CN110128845A - A kind of technical process producing high light-fast fastness, high durable fastness pigment yellow 74 - Google Patents
A kind of technical process producing high light-fast fastness, high durable fastness pigment yellow 74 Download PDFInfo
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- CN110128845A CN110128845A CN201910364720.9A CN201910364720A CN110128845A CN 110128845 A CN110128845 A CN 110128845A CN 201910364720 A CN201910364720 A CN 201910364720A CN 110128845 A CN110128845 A CN 110128845A
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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
- C09B29/32—Monoazo dyes prepared by diazotising and coupling from coupling components containing a reactive methylene group
- C09B29/33—Aceto- or benzoylacetylarylides
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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
- C09B51/00—Nitro or nitroso dyes
-
- 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
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0017—Influencing the physical properties by treatment with an acid, H2SO4
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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
Abstract
The present invention relates to Special environment protection paint fields, and in particular, to a kind of technical process for producing high light-fast fastness, high durable fastness pigment yellow 74, including following workshop section: (1) diazotising；(2) it is coupled；(3) it refines.The speed of acetic acid is added dropwise by control for the technical process of production pigment yellow 74 provided by the invention, effectively controls orthomethoxy-acetoacetanilide granular size, keeps orthomethoxy-acetoacetanilide coupling reaction complete；Optimize each workshop section of technique, the especially selection and control of reaction temperature, choose the temperature and time etc. of optimal pigment post-processing, high light-fast fastness, high durable fastness, high gloss and the high grade of transparency, good fluidity, environmental protection, durable, heat-resisting, solvent resistant characteristic pigment yellow 74 are produced, it is made to be widely used in the fields such as car paint, coloring plastic, high-grade ink.
Description
Technical field
The present invention relates to Special environment protection organic pigment field, in particular to a kind of production high light-fast fastness, high durable fastness
The technical process of pigment yellow 74.
Background technique
Pigment yellow 74 is a kind of pigment with important commercial value, is mainly used in printing ink and coatings industry.It
Mill base between pigment yellow 1 and pigment yellow 3, tinting strength, tinting power will be high than other any monoazo pigment yellow.Pigment yellow 74
Acidproof, alkaline-resisting, resistance to saponification, but its Yi Qishuan, which prevent its applications in baking enamel paint.74 light fastness of pigment yellow compares
The similar bisazo yellow uitramarine of color power is higher by 2-3 grades, therefore can be applied in the printing ink of packaging, when for block letter
When in system, it is desirable that print the low viscosity of ink.Pigment yellow 74 is also widely applied in emulsion paint simultaneously, outer as interior wall and dark color
Wall coloring is used.It is high to the application technology performance requirement of pigment in terms of being coloured for organic material, it is high such as brilliant idea intensity of colour
Coloration (chromaticity) and good light fastness and weather-proof fastness.When in coating system, it is desirable that flawless resistance to apply jail again
Degree, the low viscosity of highly colored paint concentrate (abrasive) and the low viscosity of finished product coating；Particularly, in metallic finishes
In the case of, it is desirable that pigment has the high grade of transparency and bright tone.In the case where dyeing of plastics, it is desirable that pigment has good point
Property is dissipated, good dispersibility is embodied in brilliant idea intensity of colour.
Conventional pigment Huang 74 cannot accomplish high gloss and the high grade of transparency, good fluidity simultaneously, and high light-fast fastness, height are resistance to
Wait fastness and environmental protection, durable, heat-resisting, solvent-proof product.One of production difficult point is of orthomethoxy-acetoacetanilide
Grain size directly results in coupling reaction and carries out not exclusively, and then influences the performance of product, and coloured light is partially dark, gloss difference.The two of difficult point
It is to post-process heating and turns a brilliant colourshifting process, the high crystal form of temperature obtains growing up then poor transparency；Temperature is low, do not occur discoloration or
Not exclusively then coloured light shades, mobility is bad, gloss difference for discoloration.Difficult point be repeatedly waste gas exhaust processing environmental pollution compared with
Greatly, it is unsatisfactory for the demand of sustainable development.
Summary of the invention
The purpose of invention: the purpose of the present invention is to provide a kind of production high light-fast fastness, high durable fastness pigment yellow 74
Technical process, by control be added dropwise acetic acid speed, effectively control orthomethoxy-acetoacetanilide granular size, make adjacent first
Oxygroup acetoacetanilide coupling reaction is complete；Optimize each workshop section of technique, the especially selection and control of reaction temperature, choosing
The temperature and time etc. for taking optimal pigment to post-process produces high light-fast fastness, high durable fastness, high gloss and high transparency
Degree, good fluidity, environmental protection, durable, heat-resisting, solvent resistant characteristic pigment yellow 74 make it be widely used in car paint, plastics
The fields such as color, high-grade ink.
Technical solution: in order to achieve the goal above, the invention discloses a kind of production high light-fast fastness, high durable fastness face
The technical process of material Huang 74, including three big workshop sections of diazotising, coupling and purification:
(1) diazotising workshop section:
A, tap water is added in diazonium bucket by pipeline, 2- methoxyl group -4- nitroaniline powder is passed through into feed opening
It is added in diazonium bucket, opens stirring, the hydrochloric acid acid for being then added 31% by hydrochloric acid head tank is molten, 1h is stirred, from trash ice pipe
Trash ice is added into diazonium bucket and cools to 0 DEG C for road；
B, 98% sodium nitrite is made into 30% aqueous solution in sodium nitrite material bucket, is squeezed into through sodium nitrite feed pump
It is added in diazonium bucket into sodium nitrite head tank, then from sodium nitrite head tank using high potential difference；
C, diazo-reaction is carried out in diazonium bucket, diazo-reaction carries out under the conditions of 0~10 DEG C of tiny structure, diazonium
The change reaction time is 1.5~2h, and the gas generated in reaction process goes exhaust-gas treatment；The temperature of the diazo-reaction passes through temperature
Controller is spent to control, and when the reaction temperature in diazonium bucket is more than 10 DEG C, the temperature controller of diazonium bucket issues alarm, and certainly
The dynamic dropwise addition for stopping sodium nitrite, is automatically added to trash ice from trash ice pipeline.
(2) it is coupled workshop section:
A, peracetic acid formulation: 98% acetic acid with diaphragm pump is got to beater tub, and (winter is 20 DEG C or so in the small drying chamber in workshop
Heat preservation melting), quantitative water is added, is configured to the acetic acid that concentration is 60%；Prepared acetic acid pump is squeezed into an acetic acid high position
It is spare in slot；
B, tap water is added in coupling component bucket by pipeline, by orthomethoxy-acetoacetanilide powder by adding
Material mouth is added in coupling component bucket, and 32% liquid alkaline is added by elevated tank with caustic soda liquid, stirs 2h；
C, trash ice is added into coupling component bucket from trash ice pipeline and cools to 5 DEG C, the acetic acid through measuring is passed through into acetic acid height
Position slot is added directly into coupling part bucket using high potential difference and carries out acid out, and the acid out time is 2~3h, and pH value adjustment is 6.5~7.5
Between, temperature is controlled at 20~25 DEG C, enters coupling bucket using liquid level difference after acid out；The purpose of acid out is to make material
Under acid condition, the speed control orthomethoxy-acetoacetanilide granular size of acetic acid is added dropwise by control, makes adjacent first
Oxygroup acetoacetanilide coupling reaction is complete.
D, rubble ice is added into coupling bucket by trash ice pipeline makes temperature control at 8~12 DEG C, and step (1) has been made
Good diazo liquid carries out coupling reaction from being slowly added into diazonium bucket using liquid level difference in coupling bucket, and coupling reaction control exists
It is carried out under 20~30 DEG C of tiny structure, the reaction time is 2~3h, and acetic acid head tank tune pH value, terminal are used during coupling reaction
PH value is 6；
E, it puts into water, emulsifier in dissolving bucket to stir, using high potential difference by cream prepared in dissolving bucket
Agent is added to coupling bucket, if temperature is more than that 30 DEG C of temperature controllers issue alarm in reaction process, when overtemperature is automatically cut off
Trash ice is added into coupling bucket by trash ice pipeline in charging, after stirring 1h, is passed through heating steam to coupling bucket by jet chimney
Heated material enters refinement to 80~85 DEG C under tiny structure；The exhaust gas generated in reaction process goes vent gas treatment；
(3) refinement:
Conjugates are squeezed into diaphragm filter press filters pressing 1.5h with mashing pump after pump front filter filtering, are added by pipeline
Tap water rinse material forms filter cake to neutrality, then with compressed air stripping 10min, and the waste water that filters pressing, rinsing generate removes waste water
Processing；Filter cake is sent into drying in belt machine, and filter cake drying time dry in belt machine is 1.5~2h, through crushing after drying
After machine crushes, it is put into blending bucket blending, analysis, metering, packs to obtain pigment yellow 74.
Further, step (1) diazo-reaction carries out under the conditions of 0~5 DEG C of tiny structure, when diazo-reaction
Between be 2h.
Further, all reaction temperatures are controlled using temperature controller in technical process of the invention, once overtemperature, meeting
Alarm is issued immediately, stops charging, and be automatically added to trash ice from trash ice pipeline.
Further, in terms of 2- methoxyl group -4- nitroaniline, reaction conversion ratio is step (1) diazo-reaction
95%, yield 95%.
Further, step (2) coupling reaction control carries out under 20~25 DEG C of tiny structure, and the reaction time is
3h, coupling reaction use acetic acid head tank tune pH value in the process, and terminal pH value is 6.
Further, the raw material of step (2) described emulsifier includes following component by mass parts: 45~50 parts of monohydric alcohol,
55~60 parts of hexamethylene diisocyanate, 250~260 parts of polyethylene glycol, 0.001~0.003 part of dibutyltin diacetate, deionized water
300~350 parts.
Further, step (2) the acid out time is 3h, and pH value adjustment is between 7.5~7, and temperature is controlled at 25 DEG C.
Further, the feeding temperature that filter cake in step (3) described subtractive process is sent into belt machine is set as 110~
120 DEG C, drop temperature is set as 60~80 DEG C.
Further, the drying time dry in belt machine of the filter cake in step (3) described subtractive process is 1.5h.
Further, chemical reaction involved in high light-fast fastness, the technical process of high durable fastness pigment yellow 74 is produced
Equation is as follows:
1, diazotising
2- methoxyl group -4- nitroaniline+hydrochloric acid+sodium nitrite → diazonium salt dissolving+sodium chloride+water
Side reaction:
2NaNO2+2HCl→2NaCl+NO2↑+NO↑+H2O
NO2+NO+2NaOH→2NaNO2+H2O
2, it is coupled
Diazonium salt+orthomethoxy-acetoacetanilide → pigment yellow 74+ hydrogen chloride
Acid out: CH3COOH+NaOH→CH3COONa+H2O
Tail gas absorption: NaOH+HCl → NaCl+H2O
Above-mentioned technical proposal can be seen that the invention has the following beneficial effects:
(1) a kind of technical process for producing pigment yellow 74 is provided, the speed of acetic acid is added dropwise by control, effectively control is adjacent
Methoxyl group acetoacetanilide granular size, keeps orthomethoxy-acetoacetanilide coupling reaction complete；Optimize each of technique
The temperature and time etc. of optimal pigment post-processing is chosen in the selection and control of workshop section, especially reaction temperature, produces high resistance to
Shine fastness, high durable fastness, high gloss and the high grade of transparency, good fluidity, environmental protection, durable, heat-resisting, solvent resistant characteristic pigment
Huang 74 makes it be widely used in the fields such as car paint, coloring plastic, high-grade ink；
(2) the production process design that the present invention uses is reasonable, the high conversion rate of pigment yellow 74；Technique mistake of the invention
All reaction temperatures are controlled using temperature controller in journey, once overtemperature, can issue alarm immediately, stop charging, and from trash ice
Pipeline is automatically added to trash ice, efficiently controls reaction temperature, while improving reaction conversion ratio, can make reaction more smoothly into
Row, improves the selectivity of reaction, improves the purity of product, occurs with reducing side reaction, reduces the generation of by-product, has technique
Process is simple, economical rationality, at low cost, the small feature of raw materials used environmental pollution；
(3) rationally, waste gas exhaust processing environmental pollution is extremely small, mistake for the production process design that the present invention uses
Cheng Huanbao meets the needs of sustainable development.
Specific embodiment
Below will be by several specific embodiments, the present invention is furture elucidated, these embodiments simply to illustrate that problem,
It is not a kind of limitation.
Embodiment 1:
A kind of technical process producing high light-fast fastness, high durable fastness pigment yellow 74, including diazotising, coupling and purification
Three big workshop sections:
(1) diazotising workshop section:
A, tap water is added in diazonium bucket by pipeline, 2- methoxyl group -4- nitroaniline powder is passed through into feed opening
It is added in diazonium bucket, opens stirring, the hydrochloric acid acid for being then added 31% by hydrochloric acid head tank is molten, 1h is stirred, from trash ice pipe
Trash ice is added into diazonium bucket and cools to 0 DEG C for road；
B, 98% sodium nitrite is made into 30% aqueous solution in sodium nitrite material bucket, is squeezed into through sodium nitrite feed pump
It is added in diazonium bucket into sodium nitrite head tank, then from sodium nitrite head tank using high potential difference；
C, diazo-reaction is carried out in diazonium bucket, diazo-reaction carries out under the conditions of 0~5 DEG C of tiny structure, diazonium
The change reaction time is 2h, and the gas generated in reaction process goes exhaust-gas treatment；The temperature of diazo-reaction passes through temperature controller
It controls, the temperature controller of diazonium bucket issues alarm when the reaction temperature in diazonium bucket is more than 10 DEG C, and is automatically stopped Asia
The dropwise addition of sodium nitrate is automatically added to trash ice from trash ice pipeline.In terms of 2- methoxyl group -4- nitroaniline, reaction turns diazo-reaction
Rate is 95%, yield 95%.
(2) it is coupled workshop section:
A, peracetic acid formulation: 98% acetic acid with diaphragm pump is got to beater tub, and (winter is 20 DEG C or so in the small drying chamber in workshop
Heat preservation melting), quantitative water is added, is configured to the acetic acid that concentration is 60%；Prepared acetic acid pump is squeezed into an acetic acid high position
It is spare in slot；
B, tap water is added in coupling component bucket by pipeline, by orthomethoxy-acetoacetanilide powder by adding
Material mouth is added in coupling component bucket, and 32% liquid alkaline is added by elevated tank with caustic soda liquid, stirs 2h；
C, trash ice is added into coupling component bucket from trash ice pipeline and cools to 5 DEG C, the acetic acid through measuring is passed through into acetic acid height
Position slot is added directly into coupling part bucket using high potential difference and carries out acid out, and the acid out time is 3h, and pH value adjustment is between 7~7.5,
Temperature is controlled at 25 DEG C, enters coupling bucket using liquid level difference after acid out；The purpose of acid out is to make material be in acidity
Under the conditions of, the speed control orthomethoxy-acetoacetanilide granular size of acetic acid is added dropwise, by control for O-methoxy second
Acyl antifebrin coupling reaction is complete.
D, rubble ice is added into coupling bucket by trash ice pipeline makes temperature control at 8~12 DEG C, and step (1) has been made
Good diazo liquid carries out coupling reaction from being slowly added into diazonium bucket using liquid level difference in coupling bucket, and coupling reaction control exists
It is carried out under 20~25 DEG C of tiny structure, reaction time 3h, acetic acid head tank tune pH value, terminal pH value is used during coupling reaction
It is 6；
E, it puts into water, emulsifier in dissolving bucket to stir, using high potential difference by cream prepared in dissolving bucket
Agent is added to coupling bucket, if temperature is more than that 30 DEG C of temperature controllers issue alarm in reaction process, when overtemperature is automatically cut off
Trash ice is added into coupling bucket by trash ice pipeline in charging, after stirring 1h, is passed through heating steam to coupling bucket by jet chimney
Heated material enters refinement to 80~85 DEG C under tiny structure；The exhaust gas generated in reaction process goes vent gas treatment；Above-mentioned cream
The raw material of agent includes following component by mass parts: 45~50 parts of monohydric alcohol, 55~60 parts of hexamethylene diisocyanate, and polyethylene glycol
250~260 parts, 0.001~0.003 part of dibutyltin diacetate, 300~350 parts of deionized water.
(3) refinement:
Conjugates are squeezed into diaphragm filter press filters pressing 1.5h with mashing pump after pump front filter filtering, are added by pipeline
Tap water rinse material forms filter cake to neutrality, then with compressed air stripping 10min, and the waste water that filters pressing, rinsing generate removes waste water
Processing；Filter cake is sent into drying in belt machine, and the feeding temperature that filter cake is sent into belt machine is set as 110~120 DEG C, and drop temperature is set
60~80 DEG C are set to, filter cake drying time dry in belt machine is that 1.5h is put into blending after drying after pulverizer crushes
Bucket blending, metering, packs to obtain pigment yellow 74 at analysis.
Embodiment 2:
A kind of technical process producing high light-fast fastness, high durable fastness pigment yellow 74, including diazotising, coupling and purification
Three big workshop sections:
(1) diazotising workshop section:
A, tap water is added in diazonium bucket by pipeline, 2- methoxyl group -4- nitroaniline powder is passed through into feed opening
It is added in diazonium bucket, opens stirring, the hydrochloric acid acid for being then added 31% by hydrochloric acid head tank is molten, 1h is stirred, from trash ice pipe
Trash ice is added into diazonium bucket and cools to 0 DEG C for road；
B, 98% sodium nitrite is made into 30% aqueous solution in sodium nitrite material bucket, is squeezed into through sodium nitrite feed pump
It is added in diazonium bucket into sodium nitrite head tank, then from sodium nitrite head tank using high potential difference；
C, diazo-reaction is carried out in diazonium bucket, diazo-reaction carries out under the conditions of 0~5 DEG C of tiny structure, diazonium
The change reaction time is 1.5h, and the gas generated in reaction process goes exhaust-gas treatment；The temperature of diazo-reaction is controlled by temperature
Device controls, and the temperature controller of diazonium bucket issues alarm when the reaction temperature in diazonium bucket is more than 10 DEG C, and is automatically stopped
The dropwise addition of sodium nitrite is automatically added to trash ice from trash ice pipeline.Diazo-reaction is in terms of 2- methoxyl group -4- nitroaniline, reaction
Conversion ratio is 95%, yield 95%.
(2) it is coupled workshop section:
A, peracetic acid formulation: 98% acetic acid with diaphragm pump is got to beater tub, and (winter is 20 DEG C or so in the small drying chamber in workshop
Heat preservation melting), quantitative water is added, is configured to the acetic acid that concentration is 60%；Prepared acetic acid pump is squeezed into an acetic acid high position
It is spare in slot；
B, tap water is added in coupling component bucket by pipeline, by orthomethoxy-acetoacetanilide powder by adding
Material mouth is added in coupling component bucket, and 32% liquid alkaline is added by elevated tank with caustic soda liquid, stirs 2h；
C, trash ice is added into coupling component bucket from trash ice pipeline and cools to 5 DEG C, the acetic acid through measuring is passed through into acetic acid height
Position slot is added directly into coupling part bucket using high potential difference and carries out acid out, and the acid out time is 2h, and pH value adjustment is between 6.5~7,
Temperature is controlled at 20 DEG C, enters coupling bucket using liquid level difference after acid out；The purpose of acid out is to make material be in acidity
Under the conditions of, the speed control orthomethoxy-acetoacetanilide granular size of acetic acid is added dropwise, by control for O-methoxy second
Acyl antifebrin coupling reaction is complete；
D, rubble ice is added into coupling bucket by trash ice pipeline makes temperature control at 8~12 DEG C, and step (1) has been made
Good diazo liquid carries out coupling reaction from being slowly added into diazonium bucket using liquid level difference in coupling bucket, and coupling reaction control exists
It is carried out under 25~30 DEG C of tiny structure, reaction time 2h, acetic acid head tank tune pH value, terminal pH value is used during coupling reaction
It is 6；
E, it puts into water, emulsifier in dissolving bucket to stir, using high potential difference by cream prepared in dissolving bucket
Agent is added to coupling bucket, if temperature is more than that 30 DEG C of temperature controllers issue alarm in reaction process, when overtemperature is automatically cut off
Trash ice is added into coupling bucket by trash ice pipeline in charging, after stirring 1h, is passed through heating steam to coupling bucket by jet chimney
Heated material enters refinement to 80~85 DEG C under tiny structure；The exhaust gas generated in reaction process goes vent gas treatment；Above-mentioned cream
The raw material of agent includes following component by mass parts: 45~50 parts of monohydric alcohol, 55~60 parts of hexamethylene diisocyanate, and polyethylene glycol
250~260 parts, 0.001~0.003 part of dibutyltin diacetate, 300~350 parts of deionized water.
(3) refinement:
Conjugates are squeezed into diaphragm filter press filters pressing 1.5h with mashing pump after pump front filter filtering, are added by pipeline
Tap water rinse material forms filter cake to neutrality, then with compressed air stripping 10min, and the waste water that filters pressing, rinsing generate removes waste water
Processing；Filter cake is sent into drying in belt machine, and the feeding temperature that filter cake is sent into belt machine is set as 110~120 DEG C, and drop temperature is set
60~80 DEG C are set to, filter cake drying time dry in belt machine is that 2h is put into blending bucket after drying after pulverizer crushes
Blending, metering, packs to obtain pigment yellow 74 at analysis.
The above is only embodiments of the present invention, it should be noted that for those skilled in the art,
Without departing from the principle of the present invention, several improvement can also be made, these improvement also should be regarded as protection model of the invention
It encloses.
Claims (9)
1. a kind of technical process for producing high light-fast fastness, high durable fastness pigment yellow 74, it is characterised in that: including diazotising,
Three big workshop sections of coupling and purification:
(1) diazotising workshop section:
A, tap water is added in diazonium bucket by pipeline, 2- methoxyl group -4- nitroaniline powder is added by feed opening
Into diazonium bucket, open stirring, then by hydrochloric acid head tank be added 31% hydrochloric acid acid it is molten, stir 1h, from trash ice pipeline to weight
Trash ice is added in nitrogen bucket and cools to 0 DEG C；
B, 98% sodium nitrite is made into 30% aqueous solution in sodium nitrite material bucket, is driven into nitrous through sodium nitrite feed pump
In sour sodium head tank, then it is added in diazonium bucket from sodium nitrite head tank using high potential difference；
C, diazo-reaction is carried out in diazonium bucket, diazo-reaction carries out under the conditions of 0~10 DEG C of tiny structure, and diazotising is anti-
It is 1.5 ~ 2h between seasonable, the gas generated in reaction process goes exhaust-gas treatment；
(2) it is coupled workshop section:
A, peracetic acid formulation: getting to beater tub with diaphragm pump for 98% acetic acid, quantitative water be added, and is configured to the second that concentration is 60%
Acid；Prepared acetic acid pump is squeezed into spare in acetic acid head tank；
B, tap water is added in coupling component bucket by pipeline, orthomethoxy-acetoacetanilide powder is passed through into feed opening
It is added in coupling component bucket, 32% liquid alkaline is added by elevated tank with caustic soda liquid, stirs 2h；
C, trash ice is added into coupling component bucket from trash ice pipeline and cools to 5 DEG C, the acetic acid through measuring is passed through into acetic acid head tank
It being added directly into coupling part bucket using high potential difference and carries out acid out, the acid out time is 2 ~ 3h, and pH value adjustment is between 6.5 ~ 7.5,
Temperature is controlled at 20 ~ 25 DEG C, enters coupling bucket using liquid level difference after acid out；
D, rubble ice is added into coupling bucket by trash ice pipeline makes temperature control at 8 ~ 12 DEG C, and step (1) has been made
Diazo liquid carries out coupling reaction from being slowly added into diazonium bucket using liquid level difference in coupling bucket, and coupling reaction is controlled 20 ~ 30
DEG C tiny structure under carry out, the reaction time is 2 ~ 3h, and acetic acid head tank tune pH value is used during coupling reaction, and terminal pH value is 6；
E, it puts into water, emulsifier in dissolving bucket to stir, using high potential difference by emulsifier prepared in dissolving bucket
It is added to coupling bucket, if temperature is more than that 30 DEG C of temperature controllers issue alarm in reaction process, when overtemperature, automatically cuts off charging,
Trash ice is added into coupling bucket by trash ice pipeline, after stirring 1h, heating steam heating is passed through to coupling bucket by jet chimney
Material enters refinement to 80 ~ 85 DEG C under tiny structure；The exhaust gas generated in reaction process goes vent gas treatment；
(3) refinement:
Conjugates are squeezed into diaphragm filter press filters pressing 1.5h with mashing pump after pump front filter filtering, are added originally by pipeline
Water rinses material to neutrality, then forms filter cake with compressed air stripping 10min, filters pressing, rinsing generation waste water go wastewater treatment；
Filter cake is sent into drying in belt machine, and filter cake drying time dry in belt machine is 1.5 ~ 2h, crushes after dry through pulverizer
Afterwards, it is put into blending bucket blending, analysis, metering, packs to obtain pigment yellow 74.
2. a kind of technical process for producing high light-fast fastness, high durable fastness pigment yellow 74 according to claim 1, special
Sign is: step (1) diazo-reaction carries out under the conditions of 0~5 DEG C of tiny structure, and the diazo-reaction time is 2h.
3. a kind of technical process for producing high light-fast fastness, high durable fastness pigment yellow 74 according to claim 2, special
Sign is: the temperature of step (1) described diazo-reaction is controlled by temperature controller, when the reaction temperature in diazonium bucket is super
The temperature controller of diazonium bucket issues alarm when crossing 5 DEG C, and is automatically stopped the dropwise addition of sodium nitrite, is automatically added to from trash ice pipeline
Trash ice.
4. a kind of technical process for producing high light-fast fastness, high durable fastness pigment yellow 74 according to claim 2, special
Sign is: step (1) diazo-reaction is in terms of 2- methoxyl group -4- nitroaniline, reaction conversion ratio 95%, and yield is
95%。
5. a kind of technical process for producing high light-fast fastness, high durable fastness pigment yellow 74 according to claim 1, special
Sign is: step (2) the acid out time is 3h, and pH value adjustment is between 7 ~ 7.5, and temperature is controlled at 25 DEG C.
6. a kind of technical process for producing high light-fast fastness, high durable fastness pigment yellow 74 according to claim 1, special
Sign is: step (2) the coupling reaction control carries out under 20 ~ 25 DEG C of tiny structure, reaction time 3h, coupling reaction mistake
Cheng Zhongyong acetic acid head tank tune pH value, terminal pH value are 6.
7. a kind of technical process for producing high light-fast fastness, high durable fastness pigment yellow 74 according to claim 1, special
Sign is: the raw material of step (2) described emulsifier includes following component by mass parts: 45 ~ 50 parts of monohydric alcohol, hexamethylene diisocyanate
55 ~ 60 parts, 250 ~ 260 parts of polyethylene glycol, 0.001 ~ 0.003 part of dibutyltin diacetate, 300 ~ 350 parts of deionized water.
8. a kind of technical process for producing high light-fast fastness, high durable fastness pigment yellow 74 according to claim 1, special
Sign is: the feeding temperature that the filter cake in step (3) described subtractive process is sent into belt machine is set as 110 ~ 120 DEG C, out material temperature
Degree is set as 60 ~ 80 DEG C.
9. a kind of technical process for producing high light-fast fastness, high durable fastness pigment yellow 74 according to claim 1, special
Sign is: the drying time of filter cake drying in belt machine in step (3) described subtractive process is 1.5h.
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Citations (6)
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| CN1429864A (en) * | 2001-12-03 | 2003-07-16 | 东洋油墨制造株式会社 | Pigment yellow 74 and printing ink composition |
| CN1926199A (en) * | 2004-03-01 | 2007-03-07 | 科莱恩产品（德国）有限公司 | Use of a pigment composition comprising mixed crystals based on CI pigment yellow 74 |
| CN103160145A (en) * | 2013-03-12 | 2013-06-19 | 浙江迪邦化工有限公司 | Method and device for automatic-control continuous production of dye |
| CN107446109A (en) * | 2017-08-09 | 2017-12-08 | 扬州辰鑫新材料科技有限公司 | Improve emulsifying agent, its preparation method and aqueous fluorescent dispersible pigment color paste comprising the emulsifying agent of pigment compatibility and preparation method thereof |
| CN107746612A (en) * | 2017-10-31 | 2018-03-02 | 中海油常州涂料化工研究院有限公司 | A kind of preparation method of water-based thickener |
| CN108559299A (en) * | 2018-05-21 | 2018-09-21 | 杭州红妍颜料化工有限公司 | A kind of preparation method of C.I. pigment yellows 74 |
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2019
- 2019-04-30 CN CN201910364720.9A patent/CN110128845A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1429864A (en) * | 2001-12-03 | 2003-07-16 | 东洋油墨制造株式会社 | Pigment yellow 74 and printing ink composition |
| CN1926199A (en) * | 2004-03-01 | 2007-03-07 | 科莱恩产品（德国）有限公司 | Use of a pigment composition comprising mixed crystals based on CI pigment yellow 74 |
| CN103160145A (en) * | 2013-03-12 | 2013-06-19 | 浙江迪邦化工有限公司 | Method and device for automatic-control continuous production of dye |
| CN107446109A (en) * | 2017-08-09 | 2017-12-08 | 扬州辰鑫新材料科技有限公司 | Improve emulsifying agent, its preparation method and aqueous fluorescent dispersible pigment color paste comprising the emulsifying agent of pigment compatibility and preparation method thereof |
| CN107746612A (en) * | 2017-10-31 | 2018-03-02 | 中海油常州涂料化工研究院有限公司 | A kind of preparation method of water-based thickener |
| CN108559299A (en) * | 2018-05-21 | 2018-09-21 | 杭州红妍颜料化工有限公司 | A kind of preparation method of C.I. pigment yellows 74 |
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