阅读说明：本技术 一种有色纳米球着色剂的制备方法 (Preparation method of colored nanosphere colorant ) 是由 许佳 常宇琪 陈璐怡 于 2019-10-15 设计创作，主要内容包括：本发明公开了一种有色纳米球着色剂的制备方法,按照以下步骤顺序进行：一、将纳米球加入到溶剂中,然后超声分散直至得到均匀的溶胶液；二、将溶胶液磁力搅拌,然后保持于5～100℃恒温浴中,再加入发色母体,接着加入反应调节剂；三、将加入反应调节剂之后的反应液在5～100℃的条件下反应一段时间；四、将步骤三反应结束的液体离心分离,得到粗产物；五、将粗产物经水、有机溶剂洗涤；六、将洗涤后的粗产物干燥,得到有色纳米球着色剂。本发明通过合成反应在纳米球表面引入一系列共轭结构体系发生化学键和,使得改性后的纳米球带有全色谱的颜色,作为一种通用型着色剂,可适用于纸浆、墨水的着色,同时适用于不同纤维材料的着色。(The invention discloses a preparation method of a colored nanosphere colorant, which is carried out according to the following steps in sequence: firstly, adding nanospheres into a solvent, and then carrying out ultrasonic dispersion until uniform sol solution is obtained; magnetically stirring the sol solution, keeping the sol solution in a constant-temperature bath at 5-100 ℃, adding a color development matrix, and adding a reaction regulator; thirdly, reacting the reaction solution added with the reaction regulator for a period of time at the temperature of 5-100 ℃; fourthly, centrifugally separating the liquid after the reaction in the third step to obtain a crude product; fifthly, washing the crude product by water and an organic solvent; sixthly, drying the washed crude product to obtain the colored nanosphere colorant. The invention introduces a series of conjugated structure systems on the surfaces of the nanospheres through a synthesis reaction to generate chemical bonds, so that the modified nanospheres have full-color-spectrum colors, are used as a universal colorant, and are suitable for coloring paper pulp and ink and different fiber materials.)

1. A method for preparing a colored nanosphere colorant, characterized by comprising the following steps in sequence:

firstly, adding nanospheres with active groups into a solvent, and then carrying out ultrasonic dispersion until a uniform sol solution A is obtained;

magnetically stirring the sol solution A, keeping the sol solution in a constant-temperature bath at 5-100 ℃, adding a color development matrix, and adding a reaction regulator to prepare a reaction solution B;

thirdly, reacting the reaction liquid B for 3-8 hours at the temperature of 5-100 ℃ to obtain a liquid C;

fourthly, carrying out centrifugal separation on the liquid C to obtain a crude product D;

fifthly, washing the crude product D to obtain a substance E;

and sixthly, drying the substance E to obtain the colored nanosphere colorant.

2. The method for preparing colored nanosphere colorant according to claim 1, wherein the nanospheres with active group used in step one are nanospheres with active group prepared by, but not limited to, calcining method, vapor phase method, sol-gel method or precipitation method.

3. The method for preparing colored nanosphere colorant according to claim 1 or 2, wherein the nanospheres with active group in step one are made of zero-dimensional nanomaterial.

4. The method for preparing a colored nanosphere colorant according to claim 1 or 2, wherein the nanospheres with active group in step one include but are not limited to silica nanospheres, titanium dioxide nanospheres, zinc oxide nanospheres, zirconium oxide nanospheres or football alkene nanospheres.

5. The method for preparing colored nanosphere colorant according to claim 1 or 2, wherein the solvent in step one is any one of water, ethanol, DMF and toluene.

6. The method for preparing a colored nanosphere colorant according to claim 1 or 2, wherein the reaction modifier in step two is sodium carbonate or organic base.

7. The method of claim 1 or 2, wherein in step five, the washing process is performed by washing with water and then with an organic solvent.

8. The method for preparing a colored nanosphere colorant according to claim 1 or 2, wherein in step five, the washing process comprises washing with organic solvent and then washing with water.

9. The method of claim 1 or 2, wherein in step five, the washing is performed until the residual liquid is colorless, and the absorbance value measured by a spectrophotometer is 0.

10. The method for preparing colored nanosphere colorant according to claim 1 or 2, wherein the drying temperature in the sixth step is 60-100 ℃.

Technical Field

The invention belongs to the technical field of coloring agent preparation, and relates to a preparation method of a nanometer coloring agent, in particular to a preparation method of a colored nanosphere coloring agent.

Background

In the prior art, different dyes are selected according to different fiber varieties and specifications for coloring textile fibers, and a special dyeing process is formulated to meet the requirements of specific colors on different fibers, so that higher requirements are provided for dye synthesis. However, in the process of dyeing cotton fibers by using the reactive dye, the problems of low fixation rate, easy hydrolysis of the dye, poor stability, serious environmental pollution caused by ineffective decomposition and the like exist.

The application of nano materials in the textile field is extensive and deep. The nano material has small size effect, surface effect, macroscopic quantum tunneling effect and quantum size effect. After the material is subdivided into nanometer levels, the optical, thermal, electrical, magnetic, mechanical and chemical properties of the material are obviously different from those of a bulk object. Among them, metal oxides represented by spherical nano-silica, titanium dioxide, zinc oxide, etc. have high practical value in functional textiles. Due to the surface effect, the spherical nanoparticles can realize efficient and stable adsorption on the fiber material.

Taking nano-silica as an example, as white powder with a white sphere presenting a net three-dimensional structure, the surface of the nano-silica sphere contains hydroxyl groups in different states and has certain reactivity. The preparation method of the nano silicon dioxide spheres is various and mainly comprises a calcination method, a gas phase method, a sol-gel method, a precipitation method and the like. The nano silicon dioxide spheres prepared by different methods have different properties. To introduce specific properties, they may be surface modified, including in situ modification methods and graft modification methods.

The nanometer silica ball and dye matrix with certain activity react chemically in the presence of catalyst to introduce the color body to the surface of the silica ball to obtain the color nanometer ball. At present, the research on the nanosphere composite functionalized fiber material is more, but the research on the preparation of the colored nanosphere and the coloring of the textile material is rarely reported.

Disclosure of Invention

The invention aims to provide a preparation method of a colored nanosphere colorant, which can obtain a full-color-spectrum nano-scale colorant through a series of reactions, has simple and easy synthetic method, can be used for dyeing textile materials, can be dispersed in a water system, has simple dyeing process and has no selectivity.

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

a method for preparing a colored nanosphere colorant, characterized by comprising the following steps in sequence:

firstly, adding nanospheres with active groups into a solvent, and then carrying out ultrasonic dispersion until a uniform sol solution A is obtained;

magnetically stirring the sol solution A, keeping the sol solution in a constant-temperature bath at 5-100 ℃, adding a color development matrix, and adding a reaction regulator to prepare a reaction solution B;

thirdly, reacting the reaction liquid B for 3-8 hours at the temperature of 5-100 ℃ to obtain a liquid C;

fourthly, carrying out centrifugal separation on the liquid C to obtain a crude product D;

fifthly, washing the crude product D to obtain a substance E;

and sixthly, drying the substance E to obtain the colored nanosphere colorant.

By way of limitation, the nanospheres with active groups used in the first step are nanospheres with active groups prepared by, but not limited to, calcination, vapor phase, sol-gel method or precipitation method.

As a second limitation, the nanosphere with active group in the first step is made of zero-dimensional nanomaterial.

As a third limitation, the nanospheres with active groups in step one include, but are not limited to, silica nanospheres, titanium dioxide nanospheres, zinc oxide nanospheres, zirconium oxide nanospheres, or football alkene nanospheres.

As a fourth limitation, the solvent in the first step is any one of water, ethanol, DMF and toluene.

As a fifth limitation, the reaction modifier in step two is sodium carbonate or an organic base.

As a sixth limitation, in the fifth step, the washing process is to wash with water and then with an organic solvent.

As a seventh limitation, in the fifth step, the washing process is to wash with the organic solvent and then with water.

As an eighth limitation, in step five, the wash is performed until the residual liquid is colorless, and the absorbance value measured by a spectrophotometer is 0.

As a ninth limitation, the drying temperature in the sixth step is 60 to 100 ℃.

Due to the adoption of the technical scheme, compared with the prior art, the invention has the technical progress that:

(1) by adopting the method provided by the invention, a series of color bodies are selected to graft and modify the nanospheres, so that the full-color spectrum nano colorant can be obtained, and the colorant has no selectivity and is a universal colorant; the adsorption performance test result shows that the dye has good colorability on both natural fibers and synthetic fibers, so that the dye synthesis process is greatly simplified, and a large amount of complicated dye synthesis work is avoided;

(2) different from the traditional colorant, the colorant prepared by the method is suitable for coloring paper pulp, ink and different fiber materials, is not specific to a certain fiber material, has a good coloring effect on most common textile fiber materials, and can introduce a certain functional effect;

(3) the synthesis method used in the invention is simple and easy to implement, and the dyeing process is simple and convenient to operate, and has high application value.

The invention is applicable to the technical field of colorant preparation.

Drawings

The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.

In the drawings:

FIG. 1 is a SEM photograph of the silica nanospheres prepared in step one of example 1 of the present invention;

FIG. 2 is an enlarged view of a portion of FIG. 1;

FIG. 3 is a SEM photograph of red powdered nanosphere colorant obtained in step seven of example 1 of the present invention;

fig. 4 is a partially enlarged view of fig. 3.

Detailed Description

Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for purposes of illustration and explanation only and are not intended to limit the present invention.