aromatic nitroaniline diazotization technology |
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