WO2021196101A1

WO2021196101A1 - Water-based disperse dye which can be used in water- and oil-proofing and use thereof

Info

Publication number: WO2021196101A1
Application number: PCT/CN2020/082856
Authority: WO
Inventors: 胡会娜; 柏俊峰; 朱亚伟
Original assignee: 南通纺织丝绸产业技术研究院; 苏州大学
Priority date: 2020-04-01
Filing date: 2020-04-01
Publication date: 2021-10-07

Abstract

Disclosed are a water-based disperse dye which can be used in water- and oil-proofing and the use thereof. A method for preparing the water-based disperse dye comprises the following steps: mixing a crude dye, a surfactant mixture and water, and then grinding same to obtain the water-based disperse dye; or mixing a crude dye, a surfactant mixture, a water-proofing agent and water, and then grinding same to obtain the water-based disperse dye, wherein the surfactant mixture is composed of a cationic surfactant and a nonionic surfactant. In the present invention, by using the compounded cationic surfactant and nonionic surfactant, a nanoscale water-based disperse dye satisfying printing and dyeing processing requirements can be rapidly prepared. Obtaining a dacron article with a good waterproofness when dyeing a dacron fabric is thus achieved, and same has an excellent placement stability. Not only is the process flow shortened, but the production efficiency is also improved and the energy source is saved.

Description

Water-based disperse dyes that can be used for water and oil resistance and their applications

Technical field

The invention belongs to the technical field of dye fine chemicals and textile printing and dyeing, and specifically relates to a water-based disperse dye and a preparation method and application thereof, which are used in a short process, energy saving and emission reduction printing and dyeing process of polyester fabrics.

Background technique

The original disperse dyes cannot be directly used in textile printing and dyeing due to their poor water solubility and large particle diameter. It is necessary to grind the original disperse dyes to prepare disperse dyes with fine particle diameter, good dispersibility and stability to meet the quality requirements of textile printing and dyeing.

In the grinding process of the original disperse dyes, the choice of surfactants is extremely important; the surfactants can interact with the organic disperse dyes, which can effectively prevent the disperse dyes with finer particles from agglomerating each other, which can stabilize the dispersion. The function of dye can also effectively prevent the sedimentation of dye particles. Therefore, choosing a suitable surfactant for the grinding of disperse dyes is critical to the preparation of high-quality commercial disperse dyes, and is one of the core technologies for dye preparation.

Dispersant MF is the main auxiliary in the grinding process of disperse dyes. It has a strong dispersing effect on disperse dyes and is often used in the preparation of powdered disperse dyes. Dispersant MF is an anionic surfactant. Similar anionic surfactants to dispersant MF include diffusing agent NNO, dispersing agent CNF, and modified dispersing agent MF. From the perspective of structural categories, anionic surfactants suitable for disperse dye grinding are a class of sodium methylene dimethyl naphthalene sulfonate, sodium methylene dinaphthalene sulfonate, sodium methyl naphthalene sulfonate formaldehyde condensate, and lignin Sodium sulfonate.

In powdered disperse dyes, the existence of a large amount of anionic dispersant is the main cause of high wastewater discharge and high waste residue discharge in the printing and dyeing industry. As the printing and dyeing industry advances the technical demand for energy saving and emission reduction, the disperse dye grinding technology that uses other high-efficiency surfactants to replace or partially replace anionic dispersants can improve the application performance of commercial dyes from the source of dye preparation, which is a great advantage for the downstream printing and dyeing industry. Substantially reduce the discharge of waste water and waste residues to provide technical support.

In recent years, the disperse dye grinding technology using anionic surfactants, nonionic surfactants and cationic surfactants has been rapidly developed. The existing published technology shows that by selecting suitable surfactants and combinations, liquid disperse dyes can be prepared. However, due to the weak water solubility of disperse dyes, a large amount of surfactants and auxiliary auxiliaries are still needed to prevent the liquid disperse dyes from settling and agglomerating. Especially when the solid content of the dye is high and the solid content of the surfactant is low, there are still many difficulties in the preparation of water-based disperse dyes, but the water-based disperse dyes of high solid content dyes and low solid content surfactants , Can greatly reduce the low COD discharge of wastewater at the end of dye application from the source of dye preparation.

The waterproof and oil-repellent finishing of polyester fabrics is a conventional technology. After the dyeing or printing is completed, the dyed or printed fabric is dried, and then the padding-drying-baking process is used to prepare waterproof and oil-proof dyeing or printing. Polyester fabric. Generally speaking, the dyeing process of polyester fabrics is completed before the water- and oil-repellent finishing process; if the dyeing/water- and oil-repellent finishing is to be used in the same bath or one-step process, the anionic additives in the disperse dyes and the water- and oil-repellent finishing agent ( Such as organic fluorine water and oil repellents, fluorine-free water repellents) are prone to obvious aggregation and sedimentation, that is, solutions containing disperse dyes and water and oil repellent finishing agents at the same time, because water and oil repellent finishing agents mostly show cationic characteristics, they are extremely easy to disperse The anionic auxiliaries in dyes generate ionic bonds and cause aggregation, agglomeration and sedimentation. Therefore, the two are rarely used at the same time in actual production.

technical problem

In order to improve the prior art disperse dye grinding technology of anionic surfactants and nonionic surfactants and the lack of disperse dye grinding technology of nonionic dispersants and cationic dispersants, the present invention develops an efficient disperse dye grinding process , To greatly reduce the amount of grinding aids in the preparation of water-based disperse dyes; at the same time, in the dye grinding preparation process, add organic fluorine water and oil repellents and fluorine-free water repellents, and use the interaction of dyes and additives in the dye grinding preparation process , To prepare water-based disperse dyes with good stability and high dye solid content, which can not only meet the dyeing processing requirements of medium and dark colors, but also obtain good water and oil resistance, which can be used for water and oil repellent finishing. This is extremely advantageous and necessary for the realization of energy-saving and emission-reduction technology in printing and dyeing, specifically a water-based disperse dye and its preparation method and application, which are used in the short process, energy-saving and emission-reduction printing and dyeing process of polyester fabrics.

Technical solutions

The invention provides a disperse dye abrasive containing cationic surfactants, nonionic surfactants and waterproofing agents, which solves the problems of high auxiliary agent content and low grinding processing efficiency in the preparation of water-based disperse dyes, and obtains an excellent application performance The water-based disperse dyes solve the problem of high pollution emissions that restrict the printing and dyeing industry from the source of the fine chemical The burden of washing processing greatly reduces the discharge of wastewater and the chromaticity of wastewater.

The present invention adopts the following technical solutions:

A water-based disperse dye. The preparation method of the water-based disperse dye includes the following steps: the original dye, a surfactant mixture and water are mixed and then ground to obtain a water-based disperse dye; or the original dye, a surfactant mixture, The water-repellent agent and water are mixed and ground to obtain a water-based disperse dye; the surfactant mixture is composed of a cationic surfactant and a non-ionic surfactant.

A dyeing finishing solution. The preparation method of the dye finishing solution includes the following steps:

(1) Mix the original dye, surfactant mixture and water and then grind to obtain a water-based disperse dye; or mix the original dye, surfactant mixture, water repellent and water and grind to obtain the water-based disperse dye; the surface The active agent mixture is composed of cationic surfactant and non-ionic surfactant;

(2) Mix the water-based disperse dye of step (1) with water to obtain a dyeing finishing solution.

A dyed polyester fabric, the preparation method of the dyed polyester fabric includes the following steps:

(2) Mix the water-based disperse dye of step (1) with water to obtain a dyeing finishing solution;

(3) Dyeing the polyester fabric with the dyeing finishing solution in step (2) after padding, and then baking, washing, and drying to obtain a dyed polyester fabric.

In the present invention, the grinding is carried out in a vertical continuous zirconia equipment for 30 minutes to 40 minutes.

In the present invention, during padding, the rolling liquid rate is 85%; the drying temperature is 110°C, and the drying time is 3 minutes; the baking temperature is 190°C, and the baking time is 1 minute; and the washing temperature is The temperature is 75°C, and the time is 5 minutes; drying is a conventional technique.

In the present invention, only cationic surfactants and non-ionic surfactants are used as grinding aids without adding other additives, which can effectively disperse the original dye; in particular, in the present invention, without other additives, the disperse dye can be It exists stably with the waterproofing agent, and solves the defect that the prior art requires a large amount of auxiliary agents to stabilize the disperse dyes.

The original dye of the present invention is one of the conventional original dyes for disperse dyes, and is an untreated dye, belonging to a conventional product; in the water-based disperse dye, the particle size of the solids is 200 nm to 900 nm.

In the present invention, the mass ratio of the cationic surfactant and the nonionic surfactant is 1: (0.5-3); the cationic surfactant is an amine salt type cationic surfactant, a quaternary ammonium salt type cationic surfactant One or more of the agents; the non-ionic surfactant is one or more of long-chain fatty amine polyoxyethylene ether and castor oil polyoxyethylene ether.

Specifically, the cationic surfactant has one or more of the following structures:

(A-1)

(A-2)

(A-3)

(A-4)

(A-5)

In the formula: R ₁ is monostearic acid substituent, coconut oleic acid substituent, lauric acid substituent, oleic acid substituent; R ₂ is -C ₁₂ H ₂₅ or -C ₁₆ H ₃₃ ; R ₃ is methyl or Ethyl hydroxyethyl; R ₄ is -C ₁₇ H ₃₃ or -C ₁₇ H ₃₅ ; R ₅ is ethyl, benzyl or hydroxyethyl; X is chlorine, bromine or nitro;

The nonionic surfactant has one or more of the following structures:

(B-1)

(B-2)

(B-3)

In the formula: n = 12-60; m = 12-90; R ₆ is a C _12-18 alkyl group; R ₇ is a castor oil substituent.

In the present invention, the water-repellent agent is one or a mixture of a cationic organic fluorine water-repellent agent and a cationic fluorine-free water-repellent agent.

In the present invention, in the water-based disperse dye, the mass percentage of the original dye is 25-45%, the amount of surfactant mixture is 8-15% of the original dye, and the amount of water repellent is 0-30% of the original dye. , The balance is water.

Beneficial effect

The present invention further discloses the application of the above-mentioned water-based disperse dyes in the dyeing of polyester fabrics.

The effective effects of the present invention are: 1) A water-based disperse dye with high solid content is obtained, the particle size of the dye particles is relatively fine, nano-scale, and has excellent placement stability. 2) Obtain a low surfactant content to prepare water-based disperse dye cationic surfactant and non-ionic surfactant grinding dye formula. 3) Obtain a high-efficiency dye grinding technology with high dye content and low auxiliary agent content. The grinding time is only 30 minutes to 40 minutes, which not only improves production efficiency, but also saves energy. 4) Obtain a stable, water-based disperse dye that does not undergo sedimentation and aggregation in which a cationic waterproofing agent and dye coexist, which can realize one-step processing of waterproof finishing and dyeing. 5) Water-based disperse dyes in which waterproofing agents and dyes coexist can improve the color fastness of dyed products, greatly reduce the burden on post-dyeing treatment, significantly reduce wastewater discharge, and reduce the COD value in wastewater. 6) The present invention discloses a grinding technology using cationic surfactants and non-ionic surfactants, which can quickly prepare nano-scale water-based disperse dyes.

Description of the drawings

Figure 1 is a particle size distribution diagram of the water-based dye of Example 2.

FIG. 2 is a particle size distribution diagram of the water-based dye of Example 3. FIG.

FIG. 3 is a particle size distribution diagram of the water-based dye of Example 5. FIG.

4 is a particle size distribution diagram of the water-based dye of Example 7.

Fig. 5 is a particle size distribution diagram of the water-based dye of Example 11.

Fig. 6 is a particle size distribution diagram of the water-based dye of Example 12.

Fig. 7 is a particle size distribution diagram of the water-based dye of Example 14.

Fig. 8 is a particle size distribution diagram of the water-based dye of Example 15.

FIG. 9 is a particle size distribution diagram of the water-based dye of Example 16. FIG.

FIG. 10 is a particle size distribution diagram of the water-based dye of Example 18. FIG.

11 is a particle size distribution diagram of the water-based dye of Example 20.

Figure 12 is a particle size distribution diagram of the water-based dye of Example 21.

Fig. 13 is a particle size distribution diagram of the water-based dye of Example 26.

14 is a particle size distribution diagram of the water-based dye of Example 27.

15 is a particle size distribution diagram of the water-based dye of Example 30.

Figure 16 is a water-based dye particle size distribution diagram of Comparative Example 1.

FIG. 17 is a particle size distribution diagram of water-based dyes of Comparative Example 3. FIG.

FIG. 18 is a particle size distribution diagram of water-based dyes in Comparative Example 8. FIG.

Figure 19 is a particle size distribution diagram of water-based dyes in Comparative Example 9.

Figure 20 is a view of the dyed fabric of Example 31.

Figure 21 is a view of the dyed fabric of Example 32.

FIG. 22 is a drawing of the dyed fabric of Comparative Example 9. FIG.

FIG. 23 is a drawing of the dyed fabric of Comparative Example 10. FIG.

FIG. 24 is a drawing of the dyed fabric of Comparative Example 11. FIG.

FIG. 25 is a drawing of the dyed fabric of Comparative Example 12. FIG.

FIG. 26 is a drawing of the dyed fabric of Comparative Example 13. FIG.

Embodiments of the present invention

The present invention will be further described below in conjunction with embodiments:

All the raw materials in the examples are commercially available products, and the water-repellent agent is the organic fluorine water-repellent agent AG710 and the fluorine-free water-repellent agent CS290.

Table 1 is a comparison table of original dyes, Table 2 is a comparison table of cationic surfactants, and Table 3 is a comparison table of nonionic surfactants. The structure of the cationic surfactant is as follows:

(A-1)

(A-2)

(A-3)

(A-4)

(A-5)

The structure of the nonionic surfactant is as follows:

(B-1)

(B-2)

(B-3)

The preparation method of the water-based disperse dye of the present invention is: adding the original dye, the surfactant mixture and water into a vertical continuous zirconia device and grinding for 30 to 40 minutes to obtain the water-based disperse dye; or combining the original dye and the surfactant The mixture, water repellent and water are added to a vertical continuous zirconia equipment and ground for 30 to 40 minutes to obtain a water-based disperse dye.

... (1) Preparation of water-based disperse dyes

Example 1: Mix 25.00 g of Red 54, 1.50 g of A001, 0.75 g of B001 and the remainder of water, and grind in a vertical continuous zirconia equipment for 30 minutes to obtain 100 g of water-based disperse dye red 54.

Example 2: Mix 25.00g of Red 54, 1.50g A001, 0.75g B001, 3.75g of waterproofing agent AG and the balance of water, and grind in a vertical continuous zirconia equipment for 30 minutes to obtain 100g of water-based disperse dye red 54 .

Example 3: Mix 25.00g of Red 73, 1.25g of A003, 1.25g of B003, 5.10g of waterproofing agent AG and the balance of water, and grind in a vertical continuous zirconia equipment for 30 minutes to obtain 100g of water-based disperse dye red 73 .

Example 4: Mix 25.00 g of Red 92, 1.50 g of A004, 0.75 g of B004 and the remaining amount of water, and grind in a vertical continuous zirconia equipment for 40 minutes to obtain 100 g of water-based disperse dye red 92.

Example 5: Mix 25.00g of Red 92, 1.00g of A005, 2.50g of B005, 6.25g of waterproofing agent AG and the balance of water, and grind in a vertical continuous zirconia equipment for 30 minutes to obtain 100g of water-based disperse dye red 92 .

Example 6: Mix 25.00g of red 152, 1.25g of A006, 1.25g of B006, 7.50g of water repellent AG and the balance of water, and grind in a vertical continuous zirconia equipment for 40 minutes to obtain 100g of water-based disperse dye red 152 .

Example 7: Mix 30.00g of red 153, 1.80g of A007, 0.90g of B007, 4.51g of water repellent AG and the balance of water, and grind in a vertical continuous zirconia equipment for 40 minutes to obtain 100g of water-based disperse dye red 153 .

Example 8: Mix 30.00g of red 153, 1.50g of A008, 1.50g of B008, 5.95g of water repellent AG and the balance of water, and grind in a vertical continuous zirconia equipment for 70 minutes to obtain 100g of water-based disperse dye red 153 .

Example 9: Mix 30.00g of Red 145, 1.20g of A009, 3.00g of B009, 7.43g of water repellent AG and the balance of water, and grind in a vertical continuous zirconia equipment for 40 minutes to obtain 100g of water-based disperse dye red 145 .

Example 10: Mix 30.00g red 179, 1.80g A010, 0.90 g B010, 8.85g water repellent AG and the balance of water, and grind in a vertical continuous zirconia equipment for 40 minutes to obtain 100g water-based disperse dye red 179 .

Example 11: Mix 30.00g of red 179, 1.50g of A011, 1.50g of B011, 5.50g of water repellent CS and the balance of water, and grind in a vertical continuous zirconia equipment for 35 minutes to obtain 100g of water-based disperse dye red 179 .

Example 12: Mix 35.00g of red 343, 1.75g of A012, 1.75g of B012, 5.00g of water repellent CS and the balance of water, and grind in a vertical continuous zirconia equipment for 35 minutes to obtain 100g of water-based disperse dye red 343 .

Example 13: Mix 35.00g yellow 54, 2.10g A013, 1.05 g B005, 6.95g water repellent CS and the balance of water, and grind in a vertical continuous zirconia equipment for 35 minutes to obtain 100g water-based disperse dye yellow 54 .

Example 14: Mix 35.00g of Yellow 54, 1.40g A014, 3.50g of B006, 8.75g of waterproofing agent CS and the balance of water, and grind in a vertical continuous zirconia equipment for 35 minutes to obtain 100g of water-based disperse dye yellow 54 .

Example 15: Mix 35.00g of Yellow 114, 1.40g of A015, 3.50g of B006, 10.00g of water repellent CS and the balance of water, and grind in a vertical continuous zirconia equipment for 30 minutes to obtain 100g of water-based disperse dye yellow 114 .

Example 16: Mix 35.00g yellow 211, 1.10g A014, 1.00g A004, 1.05 g B006, 2.50g of water-repellent CS and the remaining amount of water are mixed, and milled in a vertical continuous zirconia equipment for 38 minutes to obtain 100g of water-based disperse dye yellow 211.

Example 17: Mix 30.00g orange 30, 1.00g A014, 0.80g A006, 0.90 g B007, 6.85g of water-repellent CS and the balance of water were mixed, and ground in a vertical continuous zirconia equipment for 32 minutes to obtain 100g of water-based disperse dye Orange 30.

Example 18: 30.00g orange 30, 1.00g A010, 0.20g A008, 1.50 g B003, 1.50 g B012, 3.00 g water repellent CS, 3.00 g water repellent AG and the balance of water were mixed, and ground in a vertical continuous zirconia equipment for 35 minutes to obtain 100 g of water-based disperse dye Orange 30.

Example 19: 35.00g orange 44, 1.20g A010, 0.90g A008, 1.05 g B007, 3.50g water-repellent CS, 3.50g water-repellent AG and the remainder of water were mixed, and milled in a vertical continuous zirconia equipment for 35 minutes to obtain 100g of water-based disperse dye orange 44.

Example 20: Mix 35.00 g orange 44, 1.75 g A012, 1.75 g B009, 4.00 g water repellent CS, 5.00 g water repellent AG and the balance water, and grind in a vertical continuous zirconia equipment for 35 minutes to obtain 100 g Water-based disperse dye Orange 44.

Example 21: Mix 40.00g orange 288, 1.20g A002, 1.20g A013, 1.20 g B004, 6.00g water-repellent CS and the remaining amount of water are mixed, and ground in a vertical continuous zirconia equipment for 30 minutes to obtain 100g of water-based disperse dye Orange 288.

Example 22: Mix 40.00g orange 288, 1.20g A002, 0.40g A009, 1.00 g B004, 3.00 g B011, 8.00 g of water repellent CS and the balance of water were mixed, and ground in a vertical continuous zirconia equipment for 30 minutes to obtain 100 g of water-based disperse dye Orange 288.

Example 23: Mix 40.00g of Violet 63, 2.00g of A014, 2.00g of B007, 10.00g of water repellent CS and the balance of water, and grind in a vertical continuous zirconia equipment for 35 minutes to obtain 100g of water-based disperse dye Violet 63 .

Example 24: 40.00g purple 63, 0.80g A005, 0.80g A011, 4.00 g B009, 11.50g water-repellent CS and the balance of water are mixed, and milled in a vertical continuous zirconia equipment for 38 minutes to obtain 100g of water-based disperse dye violet 63.

Example 25: Mix 45.00g purple 93, 0.70g A008, 2.00g A015, 1.35 g B004, 6.70g of water-repellent CS and the remaining amount of water are mixed, and milled in a vertical continuous zirconia equipment for 33 minutes to obtain 100g of water-based disperse dye Violet 93.

Example 26: Mix 45.00g purple 93, 2.00g A010, 0.25g A015, 2.00g Mix B010, 0.25g B005, 9.00g water-repellent CS and the remaining amount of water, and grind in a vertical continuous zirconia equipment for 90 minutes to obtain 100g of water-based disperse dye Violet 93.

Example 27: Mix 30.00g of blue 60, 1.20g of A012, 3.00g of B002, 4.50g of water repellent CS and the balance of water, and grind in a vertical continuous zirconia equipment for 35 minutes to obtain 100g of water-based disperse dye blue 60 .

Example 28: Mix 45.00g of blue 79, 2.25g of A012, 2.25g of B011, 11.00g of water repellent CS and the balance of water, and grind in a vertical continuous zirconia equipment for 30 minutes to obtain 100g of water-based disperse dye blue 79 .

Example 29: Mix 35.00g blue 183, 1.75g A015, 1.75g B008, 6.50g water repellent CS and the balance of water, and grind in a vertical continuous zirconia equipment for 30 minutes to obtain 100g water-based disperse dye blue 183 .

Example 30: Mix 30.00g blue 291-1, 1.50g A014, 1.50g B005, 7.50g water repellent CS and the balance of water, and grind in a vertical continuous zirconia equipment for 35 minutes to obtain 100g water-based disperse dye Blue 291:1.

Comparative Example 1: Mix 25.00 g of Red 92, 1.50 g of A004 and the remainder of water, and grind in a vertical continuous zirconia equipment for 40 minutes to obtain 100 g of disperse dye red 92-A.

Comparative Example 2: Mix 35.00 g of Orange 44, 1.75 g of B009 and the balance of water, and grind in a vertical continuous zirconia equipment for 35 minutes to obtain 100 g of disperse dye orange 44-A.

Comparative Example 3: Mix 25.00 g of Red 92, 1.00 g of A005, 6.25 g of water repellent AG and the remainder of water, and grind in a vertical continuous zirconia equipment for 30 minutes to obtain 100 g of disperse dye red 92-B.

Comparative Example 4: Mix 35.00 g of orange 44, 1.75 g of B009, 4.00 g of water repellent CS and the balance of water, and grind in a vertical continuous zirconia equipment for 35 minutes to obtain 100 g of disperse dye orange 44-B.

Comparative Example 5: Take 96.25 g of the water-based disperse dye in Example 1, add 3.75 g of water repellent AG, and mechanically stir for 5 minutes to obtain 100 g of disperse dye red 54-B.

Comparative example 6: 35.00g yellow 54, 2.10g Tween 80 (polyoxyethylene sorbitan monooleate), 1.05 g Glycidyl trimethyl ammonium chloride (2,3-epoxypropyl trimethyl ammonium chloride) is mixed with the remaining amount of water, and ground in a vertical continuous zirconia equipment for 35 minutes to obtain 100 g of water-based disperse dyes Yellow 54-B.

Comparative example 7: 35.00g yellow 54, 2.10g Tween 80 (polyoxyethylene sorbitan monooleate), 1.05 g Glycidyl trimethyl ammonium chloride (2,3-epoxypropyl trimethyl ammonium chloride), 6.95 g of water repellent CS and the remainder of water are mixed, and grind in a vertical continuous zirconia equipment for 35 minutes. Obtain 100g of water-based disperse dye yellow 54-C.

Comparative Example 8: 35.00g yellow 54, 2.10g Tween 80, 1.05g glycidyltrimethylammonium chloride (2,3-epoxypropyltrimethylammonium chloride), 1.00g anionic diffusing agent MF , 6.95g water-repellent CS is mixed with the remaining amount of water, and grind in a vertical continuous zirconia equipment for 40 minutes to obtain 100g of water-based disperse dye yellow 54-D;

Mix 25.00g of Red 54, 1.50g of anionic diffusing agent MF, 0.75g of B001 and the balance of water, and grind in a vertical continuous zirconia equipment for 30 minutes to obtain 100g of water-based disperse dye red 54-C.

(2) Preparation and dyeing method of dyeing solution

Example 31: 1) Dye solution preparation: 3.5Kg water-based disperse dye red 54 (Example 1) and 96.5Kg water were mixed to prepare a red dye solution; 2) Padding and drying: the existing conventional polyester fabric Padding the red dye solution on the continuous open-width rolling mill, controlling the rolling rate to be 85%; after the padding is completed, it is dried on the continuous drying equipment, the drying temperature is 110℃, and the drying time is 3 minutes; 3) High temperature dye fixation: After the drying is completed, high temperature treatment is performed on the continuous baking machine to complete the dyeing and fixing of the disperse dye on the polyester fiber, the baking temperature is 190 ℃, and the baking time is 1 minute; 4) After Treatment and drying: After the baking is completed, the polyester is washed with hot water in a continuous water washing equipment, the washing temperature is 75 ℃, and the washing time is 5 minutes; after the washing is completed, the polyester fabric is subjected to conventional drying treatment to obtain red polyester dyeing Fabric.

Example 32: 1) Dye solution preparation: 3.5Kg of water-based disperse dye red 54 (Example 2) and 96.5Kg of water were mixed to prepare a red dye solution. The remaining steps and process condition control are the same as in Example 31.

Example 33: 1) Dye solution preparation: 3.0 Kg of water-based disperse dye red 92 (Example 4) and 97.0 Kg of water were mixed to prepare a red dye solution. The remaining steps and process condition control are the same as in Example 31.

Example 34: 1) Dye solution preparation: 3.0 Kg of water-based disperse dye red 92 (Example 5) and 97.0 Kg of water were mixed to prepare a red dye solution. The remaining steps and process condition control are the same as in Example 31.

Example 35: 1) Dye solution preparation: 2.5Kg of water-based disperse dye Orange 44 (Example 20) and 97.5Kg of water were mixed to prepare an orange dye solution. The remaining steps and process condition control are the same as in Example 31.

Example 36: 1) Dye solution preparation: 2.5Kg of water-based disperse dye Violet 63 (Example 23) and 97.5Kg of water were mixed to prepare a purple dye solution. The remaining steps and process condition control are the same as in Example 31.

Comparative Example 9: 1) Dye solution preparation: 2.5Kg of water-based disperse dye red 92-A (Comparative Example 1) and 97.5Kg of water were mixed to prepare a red dye solution. The remaining steps and process condition control are the same as in Example 31.

Comparative Example 10: 1) Dye solution preparation: 2.5Kg of water-based disperse dye red 92-B (Comparative Example 3) and 97.5Kg of water were mixed to prepare a red dye solution. The remaining steps and process condition control are the same as in Example 31.

Comparative Example 11: 1) Dye solution preparation: 2.5Kg of water-based disperse dye red 54-B (Comparative Example 5) and 97.5Kg of water were mixed to prepare a red dye solution. The remaining steps and process condition control are the same as in Example 31.

Comparative Example 12: 1) Dye solution preparation: 2.5Kg of water-based disperse dye yellow 54-B (Comparative Example 6) and 97.5Kg of water were mixed to prepare a yellow dye solution. The remaining steps and process condition control are the same as in Example 31.

Comparative Example 13: 1) Dye solution preparation: 2.5Kg of water-based disperse dye yellow 54-B (Comparative Example 7) and 97.5Kg of water were mixed to prepare a yellow dye solution. The remaining steps and process condition control are the same as in Example 31.

Performance test of water-based disperse dyes: see Table 4 for test results.

1) Average particle size: Test the average particle size of water-based disperse dyes on a laser particle size analyzer. For the description of the figure number of the dye particle size test chart, see Table 4, and the test results are shown in attached drawings 1 to 19;

2) Centrifugal stability: Take 5ml of the water-based disperse dye to be tested, centrifuge at 3000 rpm for 30 minutes at room temperature, and observe the degree of delamination or sedimentation of the water-based disperse dye;

3) Storage stability: Put 10g sample (disperse dye) in a 25ml glass reagent bottle, put it in a (50±2℃) constant temperature drying oven for 14h, take it out and place it at room temperature (20±2℃) for 30 days , Observe the phenomenon of liquid dye layering or sedimentation.

Continuous dyeing performance test of water-based disperse dyes: see Table 5 for test results.

1) Color fastness to rubbing: Measure and rank according to GB/T 3920-2008 "Textile Color Fastness Test and Color Fastness to Rubbing".

2) Waterproof performance: Measure and grade according to GB/T 4745-2012 "Testing and Evaluation of Textile Waterproof Performance: Water-Dipping Method".

It can be seen from Table 4 that the particle size of the water-based disperse dyes prepared by the present invention is relatively small, and the average particle size of the dye particles ranges from 212nm to 768nm, and it does not appear after the centrifugal stability test and the storage stability test. Delamination phenomenon. The prepared water-based disperse dyes have high-efficiency grinding efficiency and shorter grinding time. The prepared water-based disperse dyes have nano-level characteristics, have good stability, and no delamination occurs.

Comparative Example 1 uses Red 92 ground with only cationic surfactants. Its particle size is relatively large. The average particle size of Dye Red 92-A is 1604nm, respectively. The centrifugal stability test and the storage stability test have obvious differences. Layer phenomenon; that is, using only cationic surfactants as abrasives, it is difficult to grind the dye into nanometers, and its abrasive performance is far lower than that of the present invention.

Comparative Example 2 is orange 44 milled with only non-ionic surfactants. Its particle size is larger. The average particle size of dye orange 44-A is 1759nm respectively. It is obvious after centrifugal stability test and storage stability test. Delamination phenomenon; that is, it is difficult to grind the dye to nanometer level when only non-ionic surfactant is used as the grinding agent, and its grinding performance is far lower than that of the present invention.

Comparative Example 3 uses Red 92 ground with only cationic surfactant and water repellent agent. Its particle size is relatively large, with an average particle size of 1360 nm. The centrifugal stability test and the storage stability test both show obvious delamination.

Comparative Example 4 uses orange 44 milled with only non-ionic surfactants and water repellent agents. Its particle size is relatively large, with an average particle size of 1567nm. The centrifugal stability test and the storage stability test both show obvious delamination.

Comparative Example 5 is a dye solution mixed with water-repellent agent and water-based disperse dye (the ground dye in Example 1, without water-repellent agent), and then mechanically stirred for a short period of time, although its average particle size is also small (780nm ), but both the centrifugal stability test and the storage stability test showed slight delamination.

Comparative Example 6 is yellow 54 ground with non-ionic surfactants and cationic surfactants that are not of the present invention. Its particle size is larger, with an average particle size of 1567nm. It is obvious after centrifugal stability test and storage stability test. Delamination phenomenon.

Comparative Example 7 is yellow 54 ground with non-ionic surfactants and cationic surfactants of the present invention. Its particle size is larger, with an average particle size of 2397nm. It has obvious differences in both the centrifugal stability test and the storage stability test. The phenomenon of layering indicates that the use of a combination of surfactants other than the present invention will reduce the grinding and dispersion efficiency when a water-repellent agent is present at the same time. In the same grinding time, the grinding and dispersion effect will be weakened.

There is an anionic surfactant in the dye grinding system of Comparative Example 8. Due to the phenomenon of agglomeration and agglomeration due to electrostatic effects, nano-scale water-based disperse dyes cannot be prepared, that is, disperse dyes cannot be obtained, and stability tests are not performed.

It can be seen from Table 5 that the dyed products prepared by the continuous dyeing of water-based disperse dyes prepared by the present invention, when the dye contains water-repellent agent AG and water-repellent agent CS, all have excellent water resistance. The grades are all up to 4-5, that is, there is no wetting on the surface of the sample, only a small amount of water droplets. When the dye does not contain the water-repellent agent AG and the water-repellent CS, the water resistance of the sample is poor, that is, the surface of the sample is wetted beyond the spray point, and the wetted area is larger; the water-based disperse dye prepared by the present invention The dyed products prepared by continuous dyeing have excellent rubbing color fastness. The dry and wet rubbing color fastness of unwashed fabrics are not lower than 4-5 grades, and the dry and wet rubbing color fastness of washed fabrics All reached level 5. And the color of the surface of the cloth sample is uniform, and there are no color blocks and color spots. These excellent properties can greatly reduce the burden of washing after dyeing, reduce the consumption of water resources, and realize one-bath one-step processing of dyeing and waterproofing, which can save a lot of energy consumption and facilitate industrial applications. Compared with the dyed products prepared by continuous dyeing of water-based disperse dyes prepared by the present invention, the results of Comparative Example 9 to Comparative Example 13 show that its water resistance is not as good as that of the present invention, that is, the surface of the sample has sporadic sprays. Wetting at spots, and the rubbing fastness of unwashed and washed fabrics is also low, that is, if you want to achieve the dyeing fastness of the present invention, you need to increase the task of washing, or use the reduction cleaning method to better remove the fiber The floating color of the dye on the surface will increase the amount of pollution and increase the COD value in the waste water. The water washing COD of the present invention is less than 50 ppm. In addition, the fabric samples of Comparative Example 9 to Comparative Example 13 have more or less color points and color patches on the surface, and their surface uniformity is not as good as that of the water-based dye prepared by the patent of the present invention. This is because the optimization aid disclosed in the present invention is adopted. The combination of agents can prepare water-based disperse dyes with excellent stability, and prevent dye aggregation and agglomeration caused by the instability of water-based dyes, thereby avoiding color spots and color blocks.

Claims

A water-based disperse dye, characterized in that: the preparation method of the water-based disperse dye comprises the following steps: the original dye, the surfactant mixture and water are mixed and then ground to obtain the water-based disperse dye; or the original dye and the surface The active agent mixture, the water repellent and water are mixed and ground to obtain a water-based disperse dye; the surfactant mixture is composed of a cationic surfactant and a non-ionic surfactant; the water repellent is a cationic water repellent.
The water-based disperse dye according to claim 1, wherein the particle size of the solids in the water-based disperse dye is 200 nm to 900 nm.
The water-based disperse dye according to claim 2, wherein the mass ratio of the cationic surfactant and the nonionic surfactant is 1: (0.5-3); the cationic surfactant is an amine salt type cationic One or more of surfactants and quaternary ammonium salt type cationic surfactants; the non-ionic surfactant is one or more of long-chain fatty amine polyoxyethylene ether and castor oil polyoxyethylene ether.
The water-based disperse dye according to claim 3, wherein the cationic surfactant has one or more of the following structures:

(A-1)

(A-2)

(A-3)

(A-4)

(A-5)

In the formula: R 1 is monostearic acid substituent, coconut oleic acid substituent, lauric acid substituent or oleic acid substituent; R 2 is -C 12 H 25 or -C 16 H 33 ; R 3 is methyl or Ethyl hydroxyethyl; R 4 is -C 17 H 33 or -C 17 H 35 ; R 5 is ethyl, benzyl or hydroxyethyl; X is chlorine, bromine or nitro;

The nonionic surfactant has one or more of the following structures:

(B-1)

(B-2)

(B-3)

In the formula: n = 12-60; m = 12-90; R 6 is a C 12-18 alkyl group; R 7 is a castor oil substituent.
The water-based disperse dye according to claim 1, wherein the water-repellent agent is one or two of a cationic organic fluorine water-repellent agent and a cationic fluorine-free water-repellent agent.
The water-based disperse dye according to claim 1, characterized in that: in the water-based disperse dye, the mass percentage of the original dye is 25-45%, the amount of the surfactant mixture is 8-15% of the original dye, and the water repellent agent The dosage is 0-30% of the original dye quality, and the balance is water.
A dyeing finishing solution. The preparation method of the dye finishing solution includes the following steps:

(1) Mix the original dye, surfactant mixture and water and then grind to obtain a water-based disperse dye; or mix the original dye, surfactant mixture, water repellent and water and grind to obtain the water-based disperse dye; the surface The active agent mixture is composed of cationic surfactant and non-ionic surfactant;

(2) Mix the water-based disperse dye of step (1) with water to obtain a dyeing finishing solution.
A dyed polyester fabric, the preparation method of the dyed polyester fabric includes the following steps:

(1) Mix the original dye, surfactant mixture and water and then grind to obtain a water-based disperse dye; or mix the original dye, surfactant mixture, water repellent and water and grind to obtain the water-based disperse dye; the surface The active agent mixture is composed of cationic surfactant and non-ionic surfactant;

(2) Mix the water-based disperse dye of step (1) with water to obtain a dyeing finishing solution;

(3) Dyeing the polyester fabric with the dyeing finishing solution in step (2) after padding, and then baking, washing, and drying to obtain a dyed polyester fabric.
The dyed polyester fabric according to claim 8, characterized in that: in the water-based disperse dye, the mass percentage of the original dye is 25-45%, the amount of the surfactant mixture is 8-15% of the original dye, and the water-repellent The dosage is 0-30% of the original dye quality, and the balance is water.
Application of the water-based disperse dye of claim 1 or the dyeing finishing liquid of claim 7 in the dyeing of polyester fabrics.