阅读说明：本技术 一种黑色分散染料的制备方法及其用途 (Preparation method and application of black disperse dye ) 是由 张建威 代余容 钟鹏飞 胡梦刚 于 2019-12-04 设计创作，主要内容包括：本发明公开了一种黑色分散染料的制备方法及其用途,本发明属于染料技术领域,本发明涉及一种黑色分散染料的制备方法及其用途,所述黑色分散染料用于氯纶纤维的染色染料浓度深,覆盖性好,日晒牢度能够达到5级以上,其它色牢度优良,特别适用于氯纶纤维的染色,匀染性好,得色鲜艳,可染较深的颜色,染出来的色纱,织物手感柔软,面料爽滑,染料利用率较高。(The invention discloses a preparation method and application of a black disperse dye, belongs to the technical field of dyes, and relates to a preparation method and application of a black disperse dye.)

1. A preparation method of black disperse dye is characterized by comprising the following steps:

(1) mixing 36-48 parts of paraldehyde with an equal weight part of water at 23-25 ℃, transferring the mixture to a reaction kettle, adding 12-14 parts of water into a liquid level separating funnel, slowly adding 37-40 parts of nitric acid with the mass fraction of 63-70% from the separating funnel, standing in a water bath at 0 ℃ for 2-3 days, adding 150 parts of sodium bisulfite saturated solution, separating out a white precipitate, filtering, washing with a small amount of alcohol , and drying to obtain glyoxal-sulfurous acid hydro-sodium salt;

(2) weighing 5-7 parts of glyoxal-sodium bisulfite and 50-60 parts of water, heating the mixture on a water bath to form a solution, adding 10-13 parts of saturated sodium carbonate solution, continuously heating and stirring the mixture in the water bath for 0.5-1 h, and then dissolving and flushing 0.01-0.04L/m oxygen³Generating tetrahydroxy-p-benzoquinone disodium salt, and heating the salt for filtering to 40-50 ℃ by using 100-120 parts of water to dissolve the salt to obtain a dye dispersion liquid;

(3) uniformly mixing 65-80 parts by weight of the dye dispersion liquid obtained in the step (2), 1-1.5 parts by weight of an emulsifier and 100 parts by weight of a 4-6% NaOH methanol solution, placing the mixture in a reaction kettle, accurately weighing 30-40 parts by weight of a 20-25% polyvinyl acetate methanol solution, placing the solution in a dropping funnel, starting a stirrer, opening the dropping funnel, slowly dropping the solution at room temperature, finishing dropping within 0.3-0.5 h, continuing stirring at room temperature for reaction for 0.5-1 h, and stopping the reaction to obtain a disperse dye colloid;

(4) mixing 10-20 parts by weight of water and 100-110 parts by weight of the disperse dye glue prepared in the step (3), heating to 75-88 ℃, adding 2.4-3.7 parts by weight of ethyl acrylate trimethyl ammonium chloride, 1.3-2.1 parts by weight of an initiator-water solution and 0.2-0.4 part by weight of a regulator, stirring for 15-20 min, simultaneously adding 1.0-2.0 parts by weight of acrylamide and 1.5-2.3 parts by weight of polyacrylamide, simultaneously adding 0.02-0.1 part by weight of copper sulfate and 0.05-0.08 part by weight of ammonium persulfate, stirring at the temperature of 85-90 ℃ for 1-2 h, cooling to 20-30 ℃, filtering and drying to obtain the black disperse dye composition.

2. The method for preparing a black disperse dye according to claim 1, wherein the initiator-water solution is azobisisobutylamidine hydrochloride-water solution, potassium persulfate-water solution or azobisisobutyronitrile sodium persulfate-water solution, and the initiator mass concentration of the initiator-water solution is 2-4%.

3. The method for preparing a black disperse dye according to claim 1, wherein the regulator is tetrabutyl titanate or cobalt naphthenate.

4. The method of claim 1, wherein the emulsifier is one of polyvinylpyrrolidone, 2-acrylamido-2-methylpropanesulfonic acid, and sodium allylsulfonate.

5. The environment-friendly non-irritant black disperse dye as claimed in claim 1, wherein the polyacrylamide is low molecular weight polyacrylamide with molecular weight of 1000-10000.

6. Use of the black disperse dye according to claims 1 to 5 for dyeing polyvinyl chloride fiber.

Technical Field

The invention relates to the technical field of dyes, in particular to a preparation method and application of a black disperse dye.

Background

The disperse dye is the most important and main type of nonionic dye in the dye industry, does not contain strong water-soluble groups, and dyes in a disperse state in the dyeing process. The printing and dyeing agent is mainly used for printing and dyeing of the polyvinyl chloride fiber and blended fabrics thereof, and can also be used for printing and dyeing of synthetic fibers such as acetate fiber, chinlon, polypropylene fiber, polyvinyl chloride fiber, acrylic fiber and the like. Disperse dyes are dyes which are sparingly soluble in water and are highly dispersed in water by the action of dispersants. The disperse dye contains no water soluble group and has relatively low molecular weight, and the molecule contains polar group (such as hydroxyl, amino, hydroxyalkyl amino, cyanoalkyl amino, etc.) and is still nonionic dye. The dye post-treatment requirement is high, and the dye is usually ground by a grinder in the presence of a dispersant to form highly dispersed and crystal-form-stable particles before being used. The dye liquor of the disperse dye is a uniform and stable suspension. Disperse dyes were produced in 1922 by the company badenanilide soda ash, germany, and are used mainly for dyeing polyester fibers and acetate fibers. At the time, the dyeing method is mainly used for dyeing acetate fibers. With the appearance of polyester fibers after the 50's of the 20 th century, the rapid development has been achieved, becoming a large class of products in the dye industry.

Disclosure of Invention

Based on the above, the present invention aims to overcome the defects of the prior art and provide a preparation method of black disperse dye and its use, so as to meet the use requirements.

In order to achieve the purpose, the invention adopts the following technical scheme:

a preparation method of a black disperse dye comprises the following steps:

(1) mixing 36-48 parts of paraldehyde with an equal weight part of water at 23-25 ℃, transferring the mixture to a reaction kettle, adding 12-14 parts of water into a liquid level separating funnel, slowly adding 37-40 parts of nitric acid with the mass fraction of 63-70% from the separating funnel, standing in a water bath at 0 ℃ for 2-3 days, adding 150 parts of sodium bisulfite saturated solution, separating out a white precipitate, filtering, washing with a small amount of alcohol , and drying to obtain glyoxal-sulfurous acid hydro-sodium salt;

(2) weighing 5-7 parts of glyoxal-sodium bisulfite and 50-60 parts of water, heating the mixture on a water bath to form a solution, and adding 10-13 parts of saturated sodium carbonate solutionHeating and stirring the solution in a water bath kettle for 0.5-1 h, and then dissolving and flushing 0.01-0.04L/m oxygen³Generating tetrahydroxy-p-benzoquinone disodium salt, and heating the salt for filtering to 40-50 ℃ by using 100-120 parts of water to dissolve the salt to obtain a dye dispersion liquid;

(3) uniformly mixing 65-80 parts by weight of the dye dispersion liquid obtained in the step (2), 1-1.5 parts by weight of an emulsifier and 100 parts by weight of a 4-6% NaOH methanol solution, placing the mixture in a reaction kettle, accurately weighing 30-40 parts by weight of a 20-25% polyvinyl acetate methanol solution, placing the solution in a dropping funnel, starting a stirrer, opening the dropping funnel, slowly dropping the solution at room temperature, finishing dropping within 0.3-0.5 h, continuing stirring at room temperature for reaction for 0.5-1 h, and stopping the reaction to obtain a disperse dye colloid;

(4) mixing 10-20 parts by weight of water and 100-110 parts by weight of the disperse dye glue prepared in the step (3), heating to 75-88 ℃, adding 2.4-3.7 parts by weight of ethyl acrylate trimethyl ammonium chloride, 1.3-2.1 parts by weight of an initiator-water solution and 0.2-0.4 part by weight of a regulator, stirring for 15-20 min, simultaneously adding 1.0-2.0 parts by weight of acrylamide and 1.5-2.3 parts by weight of polyacrylamide, simultaneously adding 0.02-0.1 part by weight of copper sulfate and 0.05-0.08 part by weight of ammonium persulfate, stirring at the temperature of 85-90 ℃ for 1-2 h, cooling to 20-30 ℃, filtering and drying to obtain the black disperse dye composition.

Further, the initiator-water solution is azobisisobutylamidine hydrochloride-water solution, potassium persulfate-water solution or azobisisobutyronitrile sodium persulfate-water solution, and the initiator mass concentration of the initiator-water solution is 2-4%.

Further, the regulator is tetrabutyl titanate or cobalt naphthenate.

Further, the emulsifier is one of polyvinylpyrrolidone, 2-acrylamide-2-methylpropanesulfonic acid and sodium allylsulfonate.

Further, the polyacrylamide is low molecular weight polyacrylamide with the molecular weight of 1000-10000.

The use of the black disperse dye is used for dyeing the polyvinyl chloride fiber.

Compared with the prior art, the invention has the following beneficial effects:

the invention synthesizes black disperse dye with tetrahydroxybenzoquinone disodium salt as dye, utilizes the principle of dyeing polyvinyl chloride fiber that polar molecules in polyvinyl chloride fiber and benzoquinone in dye molecules have larger intermolecular attraction, and utilizes the interaction between acrylamide polymer, polyvinyl alcohol and polyvinyl chloride fiber in the disperse dye to relax the molecular structure of polyvinyl chloride fiber, increase fiber gaps, make molecules easily enter into fiber, meanwhile, because acrylamide polymer and polyvinyl alcohol can generate direct attraction with fiber and dye molecules, the dye can be dissolved, dye monomolecular is brought to the surface of fiber, the concentration of dye on the surface of fiber is increased, and the surface tension of fiber can be reduced, so that moving dye molecules can quickly enter into the fiber gap area, the diffusivity of the dye molecules is improved, and the dye is promoted to be combined with the fiber, thereby completing the dyeing step. After dyeing is finished, the acrylamide polymer and the polyvinyl alcohol are completely removed by alkali washing. Common acrylamide polymers, polyvinyl alcohol and the like have no toxicity, are harmless to human bodies, and have good level dyeing performance and excellent light fastness. The synthetic process route is simple, the cost is low, and the dyeing performance is excellent. The coverage is very excellent, and the lifting force is high; the dyeing has less floating color, is particularly suitable for dyeing the polyvinyl chloride superfine fiber, can achieve high light fastness after dyeing processing, simultaneously, the cost of the dye prepared by the invention is very low compared with the cost of foreign high light dye, and can make contribution to the cost reduction and environmental protection of dyeing factories.

Compared with the prior art, the invention has the following advantages:

the black disperse dye prepared by the preparation method has the advantages of deep concentration, good coverage, light fastness of more than 5 grades, excellent other color fastness, good level-dyeing property, bright color, capability of dyeing deeper color, dyed yarn, soft fabric hand feeling, smooth fabric and high dye utilization rate, and is particularly suitable for dyeing polyvinyl chloride fiber.

Detailed Description

The present invention is further illustrated by the following examples, which are not intended to limit the scope of the present invention in any way.