CN113667324A - Dark blue reactive dye composition and preparation method thereof - Google Patents
Dark blue reactive dye composition and preparation method thereof Download PDFInfo
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- CN113667324A CN113667324A CN202111041979.3A CN202111041979A CN113667324A CN 113667324 A CN113667324 A CN 113667324A CN 202111041979 A CN202111041979 A CN 202111041979A CN 113667324 A CN113667324 A CN 113667324A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0072—Preparations with anionic dyes or reactive dyes
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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
- C09B62/503—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 the reactive group being an esterified or non-esterified hydroxyalkyl sulfonyl or mercaptoalkyl sulfonyl group, a quaternised or non-quaternised aminoalkyl sulfonyl group, a heterylmercapto alkyl sulfonyl group, a vinyl sulfonyl or a substituted vinyl sulfonyl group, or a thiophene-dioxide group
- C09B62/507—Azo dyes
- C09B62/513—Disazo or polyazo dyes
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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
Abstract
The invention belongs to the technical field of dye synthesis, and particularly provides a navy blue reactive dye composition and a preparation method thereof, and navy blue with full color light and excellent application performance can be obtained by using the composition for dyeing, and the navy blue reactive dye composition is suitable for dip dyeing, jig dyeing, pad dyeing and cold pad-batch processes; when the navy blue reactive dye composition is used for dyeing or printing fiber materials, the color yield is obviously higher than the sum and average value of the dyes of single components of the mixture after dyeing or printing, and the dyeing effect is better than that of the traditional reactive navy blue dye. The invention also provides a preparation method of the navy blue reactive dye composition, which comprises the steps of diazotizing para-ester, OAVS and DMAVS, carrying out coupling reaction in the same reaction system by using H acid coupling component, and synchronously carrying out synthesis and compounding.
Description
Technical Field
The invention belongs to the technical field of dye synthesis, and particularly relates to a navy blue reactive dye composition and a preparation method thereof.
Background
The reactive dye is taken as a representative of modern dye industry, and is rapidly developed in recent years, the annual output of the reactive dye for cellulose fiber in the world is more than 30 ten thousand tons at present, which accounts for more than 30% of the annual output of the dye in the world, but with the increasing requirements of human beings on environmental protection, the traditional reactive dye, especially the reactive navy blue dye, has the defects of low fixation rate, low deep dyeing property, high-salt and high-alkali dyeing requirement and the like, and the application of the reactive dye is limited to a great extent. Environmental protection has become a major problem in the current society, the dye industry faces a severe examination, and enterprises need to develop for a long time under a new situation, and the product quality must reach a new height. In order to reduce environmental pollution and respond to national energy-saving and emission-reducing policies, the invention provides the dark blue reactive dye composition suitable for low-temperature dyeing, solves the problems of poor leveling property, more residual liquid and the like of the traditional dye, and has the advantages of low production cost, stable reaction performance, good leveling property, high color fixing rate, good solubility, less sewage discharge and the like.
Disclosure of Invention
The invention aims to solve the problems of poor level-dyeing property, low fixation rate, low deep dyeing property, high-salt and high-alkali dyeing requirement, more residual liquid and the like of the traditional dye in the prior art.
To this end, the invention provides a navy blue reactive dye composition, which comprises a dye of a formula (1), a dye of a formula (2) and a dye of a formula (3);
the dark blue reactive dye composition comprises a formula (1) dye, a formula (2) dye and a formula (3) dye in a weight part ratio of (65-75): (15-25): (5-15).
Further, the raw material of the dye of the formula (1) comprises para-ester, H acid and OAVS, and the mass ratio of the para-ester, the H acid and the OAVS is (0.663-0.75): (0.65-0.75): (0.67-0.773), preferably 0.714:0.7: 0.721.
Further, the raw material of the dye of the formula (2) comprises para-ester, H acid and DMAVS, and the mass ratio of the para-ester, the H acid and the DMAVS is (0.153-0.255): (0.15-0.25): (0.155-0.258), preferably 0.204:0.2: 0.206.
Further, the raw material of the dye of the formula (3) comprises para-ester and H acid, and the mass ratio of the para-ester to the H acid is (0.102-0.306): (0.05-0.15), preferably 0.204: 0.1.
Further, the dark blue reactive dye composition also comprises a dye additive; wherein the dye additive comprises at least one of an accelerating agent, a color fixing agent, a softening agent, a flame retardant and an electrostatic agent.
The invention also provides a preparation method of the navy blue reactive dye composition, which is characterized by comprising the following steps:
(1) weighing para-ester, H acid, OAVS and DMAVS for later use;
(2) adding a dispersing agent into the para-ester, pulping until fine particles do not exist, and then carrying out diazotization reaction to obtain para-ester diazo liquid;
(3) adding H acid into water, pulping until fine particles do not exist, adding the H acid into the para-ester diazo liquid obtained in the step (2), stirring, and carrying out coupling reaction to obtain a primary coupling reaction liquid;
(4) mixing OAVS and DMAVS, adding a dispersing agent, pulping until no fine particles exist, and then performing diazotization reaction to obtain a mixed diazotization solution of DMAVS and OAVS;
(5) slowly pouring the mixed diazonium solution of DMAVS and OAVS into the primary coupling reaction solution in the step (3), adding NaHCO3, and carrying out secondary coupling reaction;
(6) and (5) filtering the reaction liquid in the step (5) and drying to obtain the dark blue reactive dye composition.
Further, the step (2) is specifically: adding a dispersing agent into para-ester, pulping until fine particles do not exist, adding hydrochloric acid, uniformly stirring, cooling to 0-5 ℃, then slowly dropwise adding a sodium nitrite solution, stirring at 0-5 ℃, carrying out diazotization reaction for 1.5-2 hours, ensuring that the reaction solution enables Congo red test paper to be blue in the reaction process, taking a yellow cross line with an Ehrlich reagent permeation ring as a reaction end point, and adding a trace amount of sulfamic acid to remove excessive sodium nitrite to obtain the para-ester diazo liquid.
Further, the step (3) is specifically: and (3) adding H acid into water, pulping until fine particles do not exist, adding the H acid into the para-ester diazo liquid obtained in the step (2), stirring for 2-3 hours, carrying out coupling reaction, and controlling the reaction temperature to be 10-15 ℃ and the pH to be l.0-1.3 to obtain a primary coupling reaction liquid.
Further, the step (4) is specifically: mixing OAVS and DMAVS, adding a dispersing agent into the mixture, pulping until fine particles do not exist, adding hydrochloric acid into the mixture, stirring the mixture, cooling the mixture to 0-5 ℃, then adding a sodium nitrite solution into the mixture, stirring the mixture at 0-5 ℃, carrying out diazotization reaction for 1.5-2 hours, ensuring that the reaction solution enables Congo red test paper to be blue in the reaction process, adding a micro-blue starch potassium iodide test paper, and removing excessive sodium nitrite by adding trace sulfamic acid by taking a non-yellow cross line with an Eichia reagent permeation ring as a reaction end point to obtain a DMAVS and OAVS mixed diazotization solution.
Further, the step (5) is specifically: slowly pouring the mixed diazonium solution of DMAVS and OAVS into the primary coupling reaction solution in the step (3), and slowly adding NaHCO3Adjusting the pH value of the solution to 5.5-6.5, keeping the reaction temperature at 5-10 ℃, and carrying out secondary coupling reaction for l-2 h.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the dark blue reactive dye composition provided by the invention has the formula (1) of reddish blue, the formula (2) of deep blue and the formula (3) of black, and repeated experiments prove that the reddish blue, the deep blue and the black are expressed as (65-75): (15-25): (5-15) the navy blue with full color light and excellent application performance can be obtained by proportional compounding, and the method is suitable for dip dyeing, jig dyeing, pad dyeing and cold pad-batch processes; the composition has a divinyl sulfone active group, belongs to a low-temperature type when used for dyeing a cellulose fiber material, has a dye-uptake curve close to that of the cellulose fiber material, has affinity, dye-uptake rate and color fixation rate to fibers, has relatively close sensitivity to electrolyte salts and color fixing agent alkalis to bath ratio and dyeing temperature, has excellent dyeing synchronism and level-dyeing property among compounds, has higher color fixation rate and outstanding deep dyeing property, effectively overcomes the defects of single dye dyeing affinity and color fixation rate of dyes of a formula (1), a formula (2) and a formula (3), and improves the dyeing quality of the cellulose fiber material; the composite reactive red dye in the composition contains a plurality of sulfonic groups, has high solubility, has similar structures of three component dyes, plays a role in compound synergism, has good deep dyeing property, and is suitable for extra-deep dyeing; when the navy blue reactive dye composition is used for dyeing or printing fiber materials, the color yield is obviously higher than the sum and average value of the dyes of single components of the mixture after dyeing or printing, and the dyeing effect is better than that of the traditional reactive navy blue dye.
(2) According to the preparation method of the dark blue reactive dye composition, para-ester, OAVS and DMAVS are subjected to diazotization treatment, coupling reaction is carried out in the same reaction system by using H acid coupling components, synthesis and compounding are carried out synchronously, the dark blue reactive dye is prepared in one step, the process flow is simplified, the advantages of high yield, high purity and the like can be realized under mild reaction conditions, the discharge amount of sewage generated in the preparation process is greatly reduced, and the preparation method meets the high standard requirement on the aspect of environmental protection at present.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Although representative embodiments of the present invention have been described in detail, it will be understood by those skilled in the art that various modifications and changes may be made thereto without departing from the scope of the invention. Therefore, the scope of the present invention should not be limited to the embodiments, but should be defined by the appended claims and equivalents thereof.
The invention provides a dark blue reactive dye composition, which is characterized in that: comprises a formula (1)
Dyes, dyes of formula (2) and dyes of formula (3);
the dark blue reactive dye composition comprises a formula (1) dye, a formula (2) dye and a formula (3) dye in a weight part ratio of (65-75): (15-25): (5-15), preferably 70:20: 10.
Wherein the raw materials of the dye in the formula (1) comprise para-ester, H acid and OAVS, and the mass ratio of the para-ester, the H acid and the OAVS is (0.663-0.75): (0.65-0.75): (0.67-0.773), preferably 0.714:0.7: 0.721; the raw materials of the dye of the formula (2) comprise para-ester, H acid and DMAVS, and the mass ratio of the para-ester, the H acid and the DMAVS is (0.153-0.255): (0.15-0.25): 0.155-0.258), preferably 0.204:0.2: 0.206; the raw materials of the dye of the formula (3) comprise para-ester and H acid, and the mass ratio of the para-ester to the H acid is (0.102-0.306): (0.05-0.15), preferably 0.204: 0.1.
The navy blue reactive dye composition of the invention can also contain various dye additives which are conventionally used in dyeing processes and dye preparations, such as accelerating agents, fixing agents, softening agents, flame retardants, electrostatic agents and the like, and the dosage of the dye additives can be selected according to actual needs and is generally not more than 20 percent by weight.
The invention also provides a preparation method of the dark blue reactive dye composition, which comprises the following steps:
(1) weighing para-ester, H acid, OAVS and DMAVS for later use;
(2) adding a dispersing agent into the para-ester, pulping until fine particles do not exist, and then carrying out diazotization reaction to obtain para-ester diazo liquid;
adding hydrochloric acid into the beaten para-ester, uniformly stirring, cooling to 0-5 ℃, then slowly dropwise adding a sodium nitrite solution, stirring at 0-5 ℃, carrying out diazotization for 2 hours, ensuring that the reaction solution enables Congo red test paper to be blue in the reaction process, ensuring that starch potassium iodide test paper is bluish, and adding trace sulfamic acid to remove excessive sodium nitrite to obtain para-ester diazo solution by taking a non-yellow cross line with an Ehrlich reagent osmotic ring as a reaction end point;
(3) adding H acid into water, pulping until fine particles do not exist, adding the H acid into the para-ester diazo liquid obtained in the step (2), stirring, and carrying out coupling reaction to obtain a primary coupling reaction liquid;
specifically, the beaten H acid is added into the para-ester diazo liquid and stirred for 2 to 3 hours, the reaction temperature is controlled to be 10 to 15 ℃, and the pH value is controlled to be l.0 to 1.3, so as to obtain a primary coupling reaction liquid;
(4) mixing OAVS and DMAVS, adding a dispersing agent, pulping until no fine particles exist, and then performing diazotization reaction to obtain a mixed diazotization solution of DMAVS and OAVS;
adding hydrochloric acid into the beaten mixed solution of OAVS and DMAVS, stirring, cooling to 0-5 ℃, then adding 30% sodium nitrite solution, stirring at 0-5 ℃, carrying out diazotization reaction for 1.5-2 hours, ensuring that the reaction solution enables Congo red test paper to be blue in the reaction process, taking a non-yellow cross line with an Ehrlich reagent permeation ring as a reaction end point, adding a trace amount of sulfamic acid to remove excessive sodium nitrite, and obtaining mixed diazo solution of DMAVS and OAVS;
(5) slowly pouring the mixed diazonium solution of DMAVS and OAVS into the primary coupling reaction solution in the step (3), and adding NaHCO3Carrying out secondary coupling reaction;
specifically, NaHCO is added3Adjusting the pH value of the solution to 5.5-6.5, keeping the reaction temperature at 5-10 ℃, and carrying out secondary coupling reaction for l-2 h.
(6) And (5) filtering the reaction liquid in the step (5) and drying to obtain the dark blue reactive dye composition.
The effect of the navy blue reactive dye composition of the invention is studied by the following specific examples.
Example 1:
the embodiment provides a navy blue reactive dye composition, which is prepared by the following steps:
(1) adding a dispersing agent into 31.53g of p- (beta-hydroxyethyl sulfone sulfate) aniline (namely p-ester), pulping for 1 hour to confirm that no fine particles exist, adding 13.65g of 30% hydrochloric acid, stirring for 30 minutes, cooling to 5 ℃ with ice, then slowly dropwise adding 21.7g of 30% sodium nitrite solution, controlling the temperature to be 0-5 ℃, stirring and reacting for 2 hours, and in the heat preservation reaction process, ensuring that the reaction solution can enable Congo red test paper to be blue, and the starch potassium iodide test paper is microscopically blue, taking a non-yellow intersection line with an Ehrlich reagent ring as a reaction terminal point, adding trace sulfamic acid to remove excessive sodium nitrite, so that the starch potassium iodide does not test paper to be microscopically blue, and obtaining the p-ester diazo solution;
(2) adding 34.1g of 1-amino-8-naphthol-3, 6-disulfonic acid (namely H acid) into water, pulping for 1 hour, after confirming that no fine particles exist, adding the mixture into the para-ester diazo solution, stirring and reacting for 2 hours, controlling the temperature at 10-15 ℃ and the pH at l.0, detecting by using para-nitroaniline diazo salt, and taking the disappearance of all free H acid as a reaction end point to obtain a primary coupling reaction solution; the primary coupling liquid is purple red at the initial stage, and blue components exist at the middle and later stages;
(3) 22.42g of 2-aminoanisole-4-beta-hydroxyethyl sulfone sulfate (i.e., OAVS) and 7.02g of 2, 5-dimethoxyaniline-4-beta-ethylsulfone sulfate (i.e., DMAVS) were mixed, a dispersant JS-C was added thereto, and after beating for 1 hour until no fine particles were present, adding 14.66g of 30% hydrochloric acid, stirring for 30 minutes, cooling to 5 ℃ with ice, then slowly dropwise adding 21.96g of 30% sodium nitrite solution, stirring and reacting for 2 hours at the controlled temperature of 0-5 ℃, ensuring that the Congo red test paper is blue and the starch potassium iodide test paper is blue microscopically in the reaction liquid during the heat preservation reaction process, taking a non-yellow cross line with an Ehrlich reagent ring as a reaction end point, adding trace sulfamic acid to remove excessive sodium nitrite, so that the starch potassium iodide test paper is not microscopically blue, and obtaining a mixed diazo solution of DMAVS and OAVS;
(4) the mixed diazonium solution of DMAVS and OAVS is slowly poured into the primary coupling reaction solution, and 32g of NaHCO is slowly added3Adjusting the pH value of the solution to 6.0, finishing the alkali adjustment after 30min, keeping the reaction temperature at 5-10 ℃, performing secondary coupling reaction for l.5h, detecting the acidic coupling product by using a thin-layer chromatography, wherein a developing agent is n-butyl alcohol, pyridine, water and ammonia water, and the ratio of 4:5:4:1, and when the acidic coupling product is not remained, stopping the secondary coupling reaction;
(5) and filtering the secondary coupling reaction liquid, and drying at 75 ℃ to obtain the dark blue reactive dye composition.
Example 2:
the performance of the navy blue reactive dye composition is tested in the example.
(1) Reactive dye dyeing intensity and color light contrast
Pure cotton cloth is dyed by respectively adopting reactive blue 250 and blue 203 and the dark blue reactive dye composition prepared in the example 1, and the dyeing processes are as follows: 60g/l of Na2SO420g/l NaCO3And dyeing at constant temperature of 45 ℃ for 90 min. The properties of the dyed cotton cloth were measured and the results are shown in Table 1.
TABLE 1 dyeing strength and shade comparison of reactive dyes
| Sample name | UV | Intensity of dyeing | DE | DL | DC | DH | DA | DB |
| Reactive blue 250 | 132 | 135 | -0.19 | -0.12 | -0.27 | 0.12 | 0.37 | -0.19 |
| Reactive blue 203 | 128 | 127 | 0.54 | 0.08 | 0.68 | -0.45 | -0.23 | 0.29 |
| Example 1 | 135 | 136 | 0.28 | 0.35 | 0.07 | -0.09 | 0.11 | 0.17 |
(2) SERF value comparison of reactive dyes
Pure cotton yarns are dyed by respectively adopting reactive blue 250 and blue 203 and the dark blue reactive dye composition prepared in the example 1, and the dyeing processes are as follows: 60g/l of Na2SO420g/l NaCO3And dyeing at constant temperature of 45 ℃ for 90 min. The properties of the dyed yarn were measured and the results are shown in table 2.
TABLE 2 SERF value test results
(3) Color fastness comparison of reactive dyes
Pure cotton cloth is dyed by using reactive blue 250, blue 203 and the navy blue reactive dye composition prepared in example 1 respectively, and all measurement samples are dyed to navy blue and black standard depths according to the GB/T4841.2. Soaping fastness the cotton dyed with the three dyes was tested according to ISO 105C04 and rubbing fastness according to ISO 105X12, and the results are shown in table 3.
TABLE 3 color fastness test results
(4) Reactive dye perspiration fastness comparison
Dyeing is carried out by using reactive blue 250, blue 203 and the dark blue reactive dye composition prepared in the example 1, and all the test samples are dyed to a standard depth according to the specification of GB/T4841.2. Perspiration fastness the cotton cloth dyed with the three dyes was tested according to ISO 105C04 and the results are shown in table 4.
TABLE 4 perspiration fastness test results
In conclusion, the dark blue reactive dye composition provided by the invention breaks through the conventional process, is prepared by a mixing method by utilizing the characteristic that compositions with similar structures can be synchronously synthesized, has lower energy consumption, less wastewater discharge and lower production cost compared with the traditional synthesis method, is more stable in reaction performance when being dyed at low temperature compared with the traditional process, solves the problems of poor level-dyeing property, more residual liquid and the like of the traditional dark blue reactive dye, and has the advantages of good promotion rate, good level-dyeing property, high color fixing rate, good color fastness and the like.
The above examples are merely illustrative of the present invention and should not be construed as limiting the scope of the invention, which is intended to be covered by the claims and any design similar or equivalent to the scope of the invention.
Claims (10)
1. A dark blue reactive dye composition is characterized in that: comprising a dye of formula (1), a dye of formula (2) and a dye of formula (3);
the weight part ratio of the dye in the formula (1), the dye in the formula (2) and the dye in the formula (3) in the navy blue reactive dye composition is (65-75): (15-25): 5-15).
2. A navy blue reactive dye composition according to claim 1, characterized in that: the raw materials of the dye in the formula (1) comprise para-ester, H acid and OAVS, and the mass ratio of the para-ester, the H acid and the OAVS is (0.663-0.75): (0.65-0.75): (0.67-0.773).
3. A navy blue reactive dye composition according to claim 1, characterized in that: the raw material of the dye of the formula (2) comprises para-ester, H acid and DMAVS, and the mass ratio of the para-ester, the H acid and the DMAVS is (0.153-0.255): 0.15-0.25): 0.155-0.258).
4. A navy blue reactive dye composition according to claim 1, characterized in that: the raw materials of the dye in the formula (3) comprise para-ester and H acid, and the mass ratio of the para-ester to the H acid is (0.102-0.306) to (0.05-0.15).
5. A navy blue reactive dye composition according to claim 1, characterized in that: also comprises a dye additive; wherein the dye additive comprises at least one of an accelerating agent, a color fixing agent, a softening agent, a flame retardant and an electrostatic agent.
6. A process for the preparation of a navy blue reactive dye composition according to any one of claims 1 to 5, characterized in that it comprises the following steps:
(1) weighing para-ester, H acid, OAVS and DMAVS for later use;
(2) adding a dispersing agent into the para-ester, pulping until fine particles do not exist, and then carrying out diazotization reaction to obtain para-ester diazo liquid;
(3) adding H acid into water, pulping until fine particles do not exist, adding the H acid into the para-ester diazo liquid obtained in the step (2), stirring, and carrying out coupling reaction to obtain a primary coupling reaction liquid;
(4) mixing OAVS and DMAVS, adding a dispersing agent, pulping until no fine particles exist, and then performing diazotization reaction to obtain a mixed diazotization solution of DMAVS and OAVS;
(5) slowly pouring the mixed diazonium solution of DMAVS and OAVS into the primary coupling reaction solution in the step (3), and adding NaHCO3Carrying out secondary coupling reaction;
(6) and (5) filtering the reaction liquid in the step (5) and drying to obtain the dark blue reactive dye composition.
7. The preparation method of the navy blue reactive dye composition according to claim 6, wherein the step (2) is specifically as follows: adding a dispersing agent into para-ester, pulping until fine particles do not exist, adding hydrochloric acid, uniformly stirring, cooling to 0-5 ℃, then slowly dropwise adding a sodium nitrite solution, stirring at 0-5 ℃, carrying out diazotization reaction for 1.5-2 hours, ensuring that the reaction solution enables Congo red test paper to be blue in the reaction process, taking a yellow cross line with an Ehrlich reagent permeation ring as a reaction end point, and adding a trace amount of sulfamic acid to remove excessive sodium nitrite to obtain the para-ester diazo liquid.
8. The preparation method of the navy blue reactive dye composition according to claim 6, wherein the step (3) is specifically as follows: and (3) adding H acid into water, pulping until fine particles do not exist, adding the H acid into the para-ester diazo liquid obtained in the step (2), stirring for 2-3 hours, carrying out coupling reaction, and controlling the reaction temperature to be 10-15 ℃ and the pH to be l.0-1.3 to obtain a primary coupling reaction liquid.
9. The preparation method of the navy blue reactive dye composition according to claim 6, wherein the step (4) is specifically as follows: mixing OAVS and DMAVS, adding a dispersing agent into the mixture, pulping until fine particles do not exist, adding hydrochloric acid into the mixture, stirring the mixture, cooling the mixture to 0-5 ℃, then adding a sodium nitrite solution into the mixture, stirring the mixture at 0-5 ℃, carrying out diazotization reaction for 1.5-2 hours, ensuring that the reaction solution enables Congo red test paper to be blue in the reaction process, adding a micro-blue starch potassium iodide test paper, and removing excessive sodium nitrite by adding trace sulfamic acid by taking a non-yellow cross line with an Eichia reagent permeation ring as a reaction end point to obtain a DMAVS and OAVS mixed diazotization solution.
10. The preparation method of the navy blue reactive dye composition according to claim 5, wherein the step (5) is specifically as follows: slowly pouring the mixed diazonium solution of DMAVS and OAVS into the primary coupling reaction solution in the step (3), and slowly adding NaHCO3Adjusting the pH value of the solution to 5.5-6.5, keeping the reaction temperature at 5-10 ℃, and carrying out secondary coupling reaction for l-2 h.
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| CN106566281A (en) * | 2016-09-14 | 2017-04-19 | 浙江科永化工有限公司 | Reactive navy blue-to-black dye composition and dye product |
| CN109504125A (en) * | 2018-10-31 | 2019-03-22 | 湖北华丽染料工业有限公司 | A kind of compound crimson active dyestuff suitable for low temperature dyeing |
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