CN109294276A - A kind of composition of reactive dye and its preparation method and application - Google Patents
A kind of composition of reactive dye and its preparation method and application Download PDFInfo
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- CN109294276A CN109294276A CN201811329960.7A CN201811329960A CN109294276A CN 109294276 A CN109294276 A CN 109294276A CN 201811329960 A CN201811329960 A CN 201811329960A CN 109294276 A CN109294276 A CN 109294276A
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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
- C09B67/0033—Blends of pigments; Mixtured crystals; Solid solutions
- C09B67/0046—Mixtures of two or more azo dyes
- C09B67/0047—Mixtures of two or more reactive azo dyes
- C09B67/005—Mixtures of two or more reactive azo dyes all the reactive groups being not directly attached to a heterocyclic system
-
- 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
- C09B67/0033—Blends of pigments; Mixtured crystals; Solid solutions
- C09B67/0046—Mixtures of two or more azo dyes
- C09B67/0055—Mixtures of two or more disazo dyes
- C09B67/0057—Mixtures of two or more reactive disazo dyes
- C09B67/0059—Mixtures of two or more reactive disazo dyes all the reactive groups are not directly attached to a heterocyclic system
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
- D06P1/384—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes reactive group not directly attached to heterocyclic group
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/66—Natural or regenerated cellulose using reactive dyes
- D06P3/666—Natural or regenerated cellulose using reactive dyes reactive group not directly attached to heterocyclic group
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/30—Ink jet printing
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Paper (AREA)
- Coloring (AREA)
Abstract
The invention discloses a kind of reactive dye compounds, including the component A, the component B, the component C；Component B in component C structure, there is-NO2 ,-COOH ,-OH etc.；Wherein-NO2 is used to improve light fastness, and-COOH ,-OH are used to improve washing fastness, the reactive dye compound reproducibility is good, there is excellent light fastness, washing fastness, the features such as perspiration fastness, degree of fixation is high, can be used for the printing and dyeing of the fibers such as cotton, silk, polyamide and ink-jet printed.Corresponding sun-resistant, water-fastness, perspiration resistance black and active dye product can be provided according to client's needs, it is widely used.Reactive dye compound has degree of fixation high, and dye-uptake is high, and cotton good hand touch, rub resistance is water-fastness, sun-resistant, and the items fastness such as perspiration resistance is excellent.Compared to black and active dye performance on the market, every fastness is greatly promoted.
Description
Technical field
The present invention relates to reactive dye compound more particularly to a kind of composition of reactive dye and preparation method thereof and use
On the way, for printing and dyeing of the fibers such as cotton, silk, polyamide and ink-jet printed, reproducibility is good, there is excellent light fastness, washes
The features such as fastness, ozone fastness, degree of fixation is high.
Background technique
The yield of reactive dye account for entire reactive dye yield more than half.Reactive dye are as the larger color of market occupancy volume
Kind, good fastness to rubbing, washing fastness and fastness to perspiration are not only required, but also require higher fixation
Rate.However, various performance indicators are difficult to reach the requirement of people after existing reactive dye kind prints and dyes to fiber.Therefore, it opens
The reactive dye kind that sends out performance a kind of and can more preferably meet simultaneously above-mentioned characteristic requirements attracts attention and payes attention to.
Summary of the invention
The present invention is difficult to reach people to overcome existing reactive dye to exist to various performance indicators after fiber printing and dyeing
It is required that the problem of, a kind of reactive dye compound and preparation method thereof, preparation method and purposes are provided.Component B, component C structure
In have-NO2 ,-COOH ,-OH.- NO2 is used to improve ozone fastness, and-COOH ,-OH are used to improve washing fastness.The reactive dye
Composition is compounded by using these groups, greatly improves every color jail such as sun-resistant, water-fastness and perspiration resistance
Degree, and corresponding sun-resistant, water-fastness, perspiration resistance black and active dye product can be provided according to client's different demands.
The first aspect of the present invention provides a kind of compound in a kind of reactive dye compound, including chemical structural formula 1
Or the group of the component A of more than one compounds composition, one of chemical structural formula 2 compound or more than one compounds composition
A kind of component C of compound or above compound composition in point B, chemical structural formula 3, wherein X1For in hydrogen, potassium, sodium, lithium, ammonium
Any one；R1For-H or-OCH3；R2For-H ,-SO3X1、-OCH3、-CH3In any one；R3For-SO2C2H4OSO3X1；
R4For-H ,-NO2,-COOH, any one in-OH；R5For-H ,-NO2,-COOH, any one in OH；
Chemical structural formula 1:
Chemical structural formula 2:
Chemical structural formula 3:
Further, according to the parts by weight meter of the reactive dye compound, component A content is 30-80 parts by weight, group
Part B content is 5-20 parts by weight, and component C content is 10-30 parts by weight.
Further, providing the component A includes one of chemical structural formula 1-1~chemical structural formula 1-5 compound
Or it is a variety of；
Chemical structural formula 1-1:
Chemical structural formula 1-2:
Chemical structural formula 1-3:
Chemical structural formula 1-4:
Chemical structural formula 1-5:
The component B includes one of chemical structural formula 2-1~chemical structural formula 2-5 compound or a variety of；
Chemical structural formula 2-1:
Chemical structural formula 2-2:
Chemical structural formula 2-3:
Chemical structural formula 2-4:
Chemical structural formula 2-5:
Chemical structural formula 2-6:
The component C includes one of chemical structural formula 3-1~chemical structural formula 3-5 compound or a variety of；
Chemical structural formula 3-1:
Chemical structural formula 3-2:
Chemical structural formula 3-3:
Chemical structural formula 3-4:
Chemical structural formula 3-5:
Preferably: in above-mentioned dye composite, based on the total weight of the reactive dye, component A content is 30-80 weight
Measure part, preferably 35-75 parts by weight, more preferably 40-70 parts by weight；Component B content is 5-20 parts by weight, preferably 4-20 weight
Part, more preferably 5-20 parts by weight are measured, component C content is 10-30 parts by weight, preferably 10-28 parts by weight, more preferably 10-
25 parts by weight.
The preparation method of reactive dye compound is provided in the second aspect of the invention, including following component A, group
Divide the preparation method of B and component C:
One, component A preparation method the following steps are included:
S1: the first diazo-reaction: any one compound in structural formula Y1 is dissolved in the water, hydrochloric acid is then added
Solution is added rubble ice, adds sodium nitrite solution, in micro- blue after soaking potassium iodide starch paper, removes excessive nitrous acid
Sodium, react step S1 diazo liquid；
Structural formula Y1:
The reaction of S2: the first acid coupling
It dissolves it all, is added in the diazo liquid of step S1 and reacts, react to obtain acid coupling
Liquid；
The reaction of S3: the first alkaline coupling
The acid coupling liquid that step S2 is obtained reacts to obtain alkaline coupling liquid with the PH of alkali tune solution to neutral or alkalinity；
Up to the compound of above-mentioned chemical structural formula 1；
S4: the first purification step:
Salt is added in the resulting alkaline coupling liquid of step S3, after waiting solids to be precipitated completely, be added solid-liquid separator in into
Row separation, removes filtrate, collects filter cake, and filter cake is soluble in water, makes its mass concentration in 5-10%, the dyestuff purified is molten
Liquid；
S5: the first desalination and concentration step:
The dye solution Desalination machine that step S4 is obtained carries out desalination and concentration, is concentrated into 20-25%, it is dense to obtain dyestuff
Contracting liquid；
Two, component B preparation method the following steps are included:
S11: the second diazo-reaction: any one compound in the structural formula Y1 is dissolved in the water, then
Hydrochloric acid solution is added, rubble ice is added, makes its mass concentration 5-10%, adds sodium nitrite solution, potassium iodide starch paper leaching
Afterwards be in micro- blue, remove excessive sodium nitrite, react step S11 diazo liquid；
The reaction of S12: the second alkaline coupling:
By any one compound in structural formula Y2, it is dissolved all with aqueous slkali, is added to the diazonium of step S11
In liquid, with the tune PH of alkali tune solution to neutral or alkalinity, compound in chemical structural formula 2 is reacted to obtain；
Structural formula Y2:
S13: the second purification step:
Salt is added in the resulting dye solution of step S12, after waiting solids to be precipitated completely, is added in solid-liquid separator and carries out
Separation removes filtrate, collects filter cake, and filter cake is soluble in water, makes its mass concentration in 5-10%, the dyestuff purified is molten
Liquid；
S14: the second desalination and concentration step:
The dye solution Desalination machine that step 13 is obtained carries out desalination, is concentrated into 20-25%, obtains dye concentrated solution；
Three, the preparation method of component C, includes the following steps:
S21: third diazo-reaction:
Any one compound in structure above Y1 is dissolved in the water, hydrochloric acid solution is then added, trash ice is added
Block adds sodium nitrite solution, is in micro- blue after potassium iodide starch paper leaching, removes excessive sodium nitrite, react to obtain step S21
Diazo liquid；
S22: third alkaline coupling reaction
It dissolves it all any one compound aqueous slkali that structural formula is Y3, is added to step S21 diazo liquid
In, react to obtain alkaline coupling liquid；
Structural formula Y3:
S23: the four diazo-reaction:
Any one compound that structural formula is Y4 is dissolved in the water, hydrochloric acid solution is then added, rubble ice is added, then
It sodium nitrite solution is added, in micro- blue after soaking potassium iodide starch paper, removes excessive sodium nitrite, react to obtain step S23
Diazo liquid,
Structural formula Y4:
The reaction of S24: the four alkaline coupling
The alkaline coupling liquid that step S22 is obtained is added in the diazonium salt that step S23 is obtained, with the PH of alkali tune solution into
Property to get above-mentioned chemical structural formula 3 compound；
S25: third purification step: the salt being added in the resulting dye solution of step S24, after waiting solids to be precipitated completely,
It is added in solid-liquid separator and is separated, remove filtrate, collect filter cake；Dye solution filter cake is soluble in water, being purified；
S26 third desalination and concentration step: the dye solution Desalination machine that step S25 is obtained carries out desalination, is concentrated into
20-25% obtains dye concentrated solution.
5, the preparation method of reactive dye compound according to claim 4, is characterized in that: in the step S1
In, PH < 2 of first diazo-reaction, the reaction temperature of first diazo-reaction is 0-10 DEG C, described the
The reaction time of one diazo-reaction is 1-3 hours；
The first acid coupling described in the S2 step reaction PH < 2, temperature be 0-10 DEG C, described first
The acid coupling reaction time is 3-5 hours；
The PH=5.5-6 of the reaction of the first alkaline coupling described in the S3 step, first alkaline coupling
The reaction temperature of reaction is 10-20 DEG C, and the reaction time of the first alkaline coupling reaction is 1-3 hours；
In the S4 step, the dosage of the salt is the 10-20% of mass ratio；The salt is sodium chloride；
In the S5 step, conductivity of waste water=0.5-1ms/cm of the dye solution.
Further, in the step S11, PH < 2 of second diazo-reaction, second diazotising
The reaction temperature of reaction is 0-10 DEG C, and the reaction time of second diazo-reaction is 1-3 hours；
The second acid coupling described in the S12 step reaction PH < 2, temperature be 0-10 DEG C, described second
The acid coupling reaction time is 1-3 hours；
In the S14 step, the dosage of the salt is the 10-20% of mass ratio；The salt is sodium chloride；
In the S15 step, conductivity of waste water=0.5-1ms/cm of the dye solution.
Further, in the step S21, PH < 2 of the third diazo-reaction, the third diazotising
The reaction temperature of reaction is 0-10 DEG C, and the reaction time of the third diazo-reaction is 1-3 hours；
PH < 2 of the reaction of the third acid coupling described in the S22 step, the reaction of third acid coupling reaction
Temperature is 0-10 DEG C, and the reaction time of the third acid coupling reaction is 2-4 hours；
PH < 2 of the 4th diazo-reaction described in the S23 step, the reaction temperature of the 4th diazo-reaction
It is 0-10 DEG C, the reaction time of the 4th diazo-reaction is 1-3 hours；
The PH=5.5-6 of the reaction of the 4th alkaline coupling described in the S24 step, the 4th alkaline coupling
The reaction temperature of reaction is 0-10 DEG C, and the reaction time of the 4th alkaline coupling reaction is 1-3 hours；
In the S25 step, the dosage of the salt is the 10-20% of mass ratio；The salt is sodium chloride；
In the S26 step, conductivity of waste water=0.5-1ms/cm of the dye solution.
The third aspect of the present invention provides the purposes of above-mentioned Black reactive dye composition: by the reactive dye group
Object is closed to print and dye for fiber or fiber textile；The fiber is cotton, and synthetic cotton is numb, is appointed in regenerated fiber or its textile fabric
It anticipates one kind, the fiber textile is Fypro, cellulose fibre, any one in protein fibre or its textile fabric
Kind.
Further, the printing and dyeing are dyeing or ink-jet printed.
Reactive dye compound of the present invention has the advantage that degree of fixation height, and dye-uptake is high, cotton good hand touch, antifriction
It wipes, water-fastness, sun-resistant, the items fastness such as perspiration resistance is excellent.Compared to black and active dye performance on the market, every fastness is obtained
To greatly being promoted.Reactive dye compound of the invention is used for cotton, synthetic cotton, fiber crops, regenerated fiber or their textile fabric
It prints and dyes and ink-jet printed, or is Fypro, cellulose fibre, protein fibre or their textile fabric printing and dyeing and ink-jet
Stamp.
Detailed description of the invention
Fig. 1 is the preparation method flow chart of component A of the invention；
Fig. 2 is the preparation method flow chart of component B of the invention；
Fig. 3 is the preparation method flow chart of component C of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.Below by way of example, the present invention is described in detail, it should be appreciated that
The present invention will be described for this being given for example only property of embodiment, is not used to limit the invention.
Synthetic example 1
The compound of chemical structural formula 1-1,2-1,3-5 in following examples can comprise the following steps: following chemistry
Structural formula is respectively with a-e representative: a represents one of compound of chemical structural formula Y1；H acid when b represents component A processed
One of；C represents one of compound of chemical structural formula Y2；D represents the one of whichization of chemical structural formula Y3
Close object；E represents a kind of compound of chemical structural formula Y4.
The preparation method of chemical structural formula 1-1 in one, reactive dye component A
Step S1: following structural formula a is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes its matter
Amount concentration is 8-12%, 30% sodium nitrite solution is added, makes the pH < 2 in reaction solution, in micro- after potassium iodide starch paper leaching
Blue, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, react step S1 diazo liquid,
Step S2: being neutralized to pH=6.0-7.0 with 10%-20% sodium hydroxide solution for b, dissolves it all, is added
Into the diazo liquid of step S1, T=0-10 DEG C, 3-5h is reacted, reaction obtains acid coupling liquid described in step S2；
Step S3: being 10-20 DEG C by the adjustment temperature of acid coupling liquid described in step S2, with the pH=of soda ash tune solution
5.5-6.5 keeps the temperature 1-3h, reacts to obtain alkaline coupling liquid described in S3 step；It is molten up to the dyestuff of above-mentioned chemical structural formula 1-1
Liquid.Chemical structural formula 1-1 is as follows:
Step S4: the salt that 10-20% is added in resulting dye solution in the S3 step adds after waiting solids to be precipitated completely
Enter in solid-liquid separator and separated, remove filtrate, collects filter cake.Filter cake is soluble in water, make its mass concentration in 5-10%,
Obtain the dye solution of purification described in S4 step.
Step S5: by the dye solution Desalination machine of purification described in S4 step, desalination and concentration is carried out, conductivity of waste water is made
=0.5-1ms/cm is concentrated into concentration 20-25%, obtains dye concentrated solution.
The preparation method of chemical structural formula 2-1 in two, reactive dye component B
Step S11: by being dissolved in the water for chemical structural formula a, 30% hydrochloric acid solution is then added, rubble ice is added, makes
Its mass concentration is 8-12%, 30% sodium nitrite solution is added, makes the pH < 2 in reaction solution, after potassium iodide starch paper leaching
In micro- blue, T=0-10 DEG C, react 1-3h, remove excessive sodium nitrite with sulfamic acid, react described in step S11
Diazo liquid,
Step S12: being neutralized to pH=6.0-7.0 with 10%-20% sodium hydroxide solution for compound c, keeps it all molten
Solution, is added in diazo liquid described in step S11, with the pH=5.5-6.5 of soda ash tune solution, T=0-10 DEG C, keeps the temperature 1-
3h is to get dyestuff in structure above 2-1.The following dyestuff of structural formula:
Step S13: being added the salt of 10-20% in dye solution, after waiting solids to be precipitated completely, is added in solid-liquid separator
It is separated, removes filtrate, collect filter cake.Filter cake is soluble in water, make its mass concentration in 5-10%, the dyestuff purified
Solution.
Step S14: by dye solution Desalination machine, desalination and concentration is carried out, conductivity of waste water=0.5-1ms/cm is made, be concentrated
To 20-25%, dye concentrated solution described in step S14 is obtained.
The preparation method of three, reactive dye component chemical structural formula 3-5 dyestuffs
Step S21: compound a is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes its quality
Concentration is 8-12%, 30% sodium nitrite solution is added, the pH < 2 in reaction solution is made, is in micro- indigo plant after potassium iodide starch paper leaching
Color, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, reacts to obtain diazo liquid described in step S21,
Step S22: being neutralized to pH=6.0-7.0 with 10%-20% sodium hydroxide solution for compound d, keeps it all molten
Solution, is added in step S21 diazo liquid, T=0-10 DEG C, reacts 2-4h, reacts to obtain alkaline coupling liquid described in step S22；
Step S23: compound e is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes its quality
Concentration is 8-12%, adds 30% sodium nitrite solution, makes the pH < 2 in reaction solution, is in micro- indigo plant after potassium iodide starch paper leaching
Color, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, reacts to obtain diazo liquid described in step S22；
Step S24: alkaline coupling liquid is added in the resulting diazo liquid of step S22, with the pH=5.5- of soda ash tune solution
6.5, T=0-10 DEG C, 1-3h is kept the temperature to get the dyestuff of chemical structural formula 3-5.Chemical structural formula 3-5 is as follows:
Step S25: the salt that 10-20% is added in the resulting dye solution of step S24 adds after waiting solids to be precipitated completely
Enter in solid-liquid separator and separated, remove filtrate, collects filter cake.Filter cake is soluble in water, make its mass concentration in 5-10%,
Obtain the dye solution of the purification of step S25.
Step S26: the dye solution Desalination machine that step S25 is purified, carry out desalination and concentration, make conductivity of waste water=
0.5-1ms/cm is concentrated into 20-25%, obtains the resulting dye concentrated solution of step S26.
Synthetic example 2
The compound of chemical structural formula 1-4,2-4,3-4 in following embodiments 2 can comprise the following steps: wherein represent
One of compound of chemical structural formula Y1；One of H acid when b represents component A processed；C represents chemical structural formula
One of compound of Y2；D represents one of compound of chemical structural formula Y3；E-1 represents chemical structural formula Y4
A kind of compound.
The preparation method of chemical structural formula 1-4 in one, reactive dye component A is specific as follows:
Step S1: following structural formula a-1 is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes it
Mass concentration is 8-12%, 30% sodium nitrite solution is added, makes the pH < 2 in reaction solution, is in after potassium iodide starch paper leaching
Micro- blue, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, reacts to obtain weight described in step S14
Nitrogen liquid；Chemical structural formula 1-4 is specific as follows:
The step S2- step S5 and step S2- step S5 of synthetic example 1 is identical step in the present embodiment.
The preparation method of chemical structural formula 2-4 in two, reactive dye component B is specific as follows:
Step S11: following chemical structural formula a-1 is dissolved in the water, and 30% hydrochloric acid solution is then added, and trash ice is added
Block makes its mass concentration 8-12%, 30% sodium nitrite solution is added, the pH < 2 in reaction solution, potassium iodide examination are made
It is in micro- blue after paper leaching, T=0-10 DEG C, reacts 1-3h, removes excessive sodium nitrite with sulfamic acid, react to obtain step S11
The diazo liquid,
The S12- step S14 of step S12- step S14 and synthetic example 1 in the present embodiment are identical steps.
The preparation method of chemical structural formula 3-4 in three, reactive dye component C is specific as follows:
Step S21: compound a -1 is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes its matter
Amount concentration is 8-12%, 30% sodium nitrite solution is added, makes the pH < 2 in reaction solution, in micro- after potassium iodide starch paper leaching
Blue, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, reacts to obtain diazonium described in step S21
Liquid,
Step S22: being neutralized to pH=6.0-7.0 with 10%-20% sodium hydroxide solution for compound d, keeps it all molten
Solution, is added in the resulting diazo liquid of step S21, T=0-10 DEG C, reacts 2-4h, and the alkalinity for the step S22 for reacting described is even
Close liquid；
Step S23: compound e-1 is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes its matter
Amount concentration is 8-12%, 30% sodium nitrite solution is added, makes the pH < 2 in reaction solution, in micro- after potassium iodide starch paper leaching
Blue, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, reacts to obtain diazonium described in step 23
Liquid,
The step S24- step S26 step having the same of step S24- step S26 and synthetic example 1 in the present embodiment
Suddenly.
Synthetic example 3
The compound of chemical structural formula 1-5,2-5,3-1 in following examples can comprise the following steps: following chemistry
Structural formula is respectively with a-e representative: a-1 represents one of compound of chemical structural formula Y1；H when b represents component A processed
One of acid；C-1 represents one of compound of chemical structural formula Y2；D represents wherein the one of chemical structural formula Y3
Kind compound；E represents a kind of compound of chemical structural formula Y4.
The preparation method of chemical structural formula 1-5 in one, reactive dye component A
Step S1: following structural formula a-1 is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes it
Mass concentration is 8-12%, 30% sodium nitrite solution is added, makes the pH < 2 in reaction solution, is in after potassium iodide starch paper leaching
Micro- blue, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, react step S1 diazo liquid,
Step S2: being neutralized to pH=6.0-7.0 with 10%-20% lithium hydroxide solution for b, dissolves it all, is added
Into the diazo liquid of step S1, T=0-10 DEG C, 3-5h is reacted, reaction obtains acid coupling liquid described in step S2；
Step S3: being 10-20 DEG C by the adjustment temperature of acid coupling liquid described in step S2, with the pH of lithium carbonate tune solution
=5.5-6.5 keeps the temperature 1-3h, reacts to obtain alkaline coupling liquid described in S3 step；Up to the dyestuff of above-mentioned chemical structural formula 1-5
Solution.Chemical structural formula 1-5 is as follows:
Step S4: the salt that 10-20% is added in resulting dye solution in the S3 step adds after waiting solids to be precipitated completely
Enter in solid-liquid separator and separated, remove filtrate, collects filter cake.Filter cake is soluble in water, make its mass concentration in 5-10%,
Obtain the dye solution of purification described in S4 step.
Step S5: by the dye solution Desalination machine of purification described in S4 step, desalination and concentration is carried out, conductivity of waste water is made
=0.5-1ms/cm is concentrated into concentration 20-25%, obtains dye concentrated solution.
The preparation method of chemical structural formula 2-5 in two, reactive dye component B
Step S11: by being dissolved in the water for chemical structural formula a-1, being then added 30% hydrochloric acid solution, rubble ice be added,
Make its mass concentration 8-12%, 30% sodium nitrite solution is added, the pH < 2 in reaction solution, potassium iodide starch paper leaching are made
Afterwards it is in micro- blue, T=0-10 DEG C, reacts 1-3h, remove excessive sodium nitrite with sulfamic acid, reacts to obtain institute in step S11
The diazo liquid stated,
Step S12: compound c-1 is neutralized to pH=6.0-7.0 with 10%-20% sodium hydroxide solution, makes its whole
Dissolution, is added in diazo liquid described in step S11, with the pH=5.5-6.5 of soda ash tune solution, T=0-10 DEG C, keeps the temperature 1-
3h is to get dyestuff in structure above 2-5.The following dyestuff of structural formula:
Step S13: being added the salt of 10-20% in dye solution, after waiting solids to be precipitated completely, is added in solid-liquid separator
It is separated, removes filtrate, collect filter cake.Filter cake is soluble in water, make its mass concentration in 5-10%, the dyestuff purified
Solution.
Step S14: by dye solution Desalination machine, desalination and concentration is carried out, conductivity of waste water=0.5-1ms/cm is made, be concentrated
To 20-25%, dye concentrated solution described in step S14 is obtained.
The preparation method of three, reactive dye component chemical structural formula 3-1 dyestuffs
Step S21: compound a -1 is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes its matter
Amount concentration is 8-12%, 30% sodium nitrite solution is added, makes the pH < 2 in reaction solution, in micro- after potassium iodide starch paper leaching
Blue, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, reacts to obtain diazonium described in step S21
Liquid,
Step S22: being neutralized to pH=6.0-7.0 with 10%-20% sodium hydroxide solution for compound d, keeps it all molten
Solution, is added in step S21 diazo liquid, T=0-10 DEG C, reacts 2-4h, reacts to obtain alkaline coupling liquid described in step S22；
Step S23: compound e is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes its quality
Concentration is 8-12%, adds 30% sodium nitrite solution, makes the pH < 2 in reaction solution, is in micro- indigo plant after potassium iodide starch paper leaching
Color, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, reacts to obtain diazo liquid described in step S22；
Step S24: alkaline coupling liquid is added in the resulting diazo liquid of step S22, with the pH=5.5- of soda ash tune solution
6.5, T=0-10 DEG C, 1-3h is kept the temperature to get the dyestuff of chemical structural formula 3-1.Chemical structural formula 3-1 is as follows:
Step S25: the salt that 10-20% is added in the resulting dye solution of step S24 adds after waiting solids to be precipitated completely
Enter in solid-liquid separator and separated, remove filtrate, collects filter cake.Filter cake is soluble in water, make its mass concentration in 5-10%,
Obtain the dye solution of the purification of step S25.
Step S26: the dye solution Desalination machine that step S25 is purified, carry out desalination and concentration, make conductivity of waste water=
0.5-1ms/cm is concentrated into 20-25%, obtains the resulting dye concentrated solution of step S26.
Synthetic example 4
The compound of chemical structural formula 1-3,2-2,3-3 in following examples can comprise the following steps: following chemistry
Structural formula is respectively with a-e representative: a represents one of compound of chemical structural formula Y1；H acid when b represents component A processed
One of；C-2 represents one of compound of chemical structural formula Y2；D represents the one of which of chemical structural formula Y3
Compound；E-2 represents a kind of compound of chemical structural formula Y4.
The preparation method of chemical structural formula 1-3 in one, reactive dye component A
Step S1: following structural formula a-1 is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes it
Mass concentration is 8-12%, 30% sodium nitrite solution is added, makes the pH < 2 in reaction solution, is in after potassium iodide starch paper leaching
Micro- blue, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, react step S1 diazo liquid,
Step S2: being neutralized to pH=6.0-7.0 with 10%-20% lithium hydroxide solution for b, dissolves it all, is added
Into the diazo liquid of step S1, T=0-10 DEG C, 3-5h is reacted, reaction obtains acid coupling liquid described in step S2；
Step S3: being 10-20 DEG C by the adjustment temperature of acid coupling liquid described in step S2, with the pH of lithium carbonate tune solution
=5.5-6.5 keeps the temperature 1-3h, reacts to obtain alkaline coupling liquid described in S3 step；Up to the dyestuff of above-mentioned chemical structural formula 1-5
Solution.Chemical structural formula 1-3 is as follows:
Step S4: the salt that 10-20% is added in resulting dye solution in the S3 step adds after waiting solids to be precipitated completely
Enter in solid-liquid separator and separated, remove filtrate, collects filter cake.Filter cake is soluble in water, make its mass concentration in 5-10%,
Obtain the dye solution of purification described in S4 step.
Step S5: by the dye solution Desalination machine of purification described in S4 step, desalination and concentration is carried out, conductivity of waste water is made
=0.5-1ms/cm is concentrated into concentration 20-25%, obtains dye concentrated solution.
The preparation method of chemical structural formula 2-2 in two, reactive dye component B
Step S11: by being dissolved in the water for chemical structural formula a, 30% hydrochloric acid solution is then added, rubble ice is added, makes
Its mass concentration is 8-12%, 30% sodium nitrite solution is added, makes the pH < 2 in reaction solution, after potassium iodide starch paper leaching
In micro- blue, T=0-10 DEG C, react 1-3h, remove excessive sodium nitrite with sulfamic acid, react described in step S11
Diazo liquid,
Step S12: compound c-2 is neutralized to pH=6.0-7.0 with 10%-20% sodium hydroxide solution, makes its whole
Dissolution, is added in diazo liquid described in step S11, with the pH=5.5-6.5 of soda ash tune solution, T=0-10 DEG C, keeps the temperature 1-
3h is to get dyestuff in structure above 2-2.The following dyestuff of structural formula:
Step S13: being added the salt of 10-20% in dye solution, after waiting solids to be precipitated completely, is added in solid-liquid separator
It is separated, removes filtrate, collect filter cake.Filter cake is soluble in water, make its mass concentration in 5-10%, the dyestuff purified
Solution.
Step S14: by dye solution Desalination machine, desalination and concentration is carried out, conductivity of waste water=0.5-1ms/cm is made, be concentrated
To 20-25%, dye concentrated solution described in step S14 is obtained.
The preparation method of three, reactive dye component chemical structural formula 3-3 dyestuffs
Step S21: compound a is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes its quality
Concentration is 8-12%, 30% sodium nitrite solution is added, the pH < 2 in reaction solution is made, is in micro- indigo plant after potassium iodide starch paper leaching
Color, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, reacts to obtain diazo liquid described in step S21,
Step S22: being neutralized to pH=6.0-7.0 with 10%-20% sodium hydroxide solution for compound d, keeps it all molten
Solution, is added in step S21 diazo liquid, T=0-10 DEG C, reacts 2-4h, reacts to obtain alkaline coupling liquid described in step S22；
Step S23: compound e-2 is dissolved in the water, and 30% hydrochloric acid solution is then added, and rubble ice is added, makes its matter
Amount concentration is 8-12%, adds 30% sodium nitrite solution, makes the pH < 2 in reaction solution, in micro- after potassium iodide starch paper leaching
Blue, reacts 1-3h by T=0-10 DEG C, removes excessive sodium nitrite with sulfamic acid, reacts to obtain diazonium described in step S22
Liquid；
Step S24: alkaline coupling liquid is added in the resulting diazo liquid of step S22, with the pH=5.5- of soda ash tune solution
6.5, T=0-10 DEG C, 1-3h is kept the temperature to get the dyestuff of chemical structural formula 3-3.Chemical structural formula 3-3 is as follows:
Step S25: the salt that 10-20% is added in the resulting dye solution of step S24 adds after waiting solids to be precipitated completely
Enter in solid-liquid separator and separated, remove filtrate, collects filter cake.Filter cake is soluble in water, make its mass concentration in 5-10%,
Obtain the dye solution of the purification of step S25.
Step S26: the dye solution Desalination machine that step S25 is purified, carry out desalination and concentration, make conductivity of waste water=
0.5-1ms/cm is concentrated into 20-25%, obtains the resulting dye concentrated solution of step S26.
Dyeing Example 1
By the component A of 75 parts by weight chemical structural formula 1-4, the component B of 15 parts by weight chemical structural formula 2-4,10 parts by weight
The component C of chemical structural formula 3-5, is mutually mixed, and stirs evenly, and obtains reactive dye compound.With the dye composite to cotton
Cloth is dyed, and is contaminated for black.
Dyeing Example 2
By the component A of 65 parts by weight chemical structural formula 1-5, the component B of 8 parts by weight chemical structural formula 2-1,8 parts by weight
The component B of structural formula 2-4 is learned, the component C of 19 parts by weight chemical structural formula 3-4 is mutually mixed, stirs evenly, obtains the activity
Dye composite.Cotton is dyed with the dye composite, is contaminated for black.
Dyeing Example 3
By the component A of 64 parts by weight formula chemical structural formula 1-4, the component B of 12 parts by weight chemical structural formula 2-5,12 weight
The component C of part chemical structural formula 3-4；The component C of 12 parts by weight chemical structural formula 3-5, is mutually mixed, stirs evenly, be somebody's turn to do
Reactive dye compound.Cotton is dyed with the dye composite, is contaminated for black.
Staining versus's example 1
By the component A of 75 parts by weight chemical structural formula 1-4, the component of 15 parts by weight chemical structural formula f, 10 parts by weight chemistry
The component of structural formula g, is mutually mixed, and stirs evenly, and obtains the reactive dye compound.Cotton is carried out with the dye composite
Dyeing, contaminates for black.
Staining versus's example 2
By 65 parts by weight formula active black K-BN, the component B of 8 parts by weight chemical structural formula formula 2-1,8 parts by weight chemical structures
The component B of formula 2-4, the component C of 19 parts by weight chemical structural formula 3-4 are mutually mixed, stir evenly, obtain the reactive dye group
Close object.Cotton is dyed with the dye composite, is contaminated for black.
Cotton ink jet dyeing example
Printing device: Mimaki JV33 printer；Print software: safe, printing model: 4Pass is covered
Embodiment 1-3 and comparative example 1-2 blending black and active dye are respectively taken 30 parts, are separately added into 50 parts of glycerol, two is sweet
150 parts of alcohol, 50 parts of diethylene glycol monobutyl ether, 50 parts of 1-Methyl-2-Pyrrolidone, 50 parts of isopropanol, 1000 parts are then added water to,
After mixing evenly, it is successively filtered with 0.45 micron and 0.22 micron of nylon membrane, obtains the black of embodiment 1-3 and comparative example 1-2
Color active ink.It is printed upon with printer by pretreated cotton, 90 DEG C are dried 10 minutes, then in the steam of saturation
It evaporates 30 minutes, evaporating temperature is 100 DEG C.After cotton is taken out, to be washed through subcooled water, hot water wash is soaped, and hot water wash, cold water is washed,
Dehydration and drying, respectively obtains the chintz of embodiment 1-3 and comparative example 1-2.
1) its dyeability, result are tested according to GB/T3920-2008, GB/T3921-2008, GB/T3922-2013
Such as following table one.
Table one
As seen from the above table, the dye composite of the application has excellent dyeability, especially has good degree of fixation,
Fastness to rubbing, washing fastness, fastness to perspiration.
Light fastness test
2) light fastness tester (Q-sun；Model Xenon Test Chamber Xe-1).Pass through solarization with EYE-ONE test
△ E situation of change after the test of fastness instrument, result such as following table two.
Table two
It can be obtained by table two, the black and active dye of the application is sun-resistant functional.
In conclusion the reactive dye of the application, the dye composite of the application has excellent dyeability and fastness
Performance can satisfy the market demand.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (9)
1. a kind of composition of reactive dye, it is characterised in that: including compound a kind of in chemical structural formula 1 or more than one changes
Close component B, the chemical structure of one of component A, the chemical structural formula 2 of object composition compound or more than one compounds composition
A kind of component C of compound or above compound composition in formula 3, wherein X1For any one in hydrogen, potassium, sodium, lithium, ammonium；R1
For-H or-OCH3；R2For-H ,-SO3X1、-OCH3、-CH3In any one；R3For-SO2C2H4OSO3X1；R4For-H ,-NO2、-
Any one in COOH ,-OH；R5For-H ,-NO2,-COOH, any one in OH；
Chemical structural formula 1:
Chemical structural formula 2:
Chemical structural formula 3:
2. reactive dye compound according to claim 1, is characterized in that, according to the weight of the reactive dye compound
Number meter is measured, component A content is 30-80 parts by weight, and component B content is 5-20 parts by weight, and component C content is 10-30 parts by weight.
3. reactive dye compound according to claim 1 or 2, is characterized in that: the component A includes chemical structural formula 1-
One of 1~chemical structural formula 1-5 compound is a variety of；
Chemical structural formula 1-1:
Chemical structural formula 1-2:
Chemical structural formula 1-3:
Chemical structural formula 1-4:
Chemical structural formula 1-5:
The component B includes one of chemical structural formula 2-1~chemical structural formula 2-5 compound or a variety of；
Chemical structural formula 2-1:
Chemical structural formula 2-2:
Chemical structural formula 2-3:
Chemical structural formula 2-4:
Chemical structural formula 2-5:
Chemical structural formula 2-6:
The component C includes one of chemical structural formula 3-1~chemical structural formula 3-5 compound or a variety of；
Chemical structural formula 3-1:
Chemical structural formula 3-2:
Chemical structural formula 3-3:
Chemical structural formula 3-4:
Chemical structural formula 3-5:
4. the preparation method of reactive dye compound according to claim 1 or 2, is characterized in that:
The preparation method of the component A the following steps are included:
S1: the first diazo-reaction: any one compound in structural formula Y1 is dissolved in the water, and it is molten that hydrochloric acid is then added
Liquid is added rubble ice, adds sodium nitrite solution, in micro- blue after soaking potassium iodide starch paper, removes excessive sodium nitrite,
React step S1 diazo liquid；
Structural formula Y1:
The reaction of S2: the first acid coupling
It dissolves it all, is added in the diazo liquid of step S1 and reacts, react to obtain acid coupling liquid；
The reaction of S3: the first alkaline coupling
The acid coupling liquid that step S2 is obtained reacts to obtain alkaline coupling liquid with the PH of alkali tune solution to neutral or alkalinity；To obtain the final product
The compound of above-mentioned chemical structural formula 1；
S4: the first purification step:
Salt is added in the resulting alkaline coupling liquid of step S3, after waiting solids to be precipitated completely, is added in solid-liquid separator and is divided
From, filtrate is removed, filter cake is collected, filter cake is soluble in water, make its mass concentration in 5-10%, the dye solution purified；
S5: the first desalination and concentration step:
The dye solution Desalination machine that step S4 is obtained carries out desalination and concentration, is concentrated into 20-25%, obtains dye concentrated solution；
The preparation method of the component B the following steps are included:
S11: the second diazo-reaction: any one compound in the structural formula Y1 is dissolved in the water, is then added
Hydrochloric acid solution is added rubble ice, makes its mass concentration 5-10%, adds sodium nitrite solution, is in after potassium iodide starch paper leaching
Micro- blue removes excessive sodium nitrite, react step S11 diazo liquid；
The reaction of S12: the second alkaline coupling:
By any one compound in structural formula Y2, it is dissolved all with aqueous slkali, is added to the diazo liquid of step S11
In, with the tune PH of alkali tune solution to neutral or alkalinity, react to obtain compound in chemical structural formula 2；
Structural formula Y2:
S13: the second purification step:
Salt is added in the resulting dye solution of step S12, after waiting solids to be precipitated completely, is added in solid-liquid separator and is divided
From, filtrate is removed, filter cake is collected, filter cake is soluble in water, make its mass concentration in 5-10%, the dye solution purified；
S14: the second desalination and concentration step:
The dye solution Desalination machine that step 13 is obtained carries out desalination, is concentrated into 20-25%, obtains dye concentrated solution；
The preparation method of the component C, includes the following steps:
S21: third diazo-reaction:
Any one compound in structure above Y1 is dissolved in the water, hydrochloric acid solution is then added, rubble ice is added, then
Be added sodium nitrite solution, potassium iodide starch paper leaching after be in micro- blue, remove excessive sodium nitrite, react step S21 weight
Nitrogen liquid；
S22: third alkaline coupling reaction
It dissolves it all any one compound aqueous slkali that structural formula is Y3, is added in step S21 diazo liquid, instead
Deserved alkaline coupling liquid；
Structural formula Y3:
S23: the four diazo-reaction:
Any one compound that structural formula is Y4 is dissolved in the water, hydrochloric acid solution is then added, rubble ice is added, adds
Sodium nitrite solution removes excessive sodium nitrite in micro- blue after soaking potassium iodide starch paper, react step S23 diazonium
Liquid,
Structural formula Y4:
The reaction of S24: the four alkaline coupling
The alkaline coupling liquid that step S22 is obtained is added in the diazo liquid that step S23 is obtained, with the PH of alkali tune solution to neutrality, i.e.,
Obtain the compound of above-mentioned chemical structural formula 3；
S25: third purification step: the salt being added in the resulting dye solution of step S24 after waiting solids to be precipitated completely, is added
It is separated in solid-liquid separator, removes filtrate, collect filter cake；Dye solution filter cake is soluble in water, being purified；
S26 third desalination and concentration step: the dye solution Desalination machine that step S25 is obtained carries out desalination, is concentrated into 20-
25%, obtain dye concentrated solution.
5. the preparation method of reactive dye compound according to claim 4, is characterized in that: in the step S1,
PH < 2 of first diazo-reaction, the reaction temperature of first diazo-reaction are 0-10 DEG C, described first
The reaction time of diazo-reaction is 1-3 hours；
PH < 2 of the reaction of the first acid coupling described in the S2 step, temperature are 0-10 DEG C, and described first is acid
The coupling reaction time is 3-5 hours；
The PH=5.5-6 of the reaction of the first alkaline coupling described in the S3 step, the first alkaline coupling reaction
Reaction temperature be 10-20 DEG C, the reaction time of the described first alkaline coupling reaction is 1-3 hours；
In the S4 step, the dosage of the salt is the 10-20% of mass ratio；The salt is sodium chloride；
In the S5 step, conductivity of waste water=0.5-1ms/cm of the dye solution.
6. the preparation method of reactive dye compound according to claim 4, is characterized in that: in the step S11,
PH < 2 of second diazo-reaction, the reaction temperature of second diazo-reaction are 0-10 DEG C, described second
The reaction time of diazo-reaction is 1-3 hours；
PH < 2 of the reaction of the second acid coupling described in the S12 step, temperature are 0-10 DEG C, and described second is acid
The coupling reaction time is 1-3 hours；
In the S14 step, the dosage of the salt is the 10-20% of mass ratio；The salt is sodium chloride；
In the S15 step, conductivity of waste water=0.5-1ms/cm of the dye solution.
7. the preparation method of reactive dye compound according to claim 4, is characterized in that: in the step S21,
PH < 2 of the third diazo-reaction, the reaction temperature of the third diazo-reaction are 0-10 DEG C, the third
The reaction time of diazo-reaction is 1-3 hours；
PH < 2 of the reaction of the third acid coupling described in the S22 step, the reaction temperature of third acid coupling reaction
It is 0-10 DEG C, the reaction time of the third acid coupling reaction is 2-4 hours；
PH < 2 of the 4th diazo-reaction described in the S23 step, the reaction temperature of the 4th diazo-reaction are 0-
10 DEG C, the reaction time of the 4th diazo-reaction is 1-3 hours；
The PH=5.5-6 of the reaction of the 4th alkaline coupling described in the S24 step, the 4th alkaline coupling reaction
Reaction temperature be 0-10 DEG C, the reaction time of the described 4th alkaline coupling reaction is 1-3 hours；
In the S25 step, the dosage of the salt is the 10-20% of mass ratio；The salt is sodium chloride；
In the S26 step, conductivity of waste water=0.5-1ms/cm of the dye solution.
8. the purposes of reactive dye compound according to claim 1 or 2, is characterized in that: the reactive dye combination
Object is printed and dyed for fiber or fiber textile；The fiber is cotton, and synthetic cotton is numb, any in regenerated fiber or its textile fabric
One kind, the fiber textile are Fypro, cellulose fibre, any one in protein fibre or its textile fabric.
9. the purposes of reactive dye compound according to claim 8, is characterized in that, the printing and dyeing are dyeing or ink-jet
Stamp.
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| CN110670384A (en) * | 2019-11-06 | 2020-01-10 | 上海贝通色彩科技有限公司 | Digital printing active black ink suitable for starlight 1024 nozzle |
| CN113214676A (en) * | 2021-04-28 | 2021-08-06 | 杭州吉华江东化工有限公司 | Reactive dye mixture and application thereof |
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| CN110670384A (en) * | 2019-11-06 | 2020-01-10 | 上海贝通色彩科技有限公司 | Digital printing active black ink suitable for starlight 1024 nozzle |
| CN110670384B (en) * | 2019-11-06 | 2022-04-15 | 上海贝通色彩科技有限公司 | Digital printing active black ink suitable for starlight 1024 nozzle |
| CN113214676A (en) * | 2021-04-28 | 2021-08-06 | 杭州吉华江东化工有限公司 | Reactive dye mixture and application thereof |
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