CN102746713A - Blue-to-black disperse dye composition - Google Patents

Abstract

The invention provides a blue to black disperse dye composition, which mainly includes one or more blue dye components A with structures as shown in formula (I), one or more structures as shown in formula (II) The red dye component B shown and one or more orange dye components C shown in the formula (III); the disperse dye composition of the present invention breaks through the bottleneck of existing conventional disperse dyes dyeing under alkaline conditions , avoiding the problems of white powder, color spots, color flowers, and oligomers that may be produced in dyeing under acidic conditions on the inner wall of the dyeing equipment, effectively improving the dyeing quality, ensuring the stability and reproducibility of the process, and greatly improving The one-time success rate of dyeing is improved. Moreover, the prepared disperse dye has strong alkali resistance, can be applied to the alkaline burnt-out process, makes up for the shortcoming of the single color of the acidic burnt-out, and satisfies the society's requirements for clothing and accessories that are diversified and full of aesthetic feeling.

Description

A kind of blue to black disperse dye composition

(1) Technical field

The invention relates to a blue to black disperse dye composition, which is suitable for printing and dyeing of hydrophobic fiber materials or alkaline burn-out process.

(2) Background technology

At present, the dyeing of polyester fibers is usually carried out under weak acidic conditions with disperse dyes, but the refining of polyester fibers before dyeing, alkali reduction, and soaping and reduction cleaning after dyeing are all carried out under alkaline conditions. . Therefore, when dyeing in an acid bath, it is easy to cause uneven dyeing, the pH value of the dye bath fluctuates widely, the change of shade is large, and the dyeing reproducibility is poor.

Dyeing of disperse dyes under alkaline conditions can effectively remove the size and oil on polyester fabrics, overcome the shortcomings of other decomposition products such as polyester oligomers precipitated in acid baths and cause dyeing defects, often without reduction cleaning It can meet the fastness requirements, and has the effect of clean cloth surface and good fabric style. Many expert studies have shown that the pH value is required in the basic dyeing of disperse dyes, and generally should be controlled at pH=8.5~10.0. If the pH value is less than 8.5, the removal of oligomers is not sufficient, and the adsorption of dyes and serious equipment contamination still occur. If the pH value > 10.0, the requirement for the alkali resistance of the dye is particularly high, and the varieties that can be used for alkaline dyeing in the existing disperse dyes are greatly limited. Therefore, research and preparation of disperse dyes with high alkali resistance has a good market prospect.

High alkali resistance disperse dyes and alkaline burnt-out process are two necessary conditions to achieve alkaline burnt-out. Now the burnt-out printing process mostly uses acid for burnt-out printing. Although the acid burnt-out printing process is relatively mature, the burnt-out printing products have a single color and there is no mature and stable colored burnt-out printing process. If the polyester/rayon fabric can use the alkaline burn-out printing process, when the alkali removes the regenerated cellulose fiber, if the selected disperse dye has alkali resistance, the polyester that has not been rotten by alkali can be dyed at the same time. Therefore, in addition to the acid burnt-out printing style (transparent or translucent), the alkaline burn-out printing of polyester/rayon fabrics can show various colors in the ground color of the burn-out printing part, which is acid burn-out printing. unattainable.

(3) Contents of the invention

The object of the present invention is to provide a blue to black disperse dye composition, which has a wide pH dependence, is not only suitable for dyeing under conventional acidic conditions, but also suitable for dyeing under neutral and alkaline conditions, and can be used for polyester alkaline Burn-out process, and can be used alone or together with other reactive dyes for one-bath one-step dyeing process, and can obtain good dyeing effect, save energy and reduce production costs.

The technical scheme adopted in the present invention is:

A blue to black disperse dye composition, mainly comprising one or more blue dye component A with the structure shown in formula (I), one or more red dyes with the structure shown in formula (II) Component B and one or more orange dye components C with the structure shown in formula (III), based on the component A, component B and component C, the mass percentage of component A is 40 ~95%; the mass percentage of component B is 1~25%; the mass percentage of component C is 4~55%;

In formula (I), R ₁ is C ₁ ~ C ₄ alkyl, methoxyethyl or cyanoethyl, preferably ethyl; R ₂ is hydrogen or methyl, preferably methyl; Ph represents phenyl; n represents the number 1 or 2;

In formula (II), X ₁ is chlorine or bromine, R ₃ and R ₄ are independently C ₁ -C ₄ alkyl, cyanoethyl or benzyl, preferably ethyl or cyanoethyl; R ₅ is H Or C ₁ ~C ₄ alkyl, preferably methyl;

In formula (III), X ₂ is hydrogen or bromine; R ₆ and R ₇ are independently C ₁ -C ₄ alkyl, cyanoethyl or benzyl, preferably ethyl or cyanoethyl.

The structure of the component B is preferably:

Preferably, the disperse dye composition is composed of component A, component B and component C, based on the component A, component B and component C, the mass percentage of component A is 40~ 80%; the mass percentage of component B is 1-15%; the mass percentage of component C is 19-55%.

Due to the particularity of the dye industry, it is difficult and unnecessary to make a pure product, which usually contains some impurities in the preparation process. When the disperse dye composition of the present invention is made into a finished product, it is also allowed to contain a small amount of water and a small amount of physical impurities. .

The dye monomer compounds of formulas (I) to (III) used in the present invention can be easily synthesized in a manner well known to those skilled in the art, such as the methods described in patents US3573273A, CN102250486A, US3502645, GB1356695, CN1036974 or similar method for preparation.

The disperse dye composition of the present invention needs to be commercialized when it is applied to dyeing, and generally needs to be dispersed by adding an auxiliary agent. For example, after mixing the dye monomer compounds represented by component A, component B, and component C according to the above-mentioned ratio, in the presence of additives, water or other wetting agents, use a sand mill or grinder to pulverize In addition, the dye monomer compounds represented by component A, component B and component C can also be pulverized with a sand mill or a grinder in the presence of auxiliary agents, water or other wetting agents. After micronization treatment by machine, mix in the ratio mentioned above.

The composition is directly made into a finished product in the form of dye powder, and an auxiliary agent is added during use, or a part of the auxiliary agent can be added to make a finished product, and a small amount of auxiliary agent can be added during use. Preferably, the disperse dye composition is also It can be composed of component A, component B, component C and additives, and the mass of additives is 0.8 to 5 times the sum of the mass of component A, component B and component C.

The auxiliary agent is a commonly used dispersant, diffusing agent and surfactant when the disperse dye is commercialized, and it can be one of the following or a mixture of two or more of them: naphthalenesulfonic acid formaldehyde condensate, lignosulfonate, alkane Naphthalenesulfonic acid formaldehyde condensate. Such as methylnaphthalenesulfonic acid formaldehyde condensate (dispersant MF), naphthalenesulfonic acid formaldehyde condensate (diffusion agent NNO), benzylnaphthalenesulfonic acid formaldehyde condensate (diffusion agent CNF), sodium lignosulfonate (lignin 85A , lignin 83A) and so on.

The component A is preferably one of the following or a mixture of two or more thereof:

The component B is preferably one of the following or a mixture of two or more thereof:

The component C is preferably one of the following or a mixture of two or more thereof:

As a preferred combination, the component A is a compound represented by formula (I-1), component B is one of the compounds represented by formula (II-2) and (II-3) or a mixture thereof, and the component C is one of the compounds represented by formulas (III-1) and (III-3) or a mixture thereof.

The disperse dye composition of the present invention, after commercialization, can be supplied for dyeing in the liquid state after micronization, in the cream state, or in the powder state and particle state after drying by spray drying, etc., with the aforementioned specific mixing ratio Formulated to give black shades or deep blue shades. The disperse dye composition has a wide range of pH dependence, can be dyed under the condition of a pH value of 4.0 to 14.0, and obtains dyed fabrics with full hue and outstanding color fastness properties such as washing fastness.

The disperse dye composition of the present invention breaks through the bottleneck of existing conventional disperse dyes dyeing under alkaline conditions, and avoids white powder, color spots, color flowers, and oligomers that may be produced under acidic conditions on dyeing equipment. Problems such as contamination of the inner wall have effectively improved the dyeing quality, ensured the stability and reproducibility of the process, and greatly improved the first-time success rate of dyeing. At the same time, the alkaline-dyed polyester fabric has a purer shade and a softer and smoother feel than traditional acid-dyed fabrics. Moreover, this disperse dye has strong alkali resistance, can be applied to the alkaline burnt-out process, makes up for the shortcoming of the single color of the acidic burnt-out, and meets the society's requirements for clothing and accessories that are diversified and full of aesthetic feeling.

In addition, the disperse dye composition of the present invention can also cooperate with high-temperature reactive dyes to carry out one-bath dyeing of polyester-cotton blended fabrics with disperse/reactive dyes. Compared with the conventional two-bath process, this process can greatly shorten the process time. Improve labor productivity, save energy and water consumption, and reduce the burden of sewage treatment.

(4) Specific implementation methods

The present invention is further described below in conjunction with specific embodiment, but protection scope of the present invention is not limited thereto:

Example 1:

47 grams of formula (I-1) component A, 2.5 grams of formula (II-2) and 2.5 grams of formula (II-3) component B, 15 grams of formula (III-1) and 33 grams of formula (III-4 ) Component C, 200 grams of sodium lignosulfonate, mixed with 600 grams of water, ground and dispersed, dried to obtain the finished product. This dye is suitable for pretreatment and dyeing of polyester fibers and their blended fabrics under alkaline conditions Combined one-bath and one-step dyeing can provide fabrics with a uniform black color with good fastness properties.

Example 2:

After mixing 85 grams of formula (I-1) component A, 6 grams of formula (II-1) component B, 9 grams of formula (III-1) component C, 250 grams of dispersant MF, and 850 grams of water, Grind, disperse, and dry to obtain the finished product. This dye is suitable for one-bath and one-step dyeing of polyester fiber and its blended fabrics under alkaline conditions. color. Embodiment 3~13:

According to the method described in Example 1 or 2, the difference is that the weight ratio of component A, component B, component C and auxiliary agents in Table 1 are used to make slurry after adding water and blending to control the solid content of the slurry It is suitable to be 35~45%, grind and disperse, dry, and make the finished product. This dye is suitable for the one-bath one-step dyeing of polyester fiber and its blended fabrics under alkaline conditions. Uniform blue to black shade with good fastness properties. 85A and 83A in Table 1 are lignin 85A and lignin 83A respectively, and the weight unit of each component in A:B:C in Table 1 is g.

Table 1

Example 14:

Weigh 2 grams of the disperse dyes prepared in Example 1 and disperse them in 500 milliliters of water, add 1 gram of diffusion agent NNO and stir evenly, absorb 20 milliliters and mix with 100 milliliters of water, adjust the pH to 12.5 with caustic soda, add 2 grams of For polyester fabric, heat up to 70°C, continue to heat up to 130°C with a gradient of about 2°C/min, and keep it warm for 45 minutes. Then cool down to about 80°C, wash with hot water for 10 minutes, and dry. Observe the color and light of the sample fabric, and use the national standard GB/T3920, GB/T3921, and GB/T5718 to test its color fastness to rubbing, soaping, and sublimation respectively. It can provide the fabric with uniform and good black color fastness. The results are shown in the table 2.

Table 2

According to the method described in the above dyeing examples, the dyes prepared in Examples 2 to 13 are used to dye respectively, the difference is to change the dyeing pH value, and the dark blue or black fabric with basically the same dyeing performance can also be obtained, as shown in the table. 3.

table 3

Comparative example 1:

The dyeing performance of the disperse dye of the present invention in the range of pH 4 to 10 is relatively close to the dyes disclosed in patent CN101649129A and patent CN101265369A, but after the pH exceeds 12, especially 13, the performance of the dye disclosed in the above-mentioned patents declines significantly, such as washing fast The PA and PES indicators in the sublimation fastness and the polyester staining index in the sublimation fastness have dropped below level 3, which cannot meet the needs of alkaline burnt-out. However, although the performance of the dye of the present invention is reduced under strong alkaline conditions, it can still meet the needs of burnt-out under strong alkaline conditions.

Claims (8)

1. A blue to black disperse dye composition, mainly comprising one or more blue dye components A with structures as shown in formula (I), one or more structures as shown in formula (II) Red dye component B and one or more orange dye components C with the structure shown in formula (III), based on the component A, component B and component C, the mass percentage of component A 40-95%; the mass percentage of component B is 1-25%; the mass percentage of component C is 4-55%;

In formula (I), R ₁ is C ₁ ~ C ₄ alkyl, methoxyethyl or cyanoethyl; R ₂ is hydrogen or methyl; Ph represents phenyl; n represents the number 1 or 2; In formula (II), X1 is chlorine or bromine, R ₃ and R ₄ are independently C ₁ ~C ₄ alkyl, cyanoethyl or benzyl; R ₅ is H or C ₁ ~C ₄ alkyl; In formula (III), X ₂ is hydrogen or bromine; R ₆ and R ₇ are independently C ₁ -C ₄ alkyl, cyanoethyl or benzyl. 2. blue to black disperse dye composition as claimed in claim 1, is characterized in that described disperse dye composition is made up of component A, component B and component C, based on described component A, component Component B and component C, the mass percentage of component A is 40-80%; the mass percentage of component B is 1-15%; the mass percentage of component C is 19-55%. 3. blue to black disperse dye composition as claimed in claim 1, it is characterized in that said disperse dye composition is made up of component A, component B, component C and auxiliary agent, and auxiliary agent quality is component 0.8 to 5 times the sum of the mass of A, component B, and component C. 4. blue to black disperse dye compositions as claimed in claim 3, it is characterized in that described auxiliary agent is following one or the mixture of two or more thereof: naphthalenesulfonic acid formaldehyde condensate, lignosulfonate, Alkylnaphthalenesulfonic acid formaldehyde condensate. 5. The blue to black disperse dye composition as claimed in one of claims 1 to 4, wherein said component A is one of the following or a mixture of two or more thereof: 6. The blue to black disperse dye composition as claimed in one of claims 1 to 4, wherein said component B is one of the following or a mixture of two or more thereof:

7. The blue to black disperse dye composition as claimed in one of claims 1 to 4, wherein said component C is one of the following or a mixture of two or more thereof:

8. The blue to black disperse dye composition according to any one of claims 1 to 3, wherein said component A is a compound represented by formula (I-1), and component B is a compound represented by formula (II- 2), one of the compounds shown in (II-3) or a mixture thereof, component C is one of the compounds shown in formula (III-1), (III-3) or a mixture thereof;