CN107383934A - A kind of reactive brilliant bule KE GN preparation method - Google Patents
A kind of reactive brilliant bule KE GN preparation method Download PDFInfo
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- CN107383934A CN107383934A CN201710600657.5A CN201710600657A CN107383934A CN 107383934 A CN107383934 A CN 107383934A CN 201710600657 A CN201710600657 A CN 201710600657A CN 107383934 A CN107383934 A CN 107383934A
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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
- C09B62/00—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves
- C09B62/02—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group directly attached to a heterocyclic ring
- C09B62/04—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group directly attached to a heterocyclic ring to a triazine ring
- C09B62/046—Specific dyes not provided for in group C09B62/06 - C09B62/10
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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
- C09B62/00—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves
- C09B62/44—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group not directly attached to a heterocyclic ring
- C09B62/4401—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group not directly attached to a heterocyclic ring with two or more reactive groups at least one of them being directly attached to a heterocyclic system and at least one of them being directly attached to a non-heterocyclic system
- C09B62/4403—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group not directly attached to a heterocyclic ring with two or more reactive groups at least one of them being directly attached to a heterocyclic system and at least one of them being directly attached to a non-heterocyclic system the heterocyclic system being a triazine ring
- C09B62/4405—Dioxazine dyes
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of reactive brilliant bule KE GN preparation method, comprise the following steps：First p-aminobenzene sulfonic acid is added in sodium hydroxide solution, is cooled down after heating stirring dissolving, is sequentially added hydrochloric acid solution and deionization, be stirred to obtain reaction solution A；Added to after natrium nitrosum is dissolved in deionized water in reaction solution A, stirring reaction obtains reaction solution B；By N, the aminobenzaldehyde of N dimethyl 4 is with after reaction solution B reactions, adding reducing agent, reacting to obtain reaction liquid C；Anhydrous cupric sulfate is added in reaction liquid C, heating response obtains reaction solution D after adjusting pH value；After Cyanuric Chloride and reaction solution D reactions, filtering is stood, precipitation is drying to obtain.Preparation technology of the present invention is simple, and preparation condition is gentle, and raw material is common to be easy to get, and has product yield high, the advantages of cost is low is prepared, gained reactive brilliant bule KE GN solubility is high, and high-temperature stability is excellent, and degree of fixation is high, color fastness is high, complies fully with national standard, is worthy to be popularized.
Description
Technical field
The present invention relates to reactive dye preparing technical field, more particularly to a kind of reactive brilliant bule KE-GN preparation method.
Background technology
Reactive dye are also known as chemically-reactive dyes, the dye in dyeing with fiber chemically reactive.This kind of dyestuff point
Containing the group that can be chemically reacted with fiber in son, dyestuff and fiber-reactive, form therebetween covalent bond during dyeing, into
For entirety, improve washable and fastness to rubbing.Reactive dye are a kind of new dyes.Reactive dyestuff molecule includes parent dye
With two chief components of active group, active group can be referred to as with the group of fiber-reactive.
Reactive brilliant bule KE-GN is one kind in reactive dye, and its outward appearance is blue particle or uniform powder, soluble in water.
Reactive brilliant bule KE-GN is mainly used in dyeing and the stamp of the fabrics such as cotton, fiber crops, silk and soft adhesive fabric, can be used for polyester cotton, wash/
The bath method dye of viscous blending.Reactive brilliant bule KE-GN preparation method is in the prior art：With the chloro- 5- nitrobenzene-sulfonic acids of 2-, second two
Amine, tetrachloroquinone, Cyanuric Chloride and metanilic acid are raw material.The chloro- 5- nitrobenzene-sulfonic acids of 2- and ethylenediamine are condensed first,
Its nitro is reduced again；Then [mouth evil] piperazine intermediate is condensed with tetrachloroquinone；Itself and Cyanuric Chloride are condensed again, finally with
Metanilic acid is condensed to obtain product；Through saltouing, filtering, dry finished product.Above-mentioned preparation method, exists and prepares product yield
Low, the product solubility of gained is poor, and poor high temperature stability, degree of fixation is low, and a large amount of pollutions are also easy to produce in preparation process, to environment
Cause serious harm, the material such as heavy metal and harmful aromatic amine is exceeded in products obtained therefrom, does not meet national standard.Based on above-mentioned
Statement, the present invention propose a kind of reactive brilliant bule KE-GN preparation method.
The content of the invention
The invention aims to solve shortcoming present in prior art, and a kind of reactive brilliant bule KE-GN proposed
Preparation method.
A kind of reactive brilliant bule KE-GN preparation method, comprises the following steps：
S1, p-aminobenzene sulfonic acid is added in sodium hydroxide solution, is heated to 35~62 DEG C, in heating with 220~280r/
Min rotating speed stirs to after being completely dissolved to obtain lysate, and lysate is cooled into -5~0 DEG C, hydrochloric acid solution is added, is stirred
After 10~20min, deionization is added, continues to be stirred 10~20min, obtains reaction solution A；
S2, under conditions of 0~5 DEG C, natrium nitrosum is dissolved in deionized water, obtains mixed liquor, then takes part mixed liquor to delay
It is slow to add in step S1 in the reaction solution A of gained, keep the rotating speed in step S1 constant, after 18~25min of stirring reaction, obtain instead
Answer liquid B；
S3, by N, the reaction solution B of N- dimethyl -4- aminobenzaldehydes and gained in step S2 is stirred under conditions of 88~104 DEG C
After mixing 1~2h of reaction, reducing agent is added, continues 20~30min of reaction, obtains reaction liquid C；
S4, in mass ratio 1:5.3~6.5, anhydrous cupric sulfate is added in step S3 in the reaction liquid C of gained, adjusts pH value
For 4.8~6.3, and 55~85 DEG C are heated to, after reacting 30~50min, obtain reaction solution D；
S5, in mass ratio 1:3.2~4.9, Cyanuric Chloride is added in step S4 in the reaction solution D of gained, at 10~22 DEG C
Under conditions of, after 30~50min of stirring reaction, stand filtering, then cooling separate out, by precipitate drying to moisture content 0~
0.6%, produce reactive brilliant bule KE-GN.
Preferably, the mass ratio of the p-aminobenzene sulfonic acid in the step S1 and sodium hydroxide solution is 1:4~5.2.
Preferably, the addition of hydrochloric acid solution is 0.2~0.28 times of lysate total amount in the step S1, deionized water
Addition be 0.72~0.85 times of lysate total amount.
Preferably, the concentration of sodium hydroxide solution is 4~8% in the step S1, and the concentration of hydrochloric acid solution is 34~40%.
Preferably, the step S2 Sodium Nitrites and the mass ratio of deionized water are 1:6.5~8.
Preferably, the addition of part mixed liquor is 0.24~0.32 times of reaction solution A total amounts in the step S2.
Preferably, the reducing agent in the step S3 is one kind in sodium hydrogensulfite or sodium pyrosulfite.
A kind of reactive brilliant bule KE-GN proposed by the present invention preparation method, preparation technology is simple, and preparation condition is gentle, former
Expect it is common be easy to get, for preparing reactive brilliant bule KE-GN, have product yield high, prepare the advantages of cost is low, gained reactive brilliant bule
KE-GN solubility is high, and high-temperature stability is excellent, and degree of fixation is high, and color fastness is high, its coloured light and the harmful aromatic amine, the huge sum of money that include
Category content complies fully with national standard, effectively solves in the prior art, reactive brilliant bule KE-GN product yields are low, solubility
Difference, poor high temperature stability, degree of fixation is low, and a large amount of pollutions are also easy to produce in preparation process, and serious harm, gained production are caused to environment
The material such as heavy metal and harmful aromatic amine is exceeded in product, the defects of not meeting national standard, preparation process disposal of pollutants of the present invention
It is few, it is environmentally friendly, it is adapted to industrialized production, is worthy to be popularized.
Embodiment
The present invention is made with reference to specific embodiment further to explain.
Embodiment one
A kind of reactive brilliant bule KE-GN proposed by the present invention preparation method, comprises the following steps：
S1, in mass ratio 1:5.2, p-aminobenzene sulfonic acid is added in the sodium hydroxide solution that concentration is 8%, is heated to 62 DEG C,
Lysate is stirred to after being completely dissolved to obtain with 280r/min rotating speed in heating, lysate is cooled to 0 DEG C, adds lysate
0.28 times of concentration of total amount is 40% hydrochloric acid solution, after being stirred 20min, adds 0.85 times of lysate total amount and goes
Ion, continue to be stirred 20min, obtain reaction solution A；
S2, under conditions of 5 DEG C, in mass ratio 1:8, natrium nitrosum is dissolved in deionized water, obtains mixed liquor, then negating should
The mixed liquor of 0.32 times of liquid A total amounts is added slowly in step S1 in the reaction solution A of gained, keeps the rotating speed in step S1 constant,
After stirring reaction 25min, reaction solution B is obtained；
S3, by N, for the reaction solution B of N- dimethyl -4- aminobenzaldehydes and gained in step S2 under conditions of 104 DEG C, stirring is anti-
After answering 2h, sodium hydrogensulfite is added, continues to react 30min, obtains reaction liquid C；
S4, in mass ratio 1:6.5, anhydrous cupric sulfate is added in step S3 in the reaction liquid C of gained, regulation pH value is 6.3,
And 85 DEG C are heated to, after reacting 50min, obtain reaction solution D；
S5, in mass ratio 1:4.9, Cyanuric Chloride is added in step S4 in the reaction solution D of gained, under conditions of 22 DEG C,
After stirring reaction 50min, filtering is stood, then cooling separates out, and by precipitate drying to moisture content 0.6%, produces reactive brilliant bule
KE-GN。
Embodiment two
A kind of reactive brilliant bule KE-GN proposed by the present invention preparation method, comprises the following steps：
S1, in mass ratio 1:4.6, p-aminobenzene sulfonic acid is added in the sodium hydroxide solution that concentration is 6%, is heated to 48 DEG C,
Lysate is stirred to after being completely dissolved to obtain with 250r/min rotating speed in heating, lysate is cooled to -3 DEG C, adds dissolving
0.24 times of concentration of liquid total amount is 37% hydrochloric acid solution, after being stirred 15min, adds 0.78 times of lysate total amount
Deionization, continue to be stirred 15min, obtain reaction solution A；
S2, under conditions of 3 DEG C, in mass ratio 1:7.2, natrium nitrosum is dissolved in deionized water, mixed liquor is obtained, then negates
The mixed liquor of 0.28 times of liquid A total amounts is answered to be added slowly in step S1 in the reaction solution A of gained, the rotating speed in holding step S1 is not
Become, after stirring reaction 22min, obtain reaction solution B；
S3, by N, for the reaction solution B of N- dimethyl -4- aminobenzaldehydes and gained in step S2 under conditions of 95 DEG C, stirring is anti-
After answering 1.5h, sodium pyrosulfite is added, continues to react 25min, obtains reaction liquid C；
S4, in mass ratio 1:5.8, anhydrous cupric sulfate is added in step S3 in the reaction liquid C of gained, regulation pH value is 5.5,
And 70 DEG C are heated to, after reacting 40min, obtain reaction solution D；
S5, in mass ratio 1:4, Cyanuric Chloride is added in step S4 in the reaction solution D of gained, under conditions of 16 DEG C, stirred
After mixing reaction 40min, filtering is stood, then cooling separates out, and by precipitate drying to moisture content 0.3%, produces reactive brilliant bule KE-
GN。
Embodiment three
A kind of reactive brilliant bule KE-GN proposed by the present invention preparation method, comprises the following steps：
S1, in mass ratio 1:4, p-aminobenzene sulfonic acid is added in the sodium hydroxide solution that concentration is 4%, is heated to 35 DEG C, side
Lysate is stirred to after being completely dissolved to obtain in heating side with 220r/min rotating speed, and lysate is cooled into -5 DEG C, adds lysate
0.2 times of concentration of total amount is 34% hydrochloric acid solution, after being stirred 10min, add 0.72 times of lysate total amount go from
Son, continue to be stirred 10min, obtain reaction solution A；
S2, under conditions of 0 DEG C, in mass ratio 1:6.5, natrium nitrosum is dissolved in deionized water, mixed liquor is obtained, then negates
The mixed liquor of 0.24 times of liquid A total amounts is answered to be added slowly in step S1 in the reaction solution A of gained, the rotating speed in holding step S1 is not
Become, after stirring reaction 18min, obtain reaction solution B；
S3, by N, for the reaction solution B of N- dimethyl -4- aminobenzaldehydes and gained in step S2 under conditions of 88 DEG C, stirring is anti-
After answering 1h, sodium hydrogensulfite is added, continues to react 20min, obtains reaction liquid C；
S4, in mass ratio 1:5.3, anhydrous cupric sulfate is added in step S3 in the reaction liquid C of gained, regulation pH value is 4.8,
And 55 DEG C are heated to, after reacting 30min, obtain reaction solution D；
S5, in mass ratio 1:3.2, Cyanuric Chloride is added in step S4 in the reaction solution D of gained, under conditions of 10 DEG C,
After stirring reaction 30min, filtering is stood, then cooling separates out, and by precipitate drying to constant weight, produces reactive brilliant bule KE-GN.
Test in the embodiment of the present invention one~tri- the reactive brilliant bule KE-GN capability and performance prepared respectively, and with it is commercially available
Certain reactive brilliant bule KE-GN（Make to ratio）It is compared, draws following result：
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, it is any
Those familiar with the art the invention discloses technical scope in, technique according to the invention scheme and its invention
Design is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (7)
1. a kind of reactive brilliant bule KE-GN preparation method, it is characterised in that comprise the following steps：
S1, p-aminobenzene sulfonic acid is added in sodium hydroxide solution, is heated to 35~62 DEG C, in heating with 220~280r/
Min rotating speed stirs to after being completely dissolved to obtain lysate, and lysate is cooled into -5~0 DEG C, hydrochloric acid solution is added, is stirred
After 10~20min, deionization is added, continues to be stirred 10~20min, obtains reaction solution A；
S2, under conditions of 0~5 DEG C, natrium nitrosum is dissolved in deionized water, obtains mixed liquor, then takes part mixed liquor to delay
It is slow to add in step S1 in the reaction solution A of gained, keep the rotating speed in step S1 constant, after 18~25min of stirring reaction, obtain instead
Answer liquid B；
S3, by N, the reaction solution B of N- dimethyl -4- aminobenzaldehydes and gained in step S2 is stirred under conditions of 88~104 DEG C
After mixing 1~2h of reaction, reducing agent is added, continues 20~30min of reaction, obtains reaction liquid C；
S4, in mass ratio 1:5.3~6.5, anhydrous cupric sulfate is added in step S3 in the reaction liquid C of gained, adjusts pH value
For 4.8~6.3, and 55~85 DEG C are heated to, after reacting 30~50min, obtain reaction solution D；
S5, in mass ratio 1:3.2~4.9, Cyanuric Chloride is added in step S4 in the reaction solution D of gained, at 10~22 DEG C
Under conditions of, after 30~50min of stirring reaction, stand filtering, then cooling separate out, by precipitate drying to moisture content 0~
0.6%, produce reactive brilliant bule KE-GN.
2. a kind of reactive brilliant bule KE-GN according to claim 1 preparation method, it is characterised in that in the step S1
P-aminobenzene sulfonic acid and sodium hydroxide solution mass ratio be 1:4~5.2.
3. a kind of reactive brilliant bule KE-GN according to claim 1 preparation method, it is characterised in that in the step S1
The addition of hydrochloric acid solution is 0.2~0.28 times of lysate total amount, and the addition of deionized water is the 0.72 of lysate total amount
~0.85 times.
4. a kind of reactive brilliant bule KE-GN according to claim 1 preparation method, it is characterised in that in the step S1
The concentration of sodium hydroxide solution is 4~8%, and the concentration of hydrochloric acid solution is 34~40%.
5. a kind of reactive brilliant bule KE-GN according to claim 1 preparation method, it is characterised in that in the step S2
Natrium nitrosum and the mass ratio of deionized water are 1:6.5~8.
6. a kind of reactive brilliant bule KE-GN according to claim 1 preparation method, it is characterised in that in the step S2
The addition of part mixed liquor is 0.24~0.32 times of reaction solution A total amounts.
7. a kind of reactive brilliant bule KE-GN according to claim 1 preparation method, it is characterised in that in the step S3
Reducing agent be one kind in sodium hydrogensulfite or sodium pyrosulfite.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710600657.5A CN107383934A (en) | 2017-07-21 | 2017-07-21 | A kind of reactive brilliant bule KE GN preparation method |
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| CN201710600657.5A CN107383934A (en) | 2017-07-21 | 2017-07-21 | A kind of reactive brilliant bule KE GN preparation method |
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Application publication date: 20171124 |