CN108795087A - A kind of preparation method of C.I. paratoneres 2 - Google Patents
A kind of preparation method of C.I. paratoneres 2 Download PDFInfo
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- CN108795087A CN108795087A CN201810489126.8A CN201810489126A CN108795087A CN 108795087 A CN108795087 A CN 108795087A CN 201810489126 A CN201810489126 A CN 201810489126A CN 108795087 A CN108795087 A CN 108795087A
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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
- C09B29/00—Monoazo dyes prepared by diazotising and coupling
- C09B29/10—Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group
- C09B29/103—Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group of the naphthalene series
- C09B29/106—Hydroxy carboxylic acids of the naphthalene series
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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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/006—Preparation of organic pigments
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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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0079—Azoic dyestuff preparations
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- Chemical Kinetics & Catalysis (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a kind of preparation methods of C.I paratoneres 2, include the following steps：A, the preparation of the first diazonium salt solution；2, the preparation of the second diazonium salt solution；3, the preparation of Coupling Solution；4, coupling reaction.The present invention efficiently solves the content overrun issues of the banned substance Polychlorinated biphenyls contained by pigment, and because increasing the second diazol, suitable surfactant is selected, the technique of use is advanced so that reacts more complete, manufactured product purity higher, glossiness, mobility and water resistance are more preferable, environmental pollution is extremely small in terms of blowdown, and the made pigment of the invention can be widely used in food packaging article coloring, it can also be used to fabric printing and pigment coloration.
Description
Technical field
The present invention relates to a kind of preparation methods of C.I. paratoneres 2, belong to the production field of pigment.
Background technology
C.I paratoneres 2 are a kind of organic pigments of classics, and C.I paratoneres 2 provide neutral red color tone, and chemical constitution belongs to
Monoazo pigment, tinctorial strength is than general monoazo pigment higher.By 2.5- dichloroanilines after diazo-reaction with azoic coupling component AS
Aqueous slkali coupling reaction, using the pigment that is prepared of coupling post-processing, due to having added diazol and table in production process
Face activating agent, and technique is relatively advanced so that and manufactured pigment water resistance reaches 5 grades, and glossiness is good, good fluidity, product
It is detected through external professional authority mechanism, most important quality environmental protection index Polychlorinated biphenyls content meets European Union requirements.It is mainly used for
Aqueous food packing material colours and fabric printing.
The popular response of C.I paratoneres 2 is the alkali soluble after diazo-reaction with azoic coupling component AS by 2.5- dichloroanilines at present
Liquid coupling reaction, directly heats up, and since 2.5- dichloroaniline material purities are not high, and easily lumps very much, it is difficult to react completely；
Diazol reaction process is simple, again because without selecting suitable surfactant, coupling reaction technique in pigmentation reaction
Also very backward, cause the coupling reaction product uniformity poor, final pigment gloss degree is poor, poor water resistance, and production process is again right
Environment causes seriously to pollute, more than ten times of Polychlorinated biphenyls substance index exceeding standard.
Invention content
The object of the present invention is to provide a kind of preparation methods of C.I. paratoneres 2.The present invention can effectively improve face
Glossiness, mobility and the water resistance of material, and the content that the present invention solves the banned substance Polychlorinated biphenyls contained by pigment surpasses
Limit problem, environmental pollution is extremely small in terms of blowdown, has the advantages that environmental protection.
In order to solve the above technical problems, technical solution provided by the invention is as follows：A kind of preparation side of C.I. paratoneres 2
Method, this method specifically include following steps；
A, the preparation of the first diazonium salt solution, includes the following steps by weight；
In diazol reaction kettle, 50-100 parts of water is added, 30-40 portions of 2.5- dichloroanilines are added while stirring, then
The hydrochloric acid that 70-80 parts of concentration (concentration of this patent middle finger is mass percent concentration) are 20-40% is added, stirring 4-16 is small
When, ice water is added and adjusts temperature to -5-5 DEG C；13-16 parts of sodium nitrites are dissolved in 40-50 parts of water, reaction kettle is then added to
In；Stirring 1-2 hour, it (is specifically by the solution drop after stirring 1-2 hours in potassium iodide that determining, which has excessive nitrite ion,
When on starch paper, the blue chromosphere instantaneously occurred is to determine the proof of excessive nitrite ion)；It is added 0.5-1 parts
Sulfamic acid solution stirs 5-10 minutes, removes excessive nitrite ion；0.5-1 parts of activated carbon is added, stirs 15-25
Minute, filtering adjusts volume to 1000-1200 liters with ice cube and water, and temperature is less than -3 DEG C, and it is molten to obtain the first diazol
Liquid；
B, the preparation of the second diazonium salt solution, includes the following steps by weight：
In another diazol reaction kettle, 50-100 part water are added, the toast for being added 5-10 part while stirring is sour, 2B is sour or
4B acid, adds the hydrochloric acid of 5-10 parts of a concentration of 20-40%, adjusts temperature to -3-3 DEG C with ice water, stirs 30-40 minutes；It will
1-2 parts of sodium nitrites are dissolved in 10-15 parts of water, are then added in reaction kettle；Stirring 60-90 minutes, determination have excessive Asia
Nitrate ion, control temperature obtain the second diazonium salt solution in -2-2 degree；
C, the preparation of Coupling Solution
In conjugates dissolution kettle, 200-400 parts of water and 40-60 parts of azoic coupling component AS are added, stirring is slurried for 15-20 minutes；Add
Enter NaOH of 40-60 parts of the concentration 25%, be heated to 60-70 degree, azoic coupling component AS is completely dissolved；Water cooling on the rocks to 10-20 degree,
Volume is adjusted to 600-700 parts, the second diazonium salt solution is added, is uniformly mixing to obtain Coupling Solution；
D, coupling reaction：
In coupling reaction kettle, be added 200-400 parts of water, 12-18 parts of glacial acetic acid, 10-15 parts of a concentration of 30-40% it is dense
Hydrochloric acid and 0.4-1.0 parts of dodecyl sodium sulfates or surfactant, stirring and dissolving；After dissolving, accelerates mixing speed, use 40-
Pour into Coupling Solution within 45 minutes；It is heated to 45-50 DEG C, is added 5-10 part calcium carbonate, stirring 5-20 minutes, by the of wherein 70%
One diazonium salt solution is added in 35-60 minutes under liquid level, and determines that no excessive diazol (specifically takes solution
It drips on filter paper, red or purple colour band does not occur with H acid solution inspections in its profit circle edge side, indicate without excessive
Diazol)；5-10 parts of calcium carbonate are added, are stirred 5-30 minutes；By the first diazonium salt solution of residue 30% in 30-100
It is added under liquid level in minute, it is ensured that without excessive diazol；Fluid temperature is controlled at 45-60 DEG C, and continues to stir 30-60
Minute, pH value is adjusted to 8-9 with the sodium hydroxide solution of a concentration of 20-30%；It is heated to 75-90 DEG C, 30-40 points of heat preservation
Clock is cooled to 70-75 DEG C, adjusts pH value to 2-3 with hydrochloric acid, stirs 15-30 minutes；Filtering, washing, is done at 80-90 DEG C
It is dry, obtain 2 finished product of C.I. paratoneres.
In the preparation method of above-mentioned C.I. paratoneres 2, this method specifically includes following steps；
A, the preparation of the first diazonium salt solution, includes the following steps by weight；
In diazol reaction kettle, 50-100 parts of water is added, 32.4 portions of 2.5- dichloroanilines are added while stirring, then add
Enter 74.5 parts a concentration of 30% of hydrochloric acid, stir 4-16 hours, ice water is added and adjusts temperature to -5-5 DEG C；By 14.4 parts of nitrous acid
Sodium is dissolved in 40-50 parts of water, is then added in reaction kettle；Stirring 1-2 hours, determination have excessive nitrite ion；It is added
0.5-1 parts of sulfamic acid solution stirs 5-10 minutes, removes excessive nitrite ion；0.5-1 parts of activated carbon is added,
Stirring 15-25 minutes, filtering adjust volume to 1000-1200 liters with ice cube and water, and temperature is less than -3 DEG C, obtains first
Diazonium salt solution；
B, the preparation of the second diazonium salt solution, includes the following steps by weight：
In another diazol reaction kettle, 50-100 part water are added, the toast for being added 5-10 part while stirring is sour, 2B is sour or
4B acid, adds 8.4 parts a concentration of 30% of hydrochloric acid, adjusts temperature to -3-3 DEG C with ice water, stirs 30-40 minutes；By 1.6 parts
Sodium nitrite is dissolved in 10-15 parts of water, is then added in reaction kettle, and control temperature is in -2-2 degree；Stirring 60-90 minutes, really
Surely there is excessive nitrite ion, obtain the second diazonium salt solution；
C, the preparation of Coupling Solution:
In conjugates dissolution kettle, 200-400 parts of water and 55.6 parts of azoic coupling component AS are added, stirring is slurried for 15-20 minutes；It is added
NaOH of 57.6 parts of the concentration 25%, is heated to 60-70 degree, and azoic coupling component AS is completely dissolved；Water cooling on the rocks is adjusted to 10-20 DEG C
Whole product arrives 600-700 parts, and the second diazonium salt solution is added, is uniformly mixing to obtain Coupling Solution；
D, coupling reaction：
In coupling reaction kettle, 200-400 parts of water, 15.6 parts of glacial acetic acid, 12.2 parts a concentration of 37% of concentrated hydrochloric acid is added
With 0.4-1.0 parts of dodecyl sodium sulfates or surfactant, stirring and dissolving；After dissolving, accelerate mixing speed, with 40-45 points
Clock pours into Coupling Solution；It is heated to 45-50 DEG C, 8 parts of calcium carbonate are added, is stirred 5-20 minutes, by wherein 70% the first diazonium
Salting liquid is added in 35-60 minutes under liquid level, and determines no excessive diazol；8 parts of calcium carbonate are added, are stirred
It mixes 5-30 minutes；First diazonium salt solution of residue 30% is added in 30-100 minutes under liquid level, it is ensured that without excessive
Diazol；Fluid temperature is controlled at 45-60 DEG C, and continues stirring 30-60 minutes, with a concentration of 25% sodium hydroxide solution
PH value is adjusted to 8-9；80 DEG C are heated to, 30-40 minutes is kept the temperature, is cooled to 70-75 DEG C, pH value is adjusted to 2-3 with hydrochloric acid, stirs
It mixes 15-30 minutes；Filtering, washing, is dried at 80-90 DEG C, obtains 2 finished product of C.I. paratoneres.
Compared with prior art, present invention improves over production technologies, and the addition of calcium carbonate twice, can play in process
The effect that the reaction was complete is helped, the acidity and alkalinity environment of reaction is stabilized, and existing technique is that addition sodium acetate solution is slow at present
It rushes, increasing for water COD value is discharged when not only reacting not enough completely, and reaction mixture can be brought to wash, causes environmental pollution；Together
When, the present invention is when coupling reaction post-processes, adjustment pH value to 8-9, and afterwards and adjustment pH value is to 2-3, when can to react
Impurity is cleared, and finally by filtering, washing is clean, improves product purity, and mobility improves, and water resistance also improves.Second,
Invention increases the second diazol, preferred surfactant, and specific restriction has been made to its production technology, on the one hand so that
Reaction is more complete, and manufactured product purity higher, glossiness, mobility are more preferable, and intensity index of the invention can be improved after testing
15% or more；On the other hand, particle can be made finer when reaction, so that it is reduced the contact angle of water, increases particle surface polarity,
Stably dispersing performance in water is improved, water resistance improves, and environmental pollution is extremely small in terms of blowdown, efficiently solves pigment
The content overrun issues of contained banned substance Polychlorinated biphenyls.The made pigment of the present invention can be widely used in food packaging article coloring,
It can also be used for fabric printing and pigment coloration.
Description of the drawings
Attached drawing 1 is the atomic force microscope images of test group A in embodiment 3；
Attached drawing 2 is the atomic force microscope images of experiment group B in embodiment 3；
Attached drawing 3 is the atomic force microscope images of test group C in embodiment 3.
Specific implementation mode
With reference to embodiment, the present invention is further illustrated.
Embodiment 1：C.I. the preparation method of paratonere 2, specifically includes following steps：
One, the preparation of the first diazonium salt solution
1. in diazol reaction kettle, the water that 50-100 rises is added.
2. starting to stir.
3. 32.4 kilograms of 2.5- dichloroanilines are added.
4. 74.5 kilograms of hydrochloric acid (30%) is added, stir 10 hours.
5. ice water, which is added, adjusts temperature to-5-5 degrees Celsius.
6. 14.4 kilograms of sodium nitrite is dissolved in the water of 40-50 liters.It rapidly joins in reaction kettle.Keep temperature
At-5-5 degrees Celsius.
7. stirring 1-2 hours, determination has excessive nitrite ion, temperature to maintain-5-5 degrees Celsius.
8. 0.5-1.0 kilograms of sulfamic acid solution is added, stirs 5-10 minutes, remove excessive nitrite ion.Inspection
Survey must not have nitrite ion.Detection method is to drip the solution after stirring 1-2 hours when on potassium iodide starch test paper,
The blue chromosphere instantaneously occurred is to determine the proof of excessive nitrite ion.
9. 0.5-1 kilograms of activated carbon is added, stir 15-25 minutes.
10. filtering adjusts volume to 1000-1200 liters with ice cube and water, temperature is less than -3 degrees Celsius.
Two, the preparation of the second diazonium salt solution
1. in another diazonium salt oven, 50-100 kg of water is added, starts to stir.
2. 8 kilograms of toast acid is added.
3. 8.4 kilograms of hydrochloric acid (concentration 30%) is added.
4. adjusting temperature to -3-3 degrees Celsius with ice water, stir 30-40 minutes.
5. rapidly joining sodium nitrite solution (1.6 kilograms of sodium nitrite dissolving and 10-15 kilograms of water), temperature is kept
At-2-2 degrees Celsius.
6. stirring 60-90 minutes, determination has excessive nitrite ion, and temperature is at-2-2 degrees Celsius.
Three, the preparation of Coupling Solution
1. in conjugates dissolution kettle, 200-400 kg of water and 55.6 kilograms of azoic coupling component AS are added.Stirring 15-20 minutes
It is slurried.
2. 57.6 kilograms of 25%NaOH is added, it is heated to 60-70 degrees Celsius, azoic coupling component AS is completely dissolved.
3. water cooling on the rocks, to 10-20 degrees Celsius, adjustment volume is to 600-700 liters.
4. the second diazonium salt solution is added, stir evenly.
Four, coupling reactions
1. in coupling reaction kettle, 200-400 kg of water, 15.6 kilograms of glacial acetic acid, 12.2 kilograms of concentrated hydrochloric acid (concentration are added
37%) and 0.4-1.0 kilograms of dodecyl sodium sulfate or surfactant, stirring and dissolving.
2. after dissolving, accelerating mixing speed, the Coupling Solution prepared being poured into 40-45 minutes.
3. being heated to 45-50 degrees Celsius, 8 kilograms of calcium carbonate are added, stir 5-20 minutes.
4. the first diazonium salt solution prepared by 70% is added with 35-60 minutes under liquid level.
5. determining at any time without excessive diazol.After 70% diazol adds, 8 kilograms of carbonic acid are added
Calcium stirs 5-30 minutes.
6. remaining 30% the first diazonium salt solution is slowly added to 30-100 minutes under liquid level, determine in office
When between without excessive diazol.
7. keeping fluid temperature at 45-60 degrees Celsius, continue stirring 30-60 minutes.
8. adjusting pH value to 8-9 with 25% sodium hydroxide solution.
9. being heated to 80 degrees Celsius, 30-40 minutes are kept the temperature at 80 degrees Celsius.
10. being cooled to 70-75 degrees Celsius, pH value is adjusted to 2.0-3.0 with hydrochloric acid, stirs 15-30 minutes, determines that pH value exists
2.0-3.0。
11. filtering, washing are dried at 80-90 degrees Celsius to get pigment finished product.
Embodiment 2：C.I. the preparation method of paratonere 2, specifically includes following steps：
One, the preparation of the first diazonium salt solution
1. in diazol reaction kettle, the water that 50-100 rises is added.
2. starting to stir.
3. 35 kilograms of 2.5- dichloroanilines are added.
4. 75 kilograms of hydrochloric acid (30%) is added, stir 10 hours.
5. ice water, which is added, adjusts temperature to-5-5 degrees Celsius.
6. 16 kilograms of sodium nitrite is dissolved in the water of 40-50 liters.It rapidly joins in reaction kettle.Maintain the temperature at-
5-5 degrees Celsius.
7. stirring 1-2 hours, determination has excessive nitrite ion, temperature to maintain-5-5 degrees Celsius.
8. 0.5-1.0 kilograms of sulfamic acid solution is added, stirs 5-10 minutes, remove excessive nitrite ion.Inspection
Survey must not have nitrite ion.Detection method is to drip the solution after stirring 1-2 hours when on potassium iodide starch test paper,
The blue chromosphere instantaneously occurred is to determine the proof of excessive nitrite ion.
9. 0.5-1 kilograms of activated carbon is added, stir 15-25 minutes.
10. filtering adjusts volume to 1000-1200 liters with ice cube and water, temperature is less than -3 degrees Celsius.
Two, the preparation of the second diazonium salt solution
1. in another diazonium salt oven, 50-100 kg of water is added, starts to stir.
2. 5 kilograms of 2B acid is added.
3. 9 kilograms of hydrochloric acid (concentration 30%) is added.
4. adjusting temperature to -3-3 degrees Celsius with ice water, stir 30-40 minutes.
5. sodium nitrite solution (2 kilograms of sodium nitrite dissolving and 13 kilograms of water) is added, maintains the temperature at-2-2 and take the photograph
Family name's degree.
6. stirring 60-90 minutes, determination has excessive nitrite ion, and temperature is at-2-2 degrees Celsius.
Three, the preparation of Coupling Solution
1. in conjugates dissolution kettle, 200-400 kg of water and 50 kilograms of azoic coupling component AS are added.Stirring 15-20 minutes at
Slurry.
2. 50 kilograms of 25%NaOH is added, it is heated to 60-70 degrees Celsius, azoic coupling component AS is completely dissolved.
3. water cooling on the rocks, to 10-20 degrees Celsius, adjustment volume is to 600-700 liters.
4. the second diazonium salt solution is added, stir evenly.
Four, coupling reactions
1. in coupling reaction kettle, 200-400 kg of water, 13 kilograms of glacial acetic acid, 15 kilograms of concentrated hydrochloric acid (concentration are added
40%) and 0.4-1.0 kilograms of dodecyl sodium sulfate or surfactant, stirring and dissolving.
2. after dissolving, accelerating mixing speed, the Coupling Solution prepared being poured into 40-45 minutes.
3. being heated to 45-50 degrees Celsius, 10 kilograms of calcium carbonate are added, stir 5-20 minutes.
4. the first diazonium salt solution prepared by 70% is added with 35-60 minutes under liquid level.
5. determining at any time without excessive diazol.After 70% diazol adds, 10 kilograms of carbon are added
Sour calcium stirs 5-30 minutes.
6. remaining 30% the first diazonium salt solution is slowly added to 30-100 minutes under liquid level, determine in office
When between without excessive diazol.
7. keeping fluid temperature at 45-60 degrees Celsius, continue stirring 30-60 minutes.
8. adjusting pH value to 8-9 with 30% sodium hydroxide solution.
9. being heated to 85 degrees Celsius, 30-40 minutes are kept the temperature at 85 degrees Celsius.
10. being cooled to 70-75 degrees Celsius, pH value is adjusted to 2.0-3.0 with hydrochloric acid, stirs 15-30 minutes, determines that pH value exists
2.0-3.0。
11. filtering, washing are dried at 80-90 degrees Celsius to get pigment finished product.
Embodiment 3：
Applicant has also made contrast test to commercially available common product, embodiment 1, embodiment 2, and applicant will in following tests
Commercially available common product, embodiment 1, embodiment 2 are respectively defined as test group A, experiment group B and test group C, three productions of applicant couple
Product are observed using atomic force microscope, three groups of different atomic force microscope images such as figure below：
Fig. 1-Fig. 3 is that the pigment product of test group A, experiment group B and test group C are seen using atomic force microscope respectively
The image examined.Compared with test group A, experiment group B and test group C are added after the second diazol further in stock blend
The surface roughness for improving pigment, since the raw material components of experiment group B have made proportioning and technological parameter specific preferred, pigment
Surface roughness substantially reduce, therefore greatly increase adhesive force, so that it is reduced the contact angle of water, increase particle table
Face polarity, improves stably dispersing performance in water, and water resistance improves.
Claims (2)
1. a kind of preparation method of C.I. paratoneres 2, it is characterised in that：This method specifically includes following steps；
A, the preparation of the first diazonium salt solution, includes the following steps by weight；
In diazol reaction kettle, 50-100 parts of water is added, 30-40 portions of 2.5- dichloroanilines are added while stirring, add
The hydrochloric acid of 70-80 parts of a concentration of 20-40% stirs 4-16 hours, and ice water is added and adjusts temperature to -5-5 DEG C；By 13-16 parts of Asias
Sodium nitrate is dissolved in 40-50 parts of water, is then added in reaction kettle；Stirring 1-2 hours, determination have excessive nitrite ion；
0.5-1 parts of sulfamic acid solution is added, stirs 5-10 minutes, removes excessive nitrite ion；0.5-1 parts of activity is added
Carbon stirs 15-25 minute, filtering, and volume is adjusted to 1000-1200 liters with ice cube and water, and temperature is less than -3 DEG C, obtains the
One diazonium salt solution；
B, the preparation of the second diazonium salt solution, includes the following steps by weight：
In another diazol reaction kettle, 50-100 parts of water are added, 5-10 parts of toast acid, 2B acid or 4B are added while stirring
Acid adds the hydrochloric acid of 5-10 parts of a concentration of 20-40%, adjusts temperature to -3-3 DEG C with ice water, stirs 30-40 minutes；By 1-2
Part sodium nitrite is dissolved in 10-15 parts of water, is then added in reaction kettle；Stirring 60-90 minutes, determination have excessive nitrous acid
Ion, control temperature obtain the second diazonium salt solution in -2-2 degree；
C, the preparation of Coupling Solution
In conjugates dissolution kettle, 200-400 parts of water and 40-60 parts of azoic coupling component AS are added, stirring is slurried for 15-20 minutes；40- is added
NaOH of 60 parts of the concentration 25%, is heated to 60-70 degree, and azoic coupling component AS is completely dissolved；Water cooling on the rocks is adjusted to 10-20 degree
Volume is added the second diazonium salt solution, is uniformly mixing to obtain Coupling Solution to 600-700 parts；
D, coupling reaction：
In coupling reaction kettle, the concentrated hydrochloric acid of 200-400 parts of water, 12-18 parts of glacial acetic acid, 10-15 parts of a concentration of 30-40% is added
With 0.4-1.0 parts of dodecyl sodium sulfates or surfactant, stirring and dissolving；After dissolving, accelerate mixing speed, with 40-45 points
Clock pours into Coupling Solution；It is heated to 45-50 DEG C, 5-10 parts of calcium carbonate are added, is stirred 5-20 minutes, by wherein 70% the first weight
Nitrogen salt solution is added in 35-60 minutes under liquid level, and determines no excessive diazol；Add 5-10 parts of carbonic acid
Calcium stirs 5-30 minutes；First diazonium salt solution of residue 30% is added in 30-100 minutes under liquid level, it is ensured that do not have
Excessive diazol；Fluid temperature is controlled at 45-60 DEG C, and continues stirring 30-60 minutes, with the hydrogen-oxygen of a concentration of 20-30%
Change sodium solution and adjusts pH value to 8-9；It is heated to 75-90 DEG C, 30-40 minutes is kept the temperature, is cooled to 70-75 DEG C, is adjusted with hydrochloric acid
PH value stirs 15-30 minutes to 2-3；Filtering, washing, is dried at 80-90 DEG C, obtains 2 finished product of C.I. paratoneres.
2. the preparation method of C.I. paratoneres 2 according to claim 1, it is characterised in that：This method specifically includes following
Step；
A, the preparation of the first diazonium salt solution, includes the following steps by weight；
In diazol reaction kettle, 50-100 parts of water is added, 32.4 portions of 2.5- dichloroanilines are added while stirring, add
74.5 parts a concentration of 30% of hydrochloric acid stirs 4-16 hours, and ice water is added and adjusts temperature to -5-5 DEG C；By 14.4 parts of sodium nitrites
It is dissolved in 40-50 parts of water, is then added in reaction kettle；Stirring 1-2 hours, determination have excessive nitrite ion；It is added
0.5-1 parts of sulfamic acid solution stirs 5-10 minutes, removes excessive nitrite ion；0.5-1 parts of activated carbon is added,
Stirring 15-25 minutes, filtering adjust volume to 1000-1200 liters with ice cube and water, and temperature is less than -3 DEG C, obtains first
Diazonium salt solution；
B, the preparation of the second diazonium salt solution, includes the following steps by weight：
In another diazol reaction kettle, 50-100 parts of water are added, 5-10 parts of toast acid, 2B acid or 4B are added while stirring
Acid adds 8.4 parts a concentration of 30% of hydrochloric acid, adjusts temperature to -3-3 DEG C with ice water, stirs 30-40 minutes；By 1.6 parts of Asias
Sodium nitrate is dissolved in 10-15 parts of water, is then added in reaction kettle, and control temperature is in -2-2 degree；Stirring 60-90 minutes determines
There is excessive nitrite ion, obtains the second diazonium salt solution；
C, the preparation of Coupling Solution:
In conjugates dissolution kettle, 200-400 parts of water and 55.6 parts of azoic coupling component AS are added, stirring is slurried for 15-20 minutes；It is added 57.6
NaOH of the concentration of part 25%, is heated to 60-70 degree, azoic coupling component AS is completely dissolved；Water cooling on the rocks is to 10-20 DEG C, adjusting body
Product arrives 600-700 parts, and the second diazonium salt solution is added, is uniformly mixing to obtain Coupling Solution；
D, coupling reaction：
In coupling reaction kettle, be added 200-400 parts of water, 15.6 parts of glacial acetic acid, 12.2 parts a concentration of 37% of concentrated hydrochloric acid and
0.4-1.0 parts of dodecyl sodium sulfates or surfactant, stirring and dissolving；After dissolving, accelerate mixing speed, with 40-45 minutes
Pour into Coupling Solution；It is heated to 45-50 DEG C, 8 parts of calcium carbonate are added, is stirred 5-20 minutes, by wherein 70% the first diazol
Solution is added in 35-60 minutes under liquid level, and determines no excessive diazol；8 parts of calcium carbonate are added, are stirred
5-30 minutes；First diazonium salt solution of residue 30% is added in 30-100 minutes under liquid level, it is ensured that not excessive
Diazol；Fluid temperature is controlled at 45-60 DEG C, and continues stirring 30-60 minutes, with a concentration of 25% sodium hydroxide solution tune
Whole pH value is to 8-9；80 DEG C are heated to, 30-40 minutes is kept the temperature, is cooled to 70-75 DEG C, pH value is adjusted to 2-3, stirring with hydrochloric acid
15-30 minutes；Filtering, washing, is dried at 80-90 DEG C, obtains 2 finished product of C.I. paratoneres.
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| CN114479509A (en) * | 2021-12-20 | 2022-05-13 | 杭州红妍颜料化工有限公司 | Preparation method of uniformly dispersed pigment red |
| CN117417649A (en) * | 2023-10-12 | 2024-01-19 | 济宁阳光化学有限公司 | Environment-friendly high-performance pigment red P.R.2 and preparation method and application thereof |
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Application publication date: 20181113 |