CN105836754B - A kind of kaolinic method for bleaching - Google Patents
A kind of kaolinic method for bleaching Download PDFInfo
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- CN105836754B CN105836754B CN201610397377.4A CN201610397377A CN105836754B CN 105836754 B CN105836754 B CN 105836754B CN 201610397377 A CN201610397377 A CN 201610397377A CN 105836754 B CN105836754 B CN 105836754B
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
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Abstract
The invention discloses a kind of kaolinic method for bleaching, comprise the following steps:A, kaolin ore slurry is placed in container, the mass fraction that 8~12mL is added into every 100mL ore pulps is 5%~10% hydrogenperoxide steam generator, the mass fraction for adding 5~10mL into every 100mL ore pulps again is 5%~10% 42 pyridine-azo resorcinol solution, at 15~30 DEG C, 30~40min is reacted;B, with the solid matter in organic solvent and the multiple extraction container of polyacrylamide solution, carry out separation of solid and liquid, gained solid matter produces the kaolin after bleaching.The beneficial effect of invention is:By staining impurity separation of metal ions completely, kaolin whiteness is high;In separation process, the use of sulfuric acid is reduced, therefore without needing to carry out neutralization step again, reduces production link, improves production efficiency;Produced without discarded object;4th, react at normal temperatures and pressures, technique is simple;5th, production cost is reduced.
Description
Technical field
The present invention relates to a kind of method for bleaching, especially a kind of kaolinic method for bleaching.
Background technology
Whiteness is the key technical indexes of kaolin product.Kaolin in nature contains staining impurity metallic element,
Such as Fe, Ti, V, Cr, Cu, Mn.Whiteness does not reach the requirement of product, it is necessary to carry out brightening processing.Industrially usually use ore pulp
Brightened through magnetic separation, then higher whiteness is reached by chemical bleaching.Chemical bleaching is that sulfuric acid, sodium hydrosulfite etc. are added in kaolin
Chemical reagent, which separates kaolinic ferric iron back for ferrous iron, reaches the purpose brightened.Because reaction is in acid medium
Carry out, the harmful ions such as a large amount of sulfuric acid and ferrous ion can be remained in the ore pulp after bleaching, it is necessary to neutralize, except iron could be sharp again
With.Lime solution, aluminium polychloride are added i.e. in ore pulp, by the Fe in waste water2+Separated with the precipitation forms of Fe (OH) 2,
The clearance of iron about 98%.Clearance is relatively low on this condition for other staining impurity metal ions.And complex technical process, acid
Service efficiency it is low.
Therefore, a kind of staining impurity metal ion that can be efficiently separated in ore pulp, additionally it is possible to reduce the utilization rate of acid
Kaolinic method for bleaching turns into the key solved the problems, such as.
The content of the invention
As the result of various extensive and careful research and experiment, present inventors have found that:By successively
In ore pulp add oxidant and 4-2- pyridine-azo resorcinols formation complex ion, again with organic solvent extract complex ion, so
After add polyacrylamide, iron-free kaolin can be obtained.
One object of the present invention provides a kind of kaolinic method for bleaching, can not only efficiently separate the dyeing in ore pulp
Foreign metal ion, additionally it is possible to reduce the utilization rate of acid.
To achieve the above object, the present invention provides a kind of kaolinic method for bleaching, comprises the following steps:
A, kaolin ore slurry is placed in container, added into every 100mL ore pulps 8~12mL mass fraction for 5%~
10% hydrogenperoxide steam generator, then it is 5%~10% 4-2- pyrroles to add 5~10mL mass fraction into every 100mL ore pulps
Pyridine azo resorcinol solution, at 15~30 DEG C, reacts 30~40min;
B, with the solid matter in organic solvent and the multiple extraction container of polyacrylamide solution, carry out separation of solid and liquid, institute
Obtain solid matter and produce the kaolin after bleaching.
Preferably, the mass fraction of hydrogenperoxide steam generator described in step a is 8%.
Preferably, the mass fraction of 4-2- pyridine-azo resorcinols solution described in step a is 8%.
Preferably, in step a reaction temperature be 25 DEG C at, the reaction time is 35min.
Preferably, organic solvent described in step b is any one in chloroform, carbon tetrachloride or petroleum ether.
Preferably, organic solvent described in step b is chloroform.
Preferably, the mass fraction of polyacrylamide solution described in step b is 1~2%.
Preferably, extracting process is in step b:Added into every 100mL ore pulps 40~60mL organic solvents and 10~
15mL mass fractions are 1~2% polyacrylamide solution, stir 5~10min, then stand after 10~20min, stratification
Separate solid matter.
Preferably, repeatedly extraction is three times described in step b.
Preferably, it will be obtained after the water layer of the supernatant obtained in step b after separation of solid and liquid and organic layer separation
Organic layer, at 85-90 DEG C, is stirred continuously, and sodium hydroxide solution is constantly added dropwise into organic layer, until heavy there is no bronzing
Form sediment and generate, carry out again after separation of solid and liquid, gained liquid is 4-2- pyridine-azo resorcinol solution.
The beneficial effects of the invention are as follows:1st, by staining impurity separation of metal ions completely, kaolin whiteness is high;2nd, in separation
During, the use of sulfuric acid is reduced, therefore without needing to carry out neutralization step again, reduce production link, improve production efficiency;
3rd, produced without discarded object;4th, react at normal temperatures and pressures, technique is simple;5th, production cost is reduced.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, to make those skilled in the art's reference say
Bright book word can be implemented according to this.
Embodiment 1
A, 100mL ore pulp (ion for including Fe, Ti, V, Cr, Cu and/or Mn element in ore pulp) is placed in the first appearance
In device, the mass fraction for adding 10mL is 8% hydrogenperoxide steam generator, and the mass fraction for adding 8mL is 8% 4-2- pyridines
Azo resorcinol solution, is stirred continuously, at 25 DEG C, reacts 35min.Following chemical reaction occurs by taking iron ion as an example:
2Fe2++H2O2=2Fe3++2OH-
PAR+Fe3+=[PAR-Fe (III)]3+
B, the material in the first container is transferred in second container, stop valve is provided with the bottom of second container.Again to
It is 1.5% polyacrylamide solution that 50mL chloroforms and 12mL mass fractions are added in ore pulp in second container, stirs 8min,
Stand again after 15min, stratification, the solid matter that lower floor deposits is released by stop valve;Solid matter is placed in bottom again
In the 3rd container of the portion provided with stop valve, then add into the 3rd container 50mL chloroforms and 12mL mass fractions for 1.5% it is poly-
Acrylamide solution, stirs 8min, then stands after 15min, stratification, and the solids that lower floor deposits is released by stop valve
Matter, then by solid matter be placed in bottom provided with stop valve the 4th container in, then in the 4th container add 50mL chloroforms and
12mL mass fractions are 1.5% polyacrylamide solution, stir 8min, then are stood after 15min, stratification, pass through cut-off
Valve releases the solid matter of lower floor's deposition, and the sediment that solid matter is obtained after press filtration is the kaolin after bleaching.
C, will the water layer for the supernatant that obtained in step b after separation of solid and liquid and organic layer separation after obtain organic layer,
At 87 DEG C, it is stirred continuously, sodium hydroxide solution is constantly added dropwise into organic layer, until there is no reddish-brown precipitation generation, mistake
After filter, gained liquid is 4-2- pyridine-azo resorcinol solution.Embodiment 2
A, 100mL ore pulp (ion for including Fe, Ti, V, Cr, Cu and/or Mn element in ore pulp) is placed in the first appearance
In device, the mass fraction for adding 8mL is 10% hydrogenperoxide steam generator, and the mass fraction for adding 5mL is 10% 4-2- pyrroles
Pyridine azo resorcinol solution, is stirred continuously, at 15 DEG C, reacts 40min.
B, the material in the first container is transferred in second container, stop valve is provided with the bottom of second container.Again to
It is 2% polyacrylamide solution, stirring that 40mL carbon tetrachloride and 15mL mass fractions are added in ore pulp in second container
5min, then stand after 20min, stratification, the solid matter that lower floor deposits is released by stop valve;Solid matter is put again
Addition 40mL carbon tetrachloride and 15mL mass fractions are in threeth container of the bottom provided with stop valve, then into the 3rd container
2% polyacrylamide solution, stirs 5min, then stands after 20min, stratification, releases what lower floor deposited by stop valve
Solid matter, is then placed in the 4th container of the bottom provided with stop valve by solid matter, then 40mL tetra- is added in the 4th container
Chlorination carbon and the polyacrylamide solution that 15mL mass fractions are 2%, stir 5min, then stand after 20min, stratification, lead to
The solid matter that stop valve releases lower floor's deposition is crossed, the sediment that solid matter is obtained after press filtration is the kaolinite after bleaching
Soil.
C, will the water layer for the supernatant that obtained in step b after separation of solid and liquid and organic layer separation after obtain organic layer,
At 85 DEG C, it is stirred continuously, sodium hydroxide solution is constantly added dropwise into organic layer, until there is no reddish-brown precipitation generation, mistake
After filter, gained liquid is 4-2- pyridine-azo resorcinol solution.Embodiment 3
A, 100mL ore pulp (ion for including Fe, Ti, V, Cr, Cu and/or Mn element in ore pulp) is placed in the first appearance
In device, the mass fraction for adding 12mL is 5% hydrogenperoxide steam generator, and the mass fraction for adding 10mL is 5% 4-2- pyrroles
Pyridine azo resorcinol solution, is stirred continuously, at 30 DEG C, reacts 30min.
B, the material in the first container is transferred in second container, stop valve is provided with the bottom of second container.Again to
It is 1% polyacrylamide solution, stirring that 60mL petroleum ethers and 10mL mass fractions are added in ore pulp in second container
10min, then stand after 10min, stratification, the solid matter that lower floor deposits is released by stop valve;Again by solid matter
It is placed in the 3rd container of the bottom provided with stop valve, then addition 60mL petroleum ethers and 10mL mass fractions are into the 3rd container
1% polyacrylamide solution, stirs 10min, then stands after 10min, stratification, releases what lower floor deposited by stop valve
Solid matter, is then placed in the 4th container of the bottom provided with stop valve by solid matter, then 60mL stones are added in the 4th container
Oily ether and 10mL mass fraction is 1% polyacrylamide solution, stirs 10min, then is stood after 10min, stratification, is passed through
Stop valve releases the solid matter of lower floor's deposition, and the sediment that solid matter is obtained after press filtration is the kaolin after bleaching.
C, will the water layer for the supernatant that obtained in step b after separation of solid and liquid and organic layer separation after obtain organic layer,
At 90 DEG C, it is stirred continuously, sodium hydroxide solution is constantly added dropwise into organic layer, until there is no reddish-brown precipitation generation, mistake
After filter, gained liquid is 4-2- pyridine-azo resorcinol solution.Embodiment 4
A, 100mL ore pulp (ion for including Fe, Ti, V, Cr, Cu and/or Mn element in ore pulp) is placed in the first appearance
In device, the mass fraction for adding 9mL is 9% hydrogenperoxide steam generator, and the mass fraction for adding 6mL is 6% 4-2- pyridines
Azo resorcinol solution, is stirred continuously, at 18 DEG C, reacts 38min.
B, the material in the first container is transferred in second container, stop valve is provided with the bottom of second container.Again to
It is 1.8% polyacrylamide solution that 45mL chloroforms and 14mL mass fractions are added in ore pulp in second container, stirs 6min,
Stand again after 18min, stratification, the solid matter that lower floor deposits is released by stop valve;Solid matter is placed in bottom again
In the 3rd container of the portion provided with stop valve, then add into the 3rd container 45mL chloroforms and 14mL mass fractions for 1.8% it is poly-
Acrylamide solution, stirs 6min, then stands after 18min, stratification, and the solids that lower floor deposits is released by stop valve
Matter, then by solid matter be placed in bottom provided with stop valve the 4th container in, then in the 4th container add 45mL chloroforms and
14mL mass fractions are 1.8% polyacrylamide solution, stir 6min, then are stood after 18min, stratification, pass through cut-off
Valve releases the solid matter of lower floor's deposition, and the sediment that solid matter is obtained after press filtration is the kaolin after bleaching.
C, will the water layer for the supernatant that obtained in step b after separation of solid and liquid and organic layer separation after obtain organic layer,
At 86 DEG C, it is stirred continuously, sodium hydroxide solution is constantly added dropwise into organic layer, until there is no reddish-brown precipitation generation, mistake
After filter, gained liquid is 4-2- pyridine-azo resorcinol solution.Embodiment 5
A, 100mL ore pulp (ion for including Fe, Ti, V, Cr, Cu and/or Mn element in ore pulp) is placed in the first appearance
In device, the mass fraction for adding 11mL is 6% hydrogenperoxide steam generator, and the mass fraction for adding 9mL is 8% 4-2- pyridines
Azo resorcinol solution, is stirred continuously, at 36 DEG C, reacts 32min.
B, the material in the first container is transferred in second container, stop valve is provided with the bottom of second container.Again to
It is 1.2% polyacrylamide solution, stirring that 42mL carbon tetrachloride and 11mL mass fractions are added in ore pulp in second container
9min, then stand after 13min, stratification, the solid matter that lower floor deposits is released by stop valve;Solid matter is put again
Addition 42mL carbon tetrachloride and 11mL mass fractions are in threeth container of the bottom provided with stop valve, then into the 3rd container
1.2% polyacrylamide solution, stirs 9min, then stands after 13min, stratification, and releasing lower floor by stop valve deposits
Solid matter, then solid matter is placed in the 4th container of the bottom provided with stop valve, then in the 4th container add 42mL
Carbon tetrachloride and the polyacrylamide solution that 11mL mass fractions are 1.2%, stir 9min, then stand 13min, stratification
Afterwards, the solid matter that lower floor deposits is released by stop valve, after the sediment that solid matter is obtained after press filtration is bleaching
Kaolin.
C, will the water layer for the supernatant that obtained in step b after separation of solid and liquid and organic layer separation after obtain organic layer,
At 88 DEG C, it is stirred continuously, sodium hydroxide solution is constantly added dropwise into organic layer, until there is no reddish-brown precipitation generation, mistake
After filter, gained liquid is 4-2- pyridine-azo resorcinol solution.Comparative example 1
A, 100mL ore pulp (ion for including Fe, Ti, V, Cr, Cu and/or Mn element in ore pulp) is placed in the first appearance
In device, the mass fraction for adding 6mL is 4% hydrogenperoxide steam generator, and the mass fraction for adding 12mL is 11% 4-2- pyrroles
Pyridine azo resorcinol solution, is stirred continuously, at 35 DEG C, reacts 25min.
B, the material in the first container is transferred in second container, stop valve is provided with the bottom of second container.Again to
It is 2.5% polyacrylamide solution that 35mL chloroforms and 18mL mass fractions are added in ore pulp in second container, stirs 4min,
Stand again after 25min, stratification, the solid matter that lower floor deposits is released by stop valve;Solid matter is placed in bottom again
In the 3rd container of the portion provided with stop valve, then add into the 3rd container 35mL chloroforms and 18mL mass fractions for 2.5% it is poly-
Acrylamide solution, stirs 4min, then stands after 25min, stratification, and the solids that lower floor deposits is released by stop valve
Matter, then by solid matter be placed in bottom provided with stop valve the 4th container in, then in the 4th container add 35mL chloroforms and
18mL mass fractions are 2.5% polyacrylamide solution, stir 4min, then are stood after 25min, stratification, pass through cut-off
Valve releases the solid matter of lower floor's deposition, and the sediment that solid matter is obtained after press filtration is the kaolin after bleaching.
C, will the water layer for the supernatant that obtained in step b after separation of solid and liquid and organic layer separation after obtain organic layer,
At 92 DEG C, it is stirred continuously, sodium hydroxide solution is constantly added dropwise into organic layer, until there is no reddish-brown precipitation generation, mistake
After filter, gained liquid is 4-2- pyridine-azo resorcinol solution.Comparative example 2
A, 100mL ore pulp (ion for including Fe, Ti, V, Cr, Cu and/or Mn element in ore pulp) is placed in the first appearance
In device, the mass fraction for adding 13mL is 12% hydrogenperoxide steam generator, and the mass fraction for adding 4mL is 4% 4-2- pyrroles
Pyridine azo resorcinol solution, is stirred continuously, at 12 DEG C, reacts 45min.
B, the material in the first container is transferred in second container, stop valve is provided with the bottom of second container.Again to
It is 0.5% polyacrylamide solution that 65mL chloroforms and 8mL mass fractions are added in ore pulp in second container, stirs 15min,
Stand again after 8min, stratification, the solid matter that lower floor deposits is released by stop valve;Solid matter is placed in bottom again
In the 3rd container provided with stop valve, then it is 0.5% polypropylene to add 65mL chloroforms and 8mL mass fractions into the 3rd container
Amide solution, stirs 15min, then stands after 8min, stratification, releases the solid matter that lower floor deposits by stop valve, so
Solid matter is placed in the 4th container of the bottom provided with stop valve afterwards, then 65mL chloroforms and 8mL mass are added in the 4th container
Fraction is 0.5% polyacrylamide solution, stirs 15min, then is stood after 8min, stratification, is released down by stop valve
The solid matter of layer deposition, the sediment that solid matter is obtained after press filtration is the kaolin after bleaching.
C, will the water layer for the supernatant that obtained in step b after separation of solid and liquid and organic layer separation after obtain organic layer,
At 82 DEG C, it is stirred continuously, sodium hydroxide solution is constantly added dropwise into organic layer, until there is no reddish-brown precipitation generation, mistake
After filter, gained liquid is 4-2- pyridine-azo resorcinol solution.
Test and contained by the foreign metal ion in the kaolin after the bleaching of embodiment 1-5 and comparative example 1-2 preparations respectively
Amount and kaolinic yield, acquired results are shown in Table one.
Table one
Project | Kaolinic yield % | Foreign metal ion content % in kaolin |
Embodiment 1 | 91.8 | 0.00042 |
Embodiment 2 | 90.5 | 0.00048 |
Embodiment 3 | 91.3 | 0.00049 |
Embodiment 4 | 91.6 | 0.00043 |
Embodiment 5 | 91.3 | 0.00046 |
Comparative example 1 | 83.6 | 0.00098 |
Comparative example 2 | 82.5 | 0.00112 |
Data analysis
First, influence of the hydrogen peroxide addition to separation staining impurity metal ion (in terms of iron content)
100mL ore pulp (in terms of iron content 0.68%) is placed in the first container, be separately added into 5mL, 8mL, 10mL,
12mL mass fraction is 8% hydrogenperoxide steam generator, and the mass fraction for adding 8mL is 8% 4-2- pyridylazo isophthalic
Two phenol solutions, are stirred continuously, at 25 DEG C, react 35min.Again with poly- third that 50mL chloroforms and 12mL mass fractions are 1.5%
The solid matter of acrylamide solution in triplicate in extraction container, carries out separation of solid and liquid, after gained solid matter is bleached
Kaolin.The content of iron in kaolin after test gained is bleached respectively again.Acquired results are shown in Table two
Table two
The addition mL of 8% hydrogenperoxide steam generator | Iron content in kaolin, ppm |
5 | 1225 |
8 | 975 |
10 | 237 |
12 | 125 |
8~12mL mass fractions are added in table two, the ore pulp per 100mL to be advisable for 8% hydrogenperoxide steam generator.
2nd, influence of the 4-2- pyridine-azo resorcinols addition to separation staining impurity metal ion (in terms of iron content)
100mL ore pulp (in terms of iron content 0.68%) is placed in the first container, being separately added into 10mL, mass fraction is
8% hydrogenperoxide steam generator, then be separately added between the 4-2- pyridylazos that 5mL, 8mL, 10mL, 12mL mass fraction are 8%
Resorcinol solution, is stirred continuously, at 25 DEG C, reacts 35min.Again with 50mL chloroforms and 12mL mass fractions for 1.5% it is poly-
The solid matter of acrylamide solution in triplicate in extraction container, carries out separation of solid and liquid, after gained solid matter is bleached
Kaolin.The content of iron in kaolin after test gained is bleached respectively again.Acquired results are shown in Table three
Table three
Mass fraction is the addition mL of 8% 4-2- pyridine-azo resorcinol solution | Iron content in kaolin, ppm |
5 | 1325 |
8 | 1025 |
10 | 456 |
12 | 248 |
8~12mL mass fractions are added in table three, the ore pulp per 100mL to be advisable for 8% hydrogenperoxide steam generator.
I.e. when the amount ratio of 4-2- pyridine-azo resorcinols and the material of iron is 1:1, best results when 2-3% is measured.
3rd, influence of the polyacrylamide addition to separation staining impurity metal ion (in terms of iron content)
100mL ore pulp (in terms of iron content 0.68%) is placed in the first container, being separately added into 10mL, mass fraction is
8% hydrogenperoxide steam generator, then it is 8% 4-2- pyridine-azo resorcinol solution to be separately added into 8mL mass fraction, constantly
Stirring, at 25 DEG C, reacts 35min.Again with the polyacrylamide solution that 8mL, 10mL, 12mL, 15mL mass fraction are 1.5%
And the solid matter of 50mL chloroforms in triplicate in extraction container, separation of solid and liquid is carried out, after gained solid matter is bleached
Kaolin.The content of iron in kaolin after test gained is bleached respectively again.Acquired results are shown in Table four
Table four
The hydrogenperoxide steam generator that 10~15mL mass fractions are 1.5% is added in table four, the ore pulp per 100mL is
Preferably.
A kind of kaolinic method for bleaching of the present invention, complete by staining impurity separation of metal ions as described above, kaolin
Whiteness is high;In separation process, the use of sulfuric acid is reduced, therefore without needing to carry out neutralization step again, reduces production link, carries
High production efficiency;Produced without discarded object;React at normal temperatures and pressures, technique is simple;Reduce production cost.
Although embodiment of the present invention is disclosed as above, it is not restricted in bright book and embodiment listed fortune
With it can be applied to various suitable the field of the invention completely, for those skilled in the art, can be easily real
Now other modification, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited to
Specific details.
Claims (10)
1. a kind of kaolinic method for bleaching, it is characterised in that comprise the following steps:
A, kaolin ore slurry is placed in container, the mass fraction that 8~12mL is added into every 100mL ore pulps is 5%~10%
Hydrogenperoxide steam generator, then to add into every 100mL ore pulps 5~10mL mass fraction even for 5%~10% 4-2- pyridines
Nitrogen resorcinol solution, at 15~30 DEG C, reacts 30~40min;
B, with the solid matter in organic solvent and the multiple extraction container of polyacrylamide solution, carry out separation of solid and liquid, gained is solid
Body material is the kaolin after bleaching.
2. kaolinic method for bleaching as claimed in claim 1, it is characterised in that:Hydrogenperoxide steam generator described in step a
Mass fraction is 8%.
3. kaolinic method for bleaching as claimed in claim 2, it is characterised in that:Described in step a between 4-2- pyridylazos
The mass fraction of resorcinol solution is 8%.
4. kaolinic method for bleaching as claimed in claim 1 or 2, it is characterised in that:Reaction temperature is 25 DEG C in step a
Under, the reaction time is 35min.
5. kaolinic method for bleaching as claimed in claim 1 or 2, it is characterised in that:Organic solvent described in step b is chlorine
Any one in imitative, carbon tetrachloride or petroleum ether.
6. kaolinic method for bleaching as claimed in claim 5, it is characterised in that:Organic solvent described in step b is chloroform.
7. kaolinic method for bleaching as claimed in claim 1, it is characterised in that:Polyacrylamide solution described in step b
Mass fraction be 1~2%.
8. kaolinic method for bleaching as claimed in claim 7, it is characterised in that extracting process is in step b:To every
It is 1~2% polyacrylamide solution that 40~60mL organic solvents and 10~15mL mass fractions are added in 100mL ore pulps, is stirred
Mix 5~10min, then separate solid matter after standing 10~20min, stratification.
9. kaolinic method for bleaching as claimed in claim 1, it is characterised in that:Repeatedly extraction is three times described in step b.
10. kaolinic method for bleaching as claimed in claim 1, it is characterised in that:It will be obtained in step b after separation of solid and liquid
Supernatant liquor water layer and organic layer separation after obtain organic layer, at 85-90 DEG C, be stirred continuously, into organic layer constantly
Sodium hydroxide solution is added dropwise, until there is no reddish-brown precipitation generation, carrying out again after separation of solid and liquid, gained liquid is 4-2-
Pyridine-azo resorcinol solution.
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