阅读说明：本技术 一种提高kn-r活性染料染色均匀性的方法 (Method for improving dyeing uniformity of KN-R reactive dye ) 是由 张根成 杨继群 郭正祥 孙健 于 2020-12-08 设计创作，主要内容包括：本发明涉及一种提高KN-R活性染料染色均匀性的方法,具体地说,提供一种具有优异染色均匀性的KN-R活性染料,所述活性染料按重量百分比由以下组分所组成：活性艳蓝KN-R 60-80份,辅助活性染料8-12份,乳化剂1-5份,辅助盐类1-5份,缓冲剂1-5份。本发明通过加入辅助活性染料组分克服了活性艳蓝KN-R在碱性固色阶段与棉纤维间的吸色固色行为对碱的敏感性,使得染料的染色均匀性得到了明显的提升,而且上染性能也能得到兼顾,染色性能优异。(The invention relates to a method for improving dyeing uniformity of a KN-R reactive dye, and particularly provides the KN-R reactive dye with excellent dyeing uniformity, wherein the reactive dye comprises the following components in percentage by weight: 60-80 parts of reactive brilliant blue KN-R, 8-12 parts of auxiliary reactive dye, 1-5 parts of emulsifier, 1-5 parts of auxiliary salt and 1-5 parts of buffering agent. The invention overcomes the sensitivity of the color absorbing and fixing behavior of the reactive brilliant blue KN-R between the alkaline color fixing stage and the cotton fiber to alkali by adding the auxiliary reactive dye component, so that the dyeing uniformity of the dye is obviously improved, the dyeing performance can be considered, and the dyeing performance is excellent.)

1. A KN-R reactive dye with excellent dyeing uniformity comprises the following components in percentage by weight:

wherein the structural formula of the reactive brilliant blue KN-R is shown as the formula (I):

the structural formula of the auxiliary reactive dye is shown as the formula (II):

2. the KN-R reactive dye according to claim 1, wherein the emulsifier is one or a mixture of more than two of OP-10, sodium stearate, sodium dodecyl sulfate and triethanolamine.

3. The KN-R reactive dye according to claim 1, wherein the auxiliary salts are one or a mixture of two or more of sodium chloride, potassium chloride, lithium sulfate and sodium sulfate.

4. The KN-R reactive dye according to claim 1, the buffering agent being one or a mixture of two or more of sodium acetate, sodium borate, sodium bicarbonate, sodium dihydrogen phosphate, and disodium hydrogen phosphate.

5. The KN-R reactive dye of claim 1, the weight ratio of reactive brilliant blue KN-R to co-reactive dye being from 8:1 to 9.2: 1.

6. A process for the preparation of KN-R reactive dyes as claimed in any one of claims 1 to 5, comprising the process steps of: weighing reactive brilliant blue KN-R and auxiliary reactive dye according to the parts by weight, dissolving the reactive brilliant blue KN-R and the auxiliary reactive dye in water for mixing, then adding an emulsifier and auxiliary salt, finally adding a buffering agent to adjust the pH value to a proper value to obtain a mixed solution, and after uniformly mixing, carrying out spray drying to obtain the KN-R reactive dye composition.

7. A fabric dyed with the KN-R reactive dye according to any one of claims 1 to 5, specifically comprising any one of knitted fabric, denim fabric, satin fabric, ramie yarn, and woven fabric.

Technical Field

The invention relates to the field of KN-R reactive dyes, in particular to a method for improving dyeing uniformity of a KN-R reactive dye.

Background

The reactive dye has the excellent characteristics of bright color, excellent application performance, convenient use, strong applicability and the like. The reactive brilliant blue KN-R belongs to a medium-temperature reactive dye with a vinyl sulfone structure, has excellent color fastness for dyeing cotton fabrics, particularly good light fastness, bright brilliant blue light, and is difficult to color matching by other dyes. At present, due to the influence of factors such as environmental ecological restriction, economic development and the like, the requirements on production and preparation, dyeing rate, fixation rate, dyeing uniformity and dyeing wastewater of reactive dyes are higher and higher.

However, when some brilliant blue mainly comprising reactive brilliant blue KN-R is dyed by a dip dyeing method in the market at present, the problems of uneven cloth surface color and even cloth surface color patterns and poor coloring uniformity are easily caused. In order to solve the problem, the dyeing process generally needs to be carefully controlled in the actual dyeing process, and the purpose of controlling the uniformity is achieved by means of adjusting the dyeing temperature, the using amount of an alkaline agent, regulating and controlling dyeing process parameters and the like, but the problems cannot be fundamentally solved by the means, and the difficulty of process regulation and stable control is multiplied in the mass production process, so that the defective rate is high, and the production efficiency is influenced.

The reason for the uneven staining of the reactive brilliant blue KN-R is now recognized to be: the color absorbing and fixing behavior between the reactive brilliant blue KN-R and the cotton fiber is particularly sensitive to alkali, and the reactivity of covalent bond combination generated by the addition reaction between vinyl sulfone groups on the reactive brilliant blue KN-R and hydroxyl groups on the cotton fiber is very strong under the alkaline condition, so that the uneven color absorbing and fixing is caused, and even colored patterns are generated. Therefore, an effective measure at present is to strictly control the alkali content in the dyeing process, but in practice, it is not easy to monitor and adjust the alkali content at any time along with the change of reaction conditions so as to achieve the purpose of uniform dyeing. Prior art "dye adsorption kinetics: influence of dye liquor flow rate on dyeing uniformity "mention that dye flow uniformity has a large influence on dyeing uniformity, but unevenness in dyeing process is inevitable, and an effective way is to increase dyeing temperature or add chemical auxiliaries which promote dye migration, but no effective and specific solution is given therein. In the prior art, CN105199428A mentions that the alkali resistance of reactive blue is improved by preparing KN-KSR dye composition and adding para-blue and sodium naphthalene sulfonate formaldehyde condensate into the reactive brilliant blue dye, thereby improving the dyeing uniformity, but the dye is easy to adsorb and color initially due to the mutual adsorption and association of different types of dye molecules, but cannot be continuously diffused into the fiber when the dyed mass point is thick enough, but the adsorption is prevented from being continuously carried out, so that the dye dyeing property is low, and the method is not suitable for long-term batch production.

Therefore, the problem of dyeing uniformity of the KN-R reactive dye is still a difficult problem, and a proper solution is needed to be found to obtain good level dyeing performance on the basis of not influencing the dyeing performance.

Disclosure of Invention

The invention aims to provide a method for improving the dyeing uniformity of KN-R reactive dye, so as to solve the problems in the background technology.

In order to achieve the above object, one of the objects of the present invention is to provide a KN-R reactive dye composition, which can achieve better dyeing uniformity without affecting the coloring performance of the dye. The KN-R reactive dye composition comprises the following components in percentage by weight:

wherein the structural formula of the reactive brilliant blue KN-R is shown as a formula I:

the structural formula of the auxiliary reactive dye is shown as a formula II:

preferably, the emulsifier is one or a mixture of more than two of OP-10, sodium stearate, sodium dodecyl sulfate and triethanolamine.

Preferably, the auxiliary salt is one or a mixture of more than two of sodium chloride, potassium chloride, lithium sulfate and sodium sulfate.

Preferably, the buffer is one or a mixture of two or more of sodium acetate, sodium borate, sodium bicarbonate, sodium dihydrogen phosphate and disodium hydrogen phosphate.

Preferably, the weight ratio of the reactive brilliant blue KN-R to the auxiliary reactive dye is 8:1 to 9.2: 1.

The invention also aims to provide a preparation method of the KN-R reactive dye composition, which specifically comprises the following steps: weighing the reactive brilliant blue KN-R and the auxiliary reactive dye according to the parts by weight, dissolving the reactive brilliant blue KN-R and the auxiliary reactive dye in water for mixing, then adding the emulsifier and the auxiliary salt, finally adding the buffering agent for adjusting to a proper pH value to obtain a mixed solution, and after uniformly mixing, carrying out spray drying to obtain the KN-R reactive dye composition.

Compared with the prior art, the invention has the beneficial effects that: the invention overcomes the sensitivity of the color absorbing and fixing behavior of the reactive brilliant blue KN-R between the reactive brilliant blue KN-R and the cotton fiber in the alkaline color fixing stage to alkali by adding the auxiliary reactive dye component on the basis of the existing reactive brilliant blue KN-R, compared with the single reactive brilliant blue KN-R, the auxiliary reactive dye component can absorb and occupy the site with the hydroxyl on the cotton fiber to form competitive absorption with the reactive brilliant blue KN-R, thereby greatly relieving the problem that the reactivity of covalent bond combination generated by the addition reaction of the vinyl sulfone group on the molecule of the reactive brilliant blue KN-R and the hydroxyl on the cotton fiber is too strong, ensuring uniform color absorbing and fixing and improving the alkali resistance of the reactive brilliant blue KN-R.

Drawings

FIG. 1 shows the results of the dyeability test of some examples of the present invention and comparative examples.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the specific embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

The KN-R reactive dye takes reactive brilliant blue KN-R as a main component, and is assisted by an auxiliary reactive dye, an emulsifier, auxiliary salts and a buffer, so that good dyeing performance is achieved. The invention aims to solve the technical problems that the reactive dye mainly comprising reactive brilliant blue KN-R is easy to generate uneven cloth surface color and even cloth surface color patterns.

The KN-R reactive dye is a common type of the prior industrial moderate-temperature blue reactive dye, and is generally obtained by condensing bromamine acid and m- (beta-sulfate ethyl sulfonyl) aniline. For example, the compound can be obtained by using the preparation method disclosed in CN101481535A and CN101481531A, and the structural formula of the compound is shown in formula I:

the auxiliary Reactive dye is generally used as a substitute dye of Reactive Blue 221 which is a common Reactive dye, mainly exists as an auxiliary component in the invention, and the structural formula of the auxiliary Reactive dye is shown as a formula II:

the auxiliary reactive dye can be prepared by the preparation process disclosed in KR 10-20050100056. According to the invention, the auxiliary reactive dye component is added into the KN-R reactive dye system, and tests show that the uniformity of the KN-R reactive dye is effectively improved, and the alkali resistance is improved. Through analysis, the auxiliary reactive dye component is also combined with the hydroxyl of the cellulose, so that the problem of excessively strong reactivity of covalent bond combination between the vinyl sulfone group on the reactive brilliant blue KN-R molecule and the hydroxyl on the cotton fiber through addition reaction is solved to a great extent, and more importantly, the auxiliary reactive dye molecule cannot be mutually adsorbed and associated with the KN-R fuel molecule, so that the problem of low dye-uptake property is caused.

The excellent effect of the KN-R reactive dye of the present invention will be illustrated below with reference to specific examples.

Example 1

80g of reactive Brilliant blue KN-R, 10g of auxiliary reactive dye were weighed out and mixed in 1200ML of water, and after complete mixing, 5g of sodium dodecyl sulfate and 4g of potassium chloride were added thereto, followed by 5g of sodium acetate for adjusting and stabilizing the pH of the combination. And then, spray drying the mixed solution to obtain the KN-R reactive dye composition.

Example 2

80g of reactive brilliant blue KN-R, 10g of auxiliary reactive dye are weighed and mixed in 1200ML of water, and after complete mixing, 5g of triethanolamine and 4g of lithium sulfate are added thereto, followed by 5g of sodium acetate for adjusting and stabilizing the pH of the combination. And then, spray drying the mixed solution to obtain the KN-R reactive dye composition.

Example 3

80g of reactive Brilliant blue KN-R, 10g of auxiliary reactive dye were weighed and mixed in 1200ML of water, and after complete mixing, 5g of OP-10 and 4g of sodium chloride were added thereto, followed by 5g of sodium borate for adjusting and stabilizing the pH of the combination. And then, spray drying the mixed solution to obtain the KN-R reactive dye composition.

Example 4

80g of reactive Brilliant blue KN-R, 10g of auxiliary reactive dye were weighed out and mixed in 1200ML of water, and after complete mixing, 4g of sodium dodecyl sulfate and 3g of potassium chloride were added thereto, followed by 1g of sodium acetate for adjusting and stabilizing the pH of the combination. And then, spray drying the mixed solution to obtain the KN-R reactive dye composition.

Example 5

80g of reactive brilliant blue KN-R, 8.7g of auxiliary reactive dye are weighed out and mixed in 1200ML of water, and after complete mixing, 5g of sodium dodecyl sulfate and 4g of potassium chloride are added thereto, followed by 5g of sodium acetate for adjusting and stabilizing the pH of the combination. And then, spray drying the mixed solution to obtain the KN-R reactive dye composition.

Example 6

60g of reactive brilliant blue KN-R, 10g of auxiliary reactive dye are weighed out and mixed in 1200ML of water, and after complete mixing, 5g of sodium dodecyl sulfate and 4g of potassium chloride are added thereto, followed by 5g of sodium acetate for adjusting and stabilizing the pH of the combination. And then, spray drying the mixed solution to obtain the KN-R reactive dye composition.

Example 7

80g of reactive brilliant blue KN-R, 8g of auxiliary reactive dye are weighed and mixed in 1200ML of water, and after complete mixing, 5g of sodium dodecyl sulfate and 4g of potassium chloride are added thereto, followed by 5g of sodium acetate for adjusting and stabilizing the pH of the combination. And then, spray drying the mixed solution to obtain the KN-R reactive dye composition.

Comparative example 1

90g of reactive brilliant blue KN-R are weighed and mixed in 1200ML of water, and after complete mixing, 5g of sodium dodecyl sulfate and 4g of potassium chloride are added thereto, followed by 5g of sodium acetate for adjusting and stabilizing the pH of the combination. And then, spray drying the mixed solution to obtain the KN-R reactive dye composition.

Comparative example 2

Reactive brilliant blue KN-RSR was prepared as disclosed in example 1 of CN 105199428A.

Comparative example 3

100g of auxiliary reactive dye are weighed out and mixed in 1200ML of water, and after complete mixing, 5g of sodium dodecyl sulfate and 4g of potassium chloride are added thereto, followed by 5g of sodium acetate for adjusting and stabilizing the pH of the combination. And then, spray drying the mixed solution to obtain the KN-R reactive dye composition.

Then, the performance of the reactive brilliant blue KN-R dyes obtained in the examples and the comparative examples of the invention is tested, and the specific test details are as follows:

(test for uniformity of Performance)

The reactive brilliant blue KN-R dye is prepared into dye solution, and the cotton fabric after scouring and bleaching is immersed into the dye solution for dyeing. And (3) testing the dyed fabric on a computer color measuring and matching instrument, randomly selecting 20 points on the fabric according to a mathematical statistical principle, measuring the surface color depth value at the maximum absorption wavelength, then calculating an average value, and calculating the dyed unevenness rate U, wherein the smaller the unevenness rate U value is, the better the leveling property is.

(alkali resistance test)

Adding 5g of reactive brilliant blue KN-R dye into 200mL of water, then preserving the temperature at 60 ℃ for 20min to fully dissolve the dye, cooling to room temperature, adding 100mL of Na containing 20g/L under stirring₂CO₃In the alkaline solution, samples were taken every 5min at 25 ℃ and their dissolution was observed by the dot method. Until the sample had a significant halo on the filter paper, the alkali resistance time was calculated.

(dyeing Performance test)

Preparing the reactive brilliant blue KN-R dye into dye solution, immersing the bleached cotton fabric into the dye solution for dyeing, preparing 50mL of solution from 2mL of residual liquid after dyeing for 5min, 10 min, 15 min, 20min, 25 min and 30min, measuring the absorbance of the solution, and calculating the percentage of dye.

(Friction and soaping fastness test)

And (3) testing the rubbing fastness: fixing a sample on a bottom plate of a testing machine by using a friction color fastness testing machine, fixing a friction cloth on a friction head of the testing machine, rubbing for 10 times within 10s, wherein the reciprocating stroke is 100mm, the vertical pressure is 9N, and evaluating the staining grade number on the friction cloth. Soaping fastness test: putting the sample into a container, injecting soap liquid preheated to 40 ℃ at a bath ratio of 50:1, treating the sample for 30min, taking out the sample, washing and drying the sample by using clear water, and evaluating the color change of the sample.

The results of the performance tests of the KN-R reactive dyes of the examples and comparative examples of the present invention are shown in Table 1:

the test results of the embodiment 1 and the comparative example 1 show that the leveling property and the alkali resistance of the cotton fiber are obviously improved by adopting the reactive brilliant blue KN-R and the auxiliary reactive dye, and the problem of excessively strong reactivity of covalent bond bonding between the vinyl sulfone group on the molecule of the reactive brilliant blue KN-R and the hydroxyl group on the cotton fiber through addition reaction is relieved to a certain extent by adding the auxiliary reactive dye. As can be seen from comparison between the example 1 and the comparative examples 1 and 2, the reactive brilliant blue KN-R dye of the invention has improved leveling property and alkali resistance compared with the dyes in the prior art, has enhanced leveling property and alkali resistance compared with the single auxiliary reactive dye, and has relatively lower cost.

The results of the dye-uptake performance tests of some examples and comparative examples of the present invention are shown in FIG. 1. it can be seen from the results that the dye-uptake performance of the present invention using reactive brilliant blue KN-R and the auxiliary reactive dye is reduced compared with the single reactive brilliant blue KN-R, but the dye-uptake rate at 35min still reaches 88%, and the dye-uptake rate at 35min is improved by 18% compared with the dye-uptake rate at 35min of comparative example 2 which is only about 70%. From the results of example 6 and example 7, it is understood that the dye uptake of example 6 is low, and the uniformity and alkali resistance of example 7 are somewhat lowered.

In conclusion, the reactive dye KN-R of the invention takes reactive brilliant blue KN-R as a main component, and the dyeing uniformity of the reactive dye is obviously improved by the aid of the auxiliary reactive dye, the dyeing property can be considered, the dyeing property is excellent, and the industrial application value is high.

The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.