CN109971203A - A kind of preparation method of pigment lemon yellow - Google Patents

A kind of preparation method of pigment lemon yellow Download PDF

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Publication number
CN109971203A
CN109971203A CN201910333242.5A CN201910333242A CN109971203A CN 109971203 A CN109971203 A CN 109971203A CN 201910333242 A CN201910333242 A CN 201910333242A CN 109971203 A CN109971203 A CN 109971203A
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temperature
solution
parts
concentration
lemon yellow
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徐全文
韩金龙
周兆秋
梁铁钢
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SHENZHEN RESEARCH INSTITUTE OF PHOTOGRAPHIC MATERIALS & CHEMICAL INDUSTRY
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SHENZHEN RESEARCH INSTITUTE OF PHOTOGRAPHIC MATERIALS & CHEMICAL INDUSTRY
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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
    • C09B29/34—Monoazo dyes prepared by diazotising and coupling from other coupling components
    • C09B29/36—Monoazo dyes prepared by diazotising and coupling from other coupling components from heterocyclic compounds
    • C09B29/3604—Monoazo dyes prepared by diazotising and coupling from other coupling components from heterocyclic compounds containing only a nitrogen as heteroatom
    • C09B29/3647—Monoazo dyes prepared by diazotising and coupling from other coupling components from heterocyclic compounds containing only a nitrogen as heteroatom containing a five-membered ring with two nitrogen atoms as heteroatoms
    • C09B29/3652—Monoazo dyes prepared by diazotising and coupling from other coupling components from heterocyclic compounds containing only a nitrogen as heteroatom containing a five-membered ring with two nitrogen atoms as heteroatoms containing a 1,2-diazoles or hydrogenated 1,2-diazoles
    • C09B29/366—Monoazo dyes prepared by diazotising and coupling from other coupling components from heterocyclic compounds containing only a nitrogen as heteroatom containing a five-membered ring with two nitrogen atoms as heteroatoms containing a 1,2-diazoles or hydrogenated 1,2-diazoles containing hydroxy-1,2-diazoles, e.g. pyrazolone

Abstract

The present invention relates to a kind of preparation methods of pigment lemon yellow, belong to technical field of food additives.The pigment lemon yellow is synthesized in water by p-aminobenzene sulfonic acid, DMAS and phase transfer catalyst, is made up of refrigerated separation；Method particularly includes: 1. prepare diazo liquid by diazo-reaction；2. phase transfer catalyst and sodium carbonate solid are added into above-mentioned diazo liquid, it is completed at the same time condensation and coupling reaction；3. continuing to add sodium carbonate solid into above-mentioned reaction solution, hydrolyzate PH=7 is finally obtained；4. hydrolyzate is cooled to 1~5 DEG C, 1h is stirred, a large amount of yellow solids are precipitated, the sodium chloride in filtering removal solution obtains filter cake；5. filter cake methanol eddy is beaten 1h, filtration drying obtains product pigment lemon yellow.The present invention not only shortens the time of second part of diazonium salt of preparation and coupling reaction, but also has effectively promoted condensation reaction progress, and obtained pigment lemon yellow product purity is high.

Description

A kind of preparation method of pigment lemon yellow
Technical field
The invention belongs to technical field of food additives, and in particular to a kind of preparation method of pigment lemon yellow.
Background technique
Lemon yellow is also known as tartrazines, is a kind of the most frequently used in the world, widest edible color for water-soluble synthetic dyestuff Element is also widely used in cake in addition to applying in terms of food, food, beverage, with high security, it is substantially nontoxic the features such as, Colorant as cosmetics, wool, the dyeing of cicada silk and manufacture color lake.Common synthesis technology domestic at present is: (1) diazonium Coupling reaction (4) hydrolysis of (3) second parts of diazonium salts of condensation reaction and condensation product of preparation (2) diazonium salt and DMAS of salt is anti- It answers.The above-mentioned synthesis technology time is longer, and total time is 28 small left and right, and energy consumption is larger in large-scale production, and desalination after synthesis It is more difficult, the discharge of waste acid liquor is easily caused, treatment cost of waste liquor is increased.It looks for more efficient, more environmentally friendly synthesis and removes Salt method has become the development trend for preparing pigment lemon yellow.
Summary of the invention
Of the existing technology in order to solve the problems, such as, the present invention provides a kind of preparation methods of pigment lemon yellow.Purpose It is to select simple synthetic route and uses effective desalination method, while shortening the reaction time, prepares a kind of pure The pigment lemon yellow that degree is high, yield is high, can effectively improve combined coefficient.
The present invention provides a kind of pigment lemon yellow and is synthesized in water by p-aminobenzene sulfonic acid, DMAS, consisting of phase-transferring agent, by cold But separation is made；The preparation method of pigment lemon yellow is specific as follows:
A kind of preparation method of pigment lemon yellow of the present invention, the pigment lemon yellow is by p-aminobenzene sulfonic acid, DMAS and phase Transfer catalyst synthesizes in water, is made up of refrigerated separation；Specific preparation method carries out in accordance with the following steps:
(1) diazo-reaction
According to quality meter, 1 part of p-aminobenzene sulfonic acid, 8 parts of water, the sodium hydroxide solution that 0.29 part of concentration is 40% is put into In reactor with agitating device, after 17~35 DEG C, solution clarification uniformly, temperature is reduced to 5~12 DEG C, adds for temperature control Enter the hydrochloric acid solution that 1.74 parts~1.88 parts concentration are 36~38% and 1.33 parts of sodium nitrite solutions that concentration is 30%, keeps the temperature 1.0~2.5h, tune prepare diazo liquid；
(2) condensation and coupling reaction
0.55 part~0.65 part DMAS, 0.36 part~0.51 portion phase transfer catalyst, temperature are added into above-mentioned diazo liquid 11~18 DEG C are increased to, sodium carbonate solid is then constantly added into mixed solution, until PH=5~6 are constant；Then it keeps the temperature 1h is completed at the same time condensation and coupling reaction；
(3) it hydrolyzes
Continue to add sodium carbonate solid into above-mentioned reaction solution, until PH reaches 9~10, temperature is increased to 80~86 DEG C, 1~3h is kept the temperature, hydrolyzate PH=7 is finally obtained；
(4) cooling and desalting
Hydrolyzate is cooled to 1~5 DEG C, stirs 1~2h, a large amount of yellow solids are precipitated, the chlorination in filtering removal solution Sodium obtains filter cake；
(5) methanol eddy cleans
The filter cake methanol eddy that 3.43 parts of density are 0.79 is beaten 1~4h, filtration drying obtains product pigment lemon It is yellow.
Preferably, the pigment lemon yellow is synthesized in water by p-aminobenzene sulfonic acid, DMAS and phase transfer catalyst, is passed through Refrigerated separation is made；Specific preparation method carries out in accordance with the following steps:
(1) diazo-reaction
According to quality meter, 1 part of p-aminobenzene sulfonic acid, 8 parts of water, the sodium hydroxide solution that 0.29 part of concentration is 40% is put into In reactor with agitating device, temperature control is at 25 DEG C, and after solution clarification is uniform, temperature is reduced to 8 DEG C, is added 1.88 parts 1.33 parts of sodium nitrite solutions that the hydrochloric acid solution and concentration that concentration is 36~38% are 30% keep the temperature 1.0~1.5h, modulation Standby diazo liquid out；
(2) condensation and coupling reaction
0.65 part of DMAS is added into above-mentioned diazo liquid, 0.36 part of 4 bromide, temperature is increased to 18 DEG C, then to Sodium carbonate solid is constantly added in system, until PH=6 is constant；Then 1h is kept the temperature, condensation and coupling reaction are completed at the same time；
(3) it hydrolyzes
Continue to add sodium carbonate solid into above-mentioned reaction solution, until PH reaches 9.5；Temperature is increased to 84 DEG C, keeps the temperature 3h, Finally obtain hydrolyzate PH=7；
(4) cooling and desalting
Hydrolyzate is cooled to 3 DEG C, stirs 1.0h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution obtains To filter cake；
(5) methanol eddy cleans
3.43 parts of methanol eddies of filter cake are beaten 1h, filtration drying obtains product pigment lemon yellow.
Preferably, in the preparation method step:
(1) diazo-reaction
1 part of p-aminobenzene sulfonic acid, 8 parts of water, the sodium hydroxide solution investment that 0.29 part of concentration is 40% is with stirring dress In the reactor set, temperature control is at 35 DEG C, and after solution clarification is uniform, temperature is reduced to 12 DEG C, and it is 36 that 1.74 parts of concentration, which are added, The sodium nitrite solution that~38% hydrochloric acid solution and 1.33 parts of concentration are 30%, keeps the temperature 1.5~2.0h, and tune prepares diazonium Liquid；
(2) condensation and coupling reaction
0.55 part of DMAS, 0.43 part of tri-n-octyl methyl ammonium chloride are added into above-mentioned diazo liquid, temperature is increased to 13 DEG C, so Sodium carbonate solid is constantly added in backward system, until PH=6 is constant；Then 1h is kept the temperature, condensation is completed at the same time and coupling is anti- It answers；
(3) it hydrolyzes
Continue to add sodium carbonate solid into above-mentioned reaction solution, until PH reaches 9, temperature is increased to 80 DEG C, keeps the temperature 2h, most Hydrolyzate PH=7 is obtained eventually；
(4) cooling and desalting
Hydrolyzate is cooled to 1 DEG C, stirs 1.5h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution obtains To filter cake；
(5) methanol eddy cleans
3.43 parts of methanol eddies of filter cake are beaten 2.5h, filtration drying obtains product pigment lemon yellow.
Preferably, in the preparation method step:
(1) diazo-reaction
1 part of p-aminobenzene sulfonic acid, 8 parts of water, 0.29 part of concentration is that 40% sodium hydroxide solution investment has agitating device Reactor in, temperature control is at 17 DEG C, and after solution clarification is uniform, temperature is reduced to 5 DEG C, be added 1.81 parts of concentration be 36~ The sodium nitrite solution that 38% hydrochloric acid solution and 1.33 parts of concentration are 30%, keeps the temperature 2.0~2.5h, and tune prepares diazo liquid；
(2) condensation and coupling reaction
0.61 part of DMAS is added into above-mentioned diazo liquid, 0.51 part of tetrabutylammonium chloride, temperature is increased to 11 DEG C, then to Sodium carbonate solid is constantly added in mixed liquor, until PH=5 is constant；Then 1h is kept the temperature, condensation and coupling reaction are completed at the same time；
(3) it hydrolyzes
Continue to add sodium carbonate solid in reaction solution to stating, until PH reaches 10, temperature is increased to 86 DEG C, keeps the temperature 1h, most Hydrolyzate PH=7 is obtained eventually；
(4) cooling and desalting
Hydrolyzate is cooled to 5 DEG C, stirs 2h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution obtains Filter cake；
(5) methanol eddy cleans
3.43 parts of methanol eddies of filter cake are beaten 4h, filtration drying obtains product pigment lemon yellow.
Preferably, the phase transfer catalyst be 4 bromide, benzyltriethylammoinium chloride, tetrabutylammonium bromide, Tetrabutylammonium chloride, 4-butyl ammonium hydrogen sulfate, tri-n-octyl methyl ammonium chloride, dodecyl trimethyl ammonium chloride or myristyl three Ammonio methacrylate.
DMAS is not soluble in water, needs to react by phase transfer catalyst with water soluble salt, the phase transfer that the present invention uses Catalyst be 4 bromide, benzyltriethylammoinium chloride (TEBA), tetrabutylammonium bromide (TBAB), tetrabutylammonium chloride, In 4-butyl ammonium hydrogen sulfate, tri-n-octyl methyl ammonium chloride, dodecyl trimethyl ammonium chloride or tetradecyl trimethyl ammonium chloride One kind.
Beneficial effects of the present invention:
1. the present invention provides a kind of preparation method of pigment lemon yellow, by adjusting the pH value and reaction temperature of reaction solution Make condensation reaction and coupling reaction while carrying out, not only shortens the time of second part of diazonium salt of preparation and coupling reaction, also Effect promotes condensation reaction progress, shortens total time 10 hours or more.Synthesis efficiency is improved, is effectively shortened Synthesising reacting time saves energy consumption, more economical effective.
2. the present invention is in the synthesis process, using water as solvent, in post-processing and drying process and liquid waste processing, and nothing Strong acid or strong base solution and steam reduce waste water and exhaust gas discharge, reduce the harm of relevant operation personnel, reached environmental protection The purpose of safety.
3. by directly cooling hydrolyzate, filtering is precipitated, with most simple using the pigment lemon yellow of the method for the present invention synthesis The impurity sodium chloride contained in effective refining methd removal solution, avoids conventional UF membrane or electrodialysis desalination energy consumption is high, Processes and apparatus requires the features such as high, the problem of desalination difficulty after effective solution synthetic dyestuff lemon yellow, and obtained Pigment lemon yellow product purity is high, and yield is high, and pigment lemon yellow prepared by the present invention can be used as food grade additives use.
Specific embodiment
A kind of preparation step of the pigment lemon yellow of embodiment 1 is as follows:
(1) diazo-reaction
According to quality meter, 1 part of (69g) p-aminobenzene sulfonic acid, 8 parts of (560ml) water, 0.29 part of (20g) concentration 40% Sodium hydroxide solution investment is in the reactor of agitating device, and after 25 DEG C, solution clarification uniformly, temperature is reduced for temperature control To 8 DEG C, the hydrochloric acid solution that 1.88 parts of (130g) concentration are 36~38% and the nitrous acid that 1.33 parts of (92g) concentration is 30% is added Sodium solution, keeps the temperature 1.0~1.5h, and tune prepares diazo liquid；
Reaction equation are as follows:
(2) condensation and coupling reaction
0.65 part of (45g) DMAS, 0.36 part of (25g) 4 bromide are added into above-mentioned diazo liquid, temperature is increased to 18 DEG C, sodium carbonate solid is then constantly added into mixed liquor, until PH=6 is constant；Then 1h is kept the temperature, condensation is completed at the same time And coupling reaction；
Condensation reaction equation are as follows:
Coupling reaction equation are as follows:
(3) it hydrolyzes
Continue to add sodium carbonate solid into above-mentioned reaction solution, until PH reaches 9.5, temperature is increased to 84 DEG C, heat preservation 1.5h finally obtains hydrolyzate PH=7；
Hydrolysis equation are as follows:
(4) cooling and desalting
Hydrolyzate is cooled to 3 DEG C, stirs 1h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution obtains Filter cake；
(5) methanol eddy cleans
By filter cake with 3.43 parts (300ml), density is that 0.79 methanol eddy is beaten 1h, and filtration drying obtains product pigment Lemon yellow.Obtained pigment lemon yellow product purity is up to 99%, and total recovery 87%, liquid phase purity reaches 99%.
Embodiment 2
According to quality meter, 1 part of (69g) p-aminobenzene sulfonic acid, 8 parts of (560ml) water, 0.29 part of (20g) concentration is 40% Sodium hydroxide solution investment in the reactor of agitating device, temperature control is at 30 DEG C, after solution clarification is uniform, temperature drop Down to 9 DEG C, the hydrochloric acid solution that 1.86 parts of (128g) concentration are 36~38% is added and 1.33 parts (92g) that concentration is 30% is sub- Sodium nitrate solution keeps the temperature 1.0~1.5h, prepares diazo liquid；
(2) condensation and coupling reaction
0.62 part of (43g) DMAS, 045 part of (31g) tetrabutylammonium bromide (TBAB), temperature liter are added into above-mentioned diazo liquid Up to 16 DEG C, sodium carbonate solid is then constantly added into system, until PH=6 is constant；Then 1h is kept the temperature, contracting is completed at the same time Conjunction and coupling reaction；
(3) it hydrolyzes
Continue to add sodium carbonate solid into above-mentioned reaction solution, until PH reaches 9.5；Temperature is increased to 82 DEG C, heat preservation 1.5h finally obtains hydrolyzate PH=7；
(4) cooling and desalting
Hydrolyzate is cooled to 2 DEG C, stirs 1h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution obtains Filter cake；
(5) methanol eddy cleans
Methanol eddy impurity-removing method is identical as specific embodiment 1, and the obtained pigment lemon yellow product purity of this example is up to 99%, total recovery 87%, liquid phase purity reaches 99%.
Embodiment 3
(1) diazo-reaction
According to quality meter, 1 part of (69g) p-aminobenzene sulfonic acid, 8 parts of (560ml) water, 0.29 part of (20g) concentration 40% Sodium hydroxide solution investment is in the reactor of agitating device, and temperature control is at 35 DEG C, and after solution clarification is uniform, temperature is reduced To 12 DEG C, the hydrochloric acid solution of 1.74 parts of (120g) concentration 36~38% is added and nitrous acid that 1.33 parts of (92g) concentration are 30% Sodium solution, keeps the temperature 1.5~2.0h, and tune prepares diazo liquid；
(2) condensation and coupling reaction
0.55 part of (38g) DMAS, 0.43 part of (30g) tri-n-octyl methyl ammonium chloride, temperature liter are added into above-mentioned diazo liquid Up to 13 DEG C, sodium carbonate solid is then constantly added into mixed liquor, control PH=6 reaction is constant；Then 1h is kept the temperature, simultaneously Complete condensation and coupling reaction；
(3) it hydrolyzes
Continue to add sodium carbonate solid into above-mentioned reaction solution, until PH reaches 9, temperature is increased to 80 DEG C, keeps the temperature 2h, most Hydrolyzate PH=7 is obtained eventually；
(4) cooling and desalting
Hydrolyzate is cooled to 1 DEG C, stirs 1.5h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution obtains To filter cake；
Methanol eddy impurity-removing method is identical as specific embodiment 1, and the obtained pigment lemon yellow product purity of this example is up to 99%, total recovery 87%, liquid phase purity reaches 99%.
Embodiment 4
(1) diazo-reaction
According to quality meter, 1 part of (69g) p-aminobenzene sulfonic acid, 8 parts of (560ml) water, 0.29 part of (20g) concentration is 40% Sodium hydroxide solution investment in the reactor of agitating device, temperature control is at 17 DEG C, after solution clarification is uniform, temperature drop Down to 5 DEG C, the hydrochloric acid solution that 1.81 parts of (125g) concentration are 36~38% and the nitrous that 1.33 parts of (92g) concentration is 30% is added Acid sodium solution, keeps the temperature 2.0~2.5h, and tune prepares diazo liquid；
(2) condensation and coupling reaction
0.61 part of (42g) DMAS, 0.51 part of (35g) tetrabutylammonium chloride are added into above-mentioned diazo liquid, temperature is increased to 11 DEG C, then constantly add sodium carbonate solid into system, control PH=5 is constant, then keeps the temperature 1h, be completed at the same time condensation and Coupling reaction；
(3) it hydrolyzes
It answers and continues to add 30g (numerical value 30g should be deleted) sodium carbonate solid in liquid, until PH reaches 10, temperature is increased to 86 DEG C, 1.0h is kept the temperature, hydrolyzate PH=7 is finally obtained；
(4) cooling and desalting
Hydrolyzate is cooled to 5 DEG C, stirs 2h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution obtains Filter cake；
Methanol eddy impurity-removing method is identical as specific embodiment 1, the finally obtained pigment lemon yellow product purity of this example Up to 99%, total recovery 85%, liquid phase purity reaches 99%.
Embodiment 5
This example is unlike the first embodiment: in this example
(1) diazo-reaction
According to quality meter, 1 part of (69g) p-aminobenzene sulfonic acid, 8 parts of (560ml) water, 0.29 part of (20g) concentration is 40% Sodium hydroxide solution investment in the reactor of agitating device, temperature control is at 20 DEG C, after solution clarification is uniform, temperature drop Down to 10 DEG C, the hydrochloric acid solution that 1.86 parts of (128g) concentration are 36~38% and the Asia that 1.33 parts of (92g) concentration is 30% is added Sodium nitrate solution, keeps the temperature 1.5~2.0h, and tune prepares diazo liquid；
(2) condensation and coupling reaction
0.43 part of (40g) DMAS, 0.45 part of (31g) 4-butyl ammonium hydrogen sulfate are added into above-mentioned diazo liquid, temperature increases To 15 DEG C, sodium carbonate solid is then constantly added into system, control PH=6 is constant, then keeps the temperature 1h, is completed at the same time condensation And coupling reaction；
(3) it hydrolyzes
It answers and continues to add sodium carbonate solid in liquid, until PH reaches 9~10, temperature is increased to 85 DEG C, keeps the temperature 1.5h, finally Obtain hydrolyzate PH=7；
(4) cooling and desalting
Hydrolyzate is cooled to 4 DEG C, stirs 1h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution obtains Filter cake；
Methanol eddy impurity-removing method is identical as specific embodiment 1, the finally obtained pigment lemon yellow product purity of this example Up to 99%, total recovery 85%, liquid phase purity reaches 99%.

Claims (5)

1. a kind of preparation method of pigment lemon yellow, which is characterized in that the pigment lemon yellow by p-aminobenzene sulfonic acid, DMAS and Phase transfer catalyst synthesizes in water, is made up of refrigerated separation；Specific preparation method carries out in accordance with the following steps:
(1) diazo-reaction
According to quality meter, 1 part of p-aminobenzene sulfonic acid, 8 parts of water, the sodium hydroxide solution investment that 0.29 part of concentration is 40% is had In the reactor of agitating device, after 17~35 DEG C, solution clarification uniformly, temperature is reduced to 5~12 DEG C for temperature control, is added 1.33 parts of sodium nitrite solutions that the hydrochloric acid solution and concentration that 1.74 parts~1.88 parts concentration are 36~38% are 30%, heat preservation 1.0~2.5h, tune prepare diazo liquid；
(2) condensation and coupling reaction
0.55 part~0.65 part DMAS, 0.36 part~0.51 portion phase transfer catalyst are added into above-mentioned diazo liquid, temperature increases To 11~18 DEG C, sodium carbonate solid is then constantly added into mixed solution, until PH=5~6 are constant；Then 1h is kept the temperature, It is completed at the same time condensation and coupling reaction；
(3) it hydrolyzes
Continue to add sodium carbonate solid into above-mentioned reaction solution, until PH reaches 9~10, temperature is increased to 80~86 DEG C, heat preservation 1 ~3h finally obtains hydrolyzate PH=7；
(4) cooling and desalting
Hydrolyzate is cooled to 1~5 DEG C, stirs 1~2h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution obtains To filter cake；
(5) methanol eddy cleans
The filter cake methanol eddy that 3.43 parts of density are 0.79 is beaten 1~4h, filtration drying obtains product pigment lemon yellow.
2. a kind of preparation method of pigment lemon yellow, which is characterized in that the pigment lemon yellow by p-aminobenzene sulfonic acid, DMAS and Phase transfer catalyst synthesizes in water, is made up of refrigerated separation；Specific preparation method carries out in accordance with the following steps:
(1) diazo-reaction
According to quality meter, 1 part of p-aminobenzene sulfonic acid, 8 parts of water, the sodium hydroxide solution investment that 0.29 part of concentration is 40% is had In the reactor of agitating device, temperature control is at 25 DEG C, and after solution clarification is uniform, temperature is reduced to 8 DEG C, and 1.88 parts of concentration are added 1.33 parts of sodium nitrite solutions that hydrochloric acid solution and concentration for 36~38% are 30%, keep the temperature 1.0~1.5h, and tune is prepared Diazo liquid；
(2) condensation and coupling reaction
0.65 part of DMAS is added into above-mentioned diazo liquid, 0.36 part of 4 bromide, temperature is increased to 18 DEG C, then to system In constantly add sodium carbonate solid, until PH=6 is constant；Then 1h is kept the temperature, condensation and coupling reaction are completed at the same time；
(3) it hydrolyzes
Continue to add sodium carbonate solid into above-mentioned reaction solution, until PH reaches 9.5；Temperature is increased to 84 DEG C, keeps the temperature 3h, finally Obtain hydrolyzate PH=7；
(4) cooling and desalting
Hydrolyzate is cooled to 3 DEG C, stirs 1.0h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution is filtered Cake；
(5) methanol eddy cleans
3.43 parts of methanol eddies of filter cake are beaten 1h, filtration drying obtains product pigment lemon yellow.
3. the preparation method of pigment lemon yellow as described in claim 1, which is characterized in that in the preparation method step:
(1) diazo-reaction
1 part of p-aminobenzene sulfonic acid, 8 parts of water, the sodium hydroxide solution investment that 0.29 part of concentration is 40% is with agitating device In reactor, temperature control is at 35 DEG C, and after solution clarification is uniform, temperature is reduced to 12 DEG C, be added 1.74 parts of concentration be 36~ The sodium nitrite solution that 38% hydrochloric acid solution and 1.33 parts of concentration are 30%, keeps the temperature 1.5~2.0h, and tune prepares diazo liquid；
(2) condensation and coupling reaction
0.55 part of DMAS is added into above-mentioned diazo liquid, 0.43 part of tri-n-octyl methyl ammonium chloride, temperature is increased to 13 DEG C, then to Sodium carbonate solid is constantly added in system, until PH=6 is constant；Then 1h is kept the temperature, condensation and coupling reaction are completed at the same time；
(3) it hydrolyzes
Continue to add sodium carbonate solid into above-mentioned reaction solution, until PH reaches 9, temperature is increased to 80 DEG C, keeps the temperature 2h, final to obtain To hydrolyzate PH=7；
(4) cooling and desalting
Hydrolyzate is cooled to 1 DEG C, stirs 1.5h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution is filtered Cake；
(5) methanol eddy cleans
3.43 parts of methanol eddies of filter cake are beaten 2.5h, filtration drying obtains product pigment lemon yellow.
4. the preparation method of pigment lemon yellow as described in claim 1, it is characterised in that: in the preparation method step:
(1) diazo-reaction
1 part of p-aminobenzene sulfonic acid, 8 parts of water, 0.29 part of concentration is 40% sodium hydroxide solution investment with the anti-of agitating device It answers in device, temperature control is at 17 DEG C, and after solution clarification is uniform, temperature is reduced to 5 DEG C, and it is 36~38% salt that 1.81 parts of concentration, which are added, The sodium nitrite solution that acid solution and 1.33 parts of concentration are 30%, keeps the temperature 2.0~2.5h, and tune prepares diazo liquid；
(2) condensation and coupling reaction
0.61 part of DMAS is added into above-mentioned diazo liquid, 0.51 part of tetrabutylammonium chloride, temperature is increased to 11 DEG C, then to mixing Sodium carbonate solid is constantly added in liquid, until PH=5 is constant；Then 1h is kept the temperature, condensation and coupling reaction are completed at the same time；
(3) it hydrolyzes
Continue to add sodium carbonate solid in reaction solution to stating, until PH reaches 10, temperature is increased to 86 DEG C, keeps the temperature 1h, final to obtain To hydrolyzate PH=7；
(4) cooling and desalting
Hydrolyzate is cooled to 5 DEG C, stirs 2h, a large amount of yellow solids are precipitated, and the sodium chloride in filtering removal solution is filtered Cake；
(5) methanol eddy cleans
3.43 parts of methanol eddies of filter cake are beaten 4h, filtration drying obtains product pigment lemon yellow.
5. the preparation method of pigment lemon yellow as described in any one of Claims 1 to 4, it is characterised in that: the phase transfer catalysis (PTC) Agent is 4 bromide, benzyltriethylammoinium chloride, tetrabutylammonium bromide, tetrabutylammonium chloride, 4-butyl ammonium hydrogen sulfate, three Octylmethylammonium chloride, dodecyl trimethyl ammonium chloride or tetradecyl trimethyl ammonium chloride.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112111171A (en) * 2020-09-21 2020-12-22 恒升化工有限公司 C.I. acid yellow 23 dye and clean production process thereof

Citations (4)

* Cited by examiner, † Cited by third party
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