阅读说明：本技术 一种纳米促染助剂 (Nano dyeing promoter ) 是由 范艳苹 李琪 胡克勤 于 2020-07-15 设计创作，主要内容包括：公开了一种纳米促染助剂,由以下方法制备：二氧化硅纳米球原粉脱除模板剂得到介孔二氧化硅纳米球；与壳聚糖反应得到复合材料；后者再与季铵化得到产物。该助剂不仅使得高温活性染料的上染率较高,而且使得染色亚麻织物耐干湿摩擦色牢度更高。(Discloses a nano dyeing promoter, which is prepared by the following steps: removing the template agent from the silicon dioxide nanosphere raw powder to obtain mesoporous silicon dioxide nanospheres; reacting with chitosan to obtain a composite material; the latter is then quaternized to give the product. The auxiliary agent not only enables the dye-uptake of the high-temperature reactive dye to be higher, but also enables the dry and wet rubbing fastness of the dyed linen fabric to be higher.)

1. The nanometer dyeing promoter is characterized by being prepared by the following method:

step 1: mixing ethyl orthosilicate and a template agent in the presence of ammonia water to obtain silicon dioxide nanosphere raw powder, and then removing the template agent to obtain mesoporous silicon dioxide nanospheres;

step 2: reacting the mesoporous silica nanospheres with chitosan in the presence of an acid solvent to obtain a mesoporous silica nanosphere-chitosan composite material;

and step 3: the mesoporous silica nanosphere-chitosan composite material reacts with a quaternizing agent to obtain the nano dyeing promoter.

2. The adjuvant according to claim 1, wherein the templating agent of step 1 is selected from the group consisting of cetyltrimethylammonium bromide; and/or the proportion of the template agent to the tetraethoxysilane and the ammonia water is 1 g: (2-4) mL: (1-2) mL.

3. The additive as claimed in claim 1, wherein the removing conditions in step 1 are 500-600 ℃ roasting for 2-10 h.

4. The auxiliary according to claim 1, wherein the mesoporous silica nanospheres of step 1 have an average particle size of 50-150 nm; and/or the mesoporous silica nanospheres have a double-pore structure; preferably, the diplopore structure comprises a primary pore size of 1-5nm and a particle size of 20-30 nm.

5. The aid according to claim 1, wherein the mesoporous silica nanospheres of step 2 are previously vacuum activated.

6. The additive as claimed in claim 1, wherein the viscosity average molecular weight of the chitosan obtained in step 2 is 1000-6000; the deacetylation degree is more than or equal to 85 percent; preferably, the viscosity average molecular weight of the chitosan is 2000-; the deacetylation degree is more than or equal to 90 percent; and/or the mass ratio of the mesoporous silica nanospheres to the chitosan is 1 (0.4-0.8).

7. The adjuvant according to claim 1, wherein the acidic solvent of step 2 is selected from acidified ethanol solutions.

8. The adjuvant according to claim 1, wherein the reaction temperature of step 2 is 50-90 ℃; the reaction time is 12-48 h.

9. The adjuvant according to claim 1, wherein the quaternizing agent of step 3 is selected from glycidyltrimethylammonium chloride; and/or the mass ratio of the mesoporous silica nanosphere-chitosan composite material to the quaternizing agent is 1 (0.1-0.4).

10. The adjuvant according to claim 1, wherein the reaction temperature of step 3 is 70-95 ℃; the reaction time is 8-36 h.

Technical Field

The invention belongs to the technical field, and particularly relates to a nano dyeing promoter.

Background

Flax is one of the first fibers extracted and woven into textiles by humans. The flax fabric has the advantages of good moisture absorption and air permeability, high strength, wear resistance, antibiosis, deodorization, static resistance, ultraviolet resistance, natural and rough hand feeling, tough and stiff style, economy, practicality and the like, and is honored as 'queen' in the fiber.

The flax fabric has wide application and can be used as clothing fabrics, decorative fabrics, household textiles, industrial products and the like. The flax textile production technology in the world originates, develops and matures in European countries, although the flax planting area in China is wide, the textile industry scale is second to Russia and second place around the world, but the technical process and the production equipment are relatively backward, and the improvement of the added value and the economic benefit of the flax product becomes an important issue for developing ecological dyeing and finishing in China.

The flax fiber contains a large amount of hydroxyl in molecules, so that the flax fiber can be grafted and crosslinked with most organic matters to modify the fiber. However, due to the characteristics of microstructure and chemical composition, flax fibers are usually dyed using reactive dyes. Reactive dyes, especially high temperature reactive dyes, suffer from low dye uptake and poor color fastness during the dyeing process. These problems severely restrict the development of high-end flax clothes, and have become a technical problem which troubles flax textile industry for many years.

Chen Koghui et al (chemical Engineers, 2017, 12, P22-25) prepared nano-degraded chitosan by using degraded chitosan as a raw material, sodium Tripolyphosphate (TPP) as a cross-linking agent and span 80 as a dispersing agent, and the particle size of the nano-degraded chitosan is 100-800 nm as shown by a scanning electron microscope. The dye is used for pretreatment of linen fabric, and reactive brilliant blue K-2RL dye is used for dyeing the linen fabric, so that the dye-uptake of the fabric under the optimal process is 43.3%. From the results, the dye uptake of the dye was not high. Meanwhile, researches show that the dry and wet rubbing fastness of the dyed linen fabric is poor.

Therefore, for the high-temperature reactive dyes, especially for the flax fabric dyeing of reactive brilliant blue K-2RL, a nano dyeing promoter with higher dye uptake and higher dry-wet rubbing fastness needs to be found.

Disclosure of Invention

In view of the above problems, the present invention aims to provide a nano dyeing promoter. After the linen fabric is treated by the aid of the auxiliary agent, the dye-uptake of the high-temperature reactive dye is high, and the dry-wet friction fastness of the dyed linen fabric is high.

In order to achieve the purpose, the invention adopts the following technical scheme: a nanometer dyeing promoter is prepared by the following steps:

step 1: mixing ethyl orthosilicate and a template agent in the presence of ammonia water to obtain silicon dioxide nanosphere raw powder, and then removing the template agent to obtain mesoporous silicon dioxide nanospheres;

step 2: reacting the mesoporous silica nanospheres with chitosan in the presence of an acid solvent to obtain a mesoporous silica nanosphere-chitosan composite material;

and step 3: the mesoporous silica nanosphere-chitosan composite material reacts with a quaternizing agent to obtain the nano dyeing promoter.

The auxiliary agent of the invention, wherein the template agent of the step 1 is selected from cetyl trimethyl ammonium bromide.

The auxiliary agent provided by the invention is prepared from the template agent obtained in the step 1, ethyl orthosilicate and ammonia water in a ratio of 1 g: (2-4) mL: (1-2) mL.

The auxiliary agent provided by the invention is characterized in that the removing condition in the step 1 is roasting at 600 ℃ for 2-10h at 500-.

The auxiliary agent provided by the invention is characterized in that the average particle size of the mesoporous silica nanospheres obtained in the step 1 is 50-150 nm; and/or the mesoporous silica nanospheres have a double-pore structure.

Advantageously, the diplopore structure comprises a primary pore size of 1-5nm and a particle size of 20-30 nm.

According to the auxiliary agent, the mesoporous silica nanospheres of the step 2 are subjected to vacuum activation in advance.

The auxiliary agent provided by the invention, wherein the viscosity-average molecular weight of the chitosan obtained in the step 2 is 1000-6000; the deacetylation degree is more than or equal to 85 percent.

Preferably, the viscosity average molecular weight of the chitosan is 2000-; the deacetylation degree is more than or equal to 90 percent.

The auxiliary agent provided by the invention is characterized in that the mass ratio of the mesoporous silica nanospheres in the step 2 to the chitosan is 1 (0.4-0.8).

The auxiliary agent of the invention, wherein the acidic solvent of the step 2 is selected from acidified ethanol solution.

The auxiliary agent provided by the invention is characterized in that the reaction temperature of the step 2 is 50-90 ℃; the reaction time is 12-48 h.

The auxiliary agent of the invention, wherein the quaternizing agent of the step 3 is selected from glycidyltrimethylammonium chloride.

The auxiliary agent provided by the invention is characterized in that the mass ratio of the mesoporous silica nanosphere-chitosan composite material obtained in the step 3 to the quaternizing agent is 1 (0.1-0.4).

The auxiliary agent provided by the invention is characterized in that the reaction temperature in the step 3 is 70-95 ℃; the reaction time is 8-36 h.

The invention has the beneficial effects that: compared with the prior art, the nano dyeing promoter disclosed by the invention has a better dyeing promoting effect, so that the dye-uptake of high-temperature reactive dyes, especially reactive brilliant blue K-2RL is higher, and the dry-wet friction color fastness of dyed linen fabrics is higher.

Without wishing to be bound by any theory, the specific mesoporous structure of the inventive nanopigmentation assistant and the specific chitosan-quaternizing agent bring about the above-mentioned advantageous effects.

Detailed Description

The following examples are put forth so as to provide those of ordinary skill in the art with a complete disclosure and description of how the compounds, compositions, articles, devices, and/or methods described and claimed herein are made and evaluated, and are intended to be purely exemplary and are not intended to limit the scope of what the inventors regard as their invention. Efforts have been made to ensure accuracy with respect to numbers (e.g., amounts, temperature, etc.) but some errors and deviations should be accounted for.

Unless otherwise indicated, parts are parts by weight, temperatures are in degrees Celsius or at ambient temperature, and pressures are at or near atmospheric. There are many variations and combinations of reaction conditions (e.g., component concentrations, desired solvents, solvent mixtures, temperatures, pressures, and other reaction ranges) and conditions that can be used to optimize the purity and yield of the product obtained by the process. Only reasonable routine experimentation will be required to optimize such process conditions.