阅读说明：本技术 天然蛋白质纤维高色牢度染品原位矿化染色方法 (In-situ mineralization dyeing method for natural protein fiber high-color-fastness dye ) 是由 邢建伟 沈兰萍 徐成书 欧阳磊 苏广召 任燕 师文钊 陆少锋 刘瑾姝 张晶 ** 于 2019-11-05 设计创作，主要内容包括：本发明公开的天然蛋白质纤维高色牢度染品原位矿化染色方法,包括：将待染色纺织品置入染色设备中,第一次加入软水,保持染浴循环；进行染色加工,染色结束后暂不排放染色残液；将染色残液降温,随后加入XFL保温循环,排放第一次残液；第二次加入软水,升温循环处理,排放第二次残液；第三次加入软水,随后依次加入XBM和XYM,循环均匀后升温并保温,排放第三次残液；第四次加入软水,升温后循环处理,排放第四次残液。本发明原位矿化染色方法通过原位矿化方法的实施,在保证染品相关色牢度指标的前提下,达到节约用水50％,使染色流程显著缩短,提高生产效率,同时实现节能的效果。(The invention discloses an in-situ mineralization dyeing method of a natural protein fiber high-color-fastness dye product, which comprises the following steps: putting the textile to be dyed into dyeing equipment, adding soft water for the first time, and keeping the dye bath circulation; carrying out dyeing processing, and after dyeing is finished, temporarily not discharging dyeing residual liquid; cooling the dyeing residual liquid, adding XFL heat preservation circulation, and discharging the first residual liquid; adding soft water for the second time, heating for circulation treatment, and discharging the second residual liquid; adding soft water for the third time, then sequentially adding XBM and XYM, uniformly circulating, heating and preserving heat, and discharging the residual liquid for the third time; adding soft water for the fourth time, heating, performing circulation treatment, and discharging the fourth residual liquid. The in-situ mineralization dyeing method achieves 50 percent of water saving by implementing the in-situ mineralization method on the premise of ensuring the related color fastness index of the dye, obviously shortens the dyeing process, improves the production efficiency and realizes the effect of energy saving.)

1. The in-situ mineralization dyeing method of the natural protein fiber high-color-fastness dye is characterized by comprising the following steps:

step 1, preparation link before dyeing

Putting the textile to be dyed into dyeing equipment, adding soft water for the first time, and keeping the dye bath circulation;

step 2, dyeing processing and post-treatment links

Dyeing the textile to be dyed in the step 1, and after dyeing is finished, temporarily not discharging dyeing residual liquid;

step 3, cooling the dyeing residual liquid in the step 2 in a heat exchange mode, then adding an auxiliary agent XFL for dye and fiber separation for heat preservation circulation, and discharging the first residual liquid;

step 4, adding soft water into the dyeing equipment treated in the step 3 for the second time, performing heating circulation treatment, and discharging second residual liquid;

step 5, adding soft water into the dyeing equipment treated in the step 4 for the third time, sequentially adding the natural protein fiber dyeing post-treatment auxiliary XBM and the natural protein fiber dyeing post-treatment auxiliary XYM, uniformly stirring, heating and preserving heat, and then discharging a third residual liquid;

and 6, adding soft water into the dyeing equipment treated in the step 5 for the fourth time, performing circulating treatment after heating, then discharging the residual liquid for the fourth time, and finishing dyeing.

2. The in-situ mineralization dyeing method for natural protein fiber high-fastness dyed products, according to claim 1, wherein the dyeing equipment in the step 1 is any one of a loose fiber dyeing machine, a top dyeing machine, a cheese dyeing machine, a hank dyeing machine, a garment dyeing machine, a jig dyeing machine, an overflow dyeing machine and an airflow dyeing machine.

3. The in-situ mineralization dyeing method of natural protein fiber high-color fastness dyeings according to claim 1, wherein the textiles to be dyed in step 1 are any one of wool fibers, cashmere fibers, camel wool fibers, yak wool fibers, mohair fibers, alpaca fibers, rabbit hair fibers, fox wool fibers, silk fibers, yarns spun from the fibers and woven fabrics.

4. The in-situ mineralization dyeing method of natural protein fiber high-fastness dye according to any one of claims 1 to 3, wherein the temperature of the soft water added in four times in the steps 1 to 6 is 25 ℃ to 35 ℃.

5. The in-situ mineralization dyeing method of a natural protein fiber high-color-fastness dye product according to claim 1, wherein in the step 3, the temperature of the dyeing residual liquid is reduced to 70-90 ℃;

the amount of the auxiliary agent XFL for separating the dye and the fiber is 0.001-10% owf, and the heat preservation circulation is carried out for 1-30 min.

6. The in-situ mineralization dyeing method of a natural protein fiber high-color-fastness dyed product according to claim 1, wherein the temperature rise in the step 4 is 70-90 ℃, and the cycle treatment time is 1-30 min.

7. The in-situ mineralization dyeing method of a natural protein fiber high-color-fastness dye product according to claim 1, wherein the dosage of the natural protein fiber dyeing post-treatment auxiliary agent XBM in the step 5 is 0.001% owf-10% owf; the dosage of the treatment auxiliary agent XYM after the natural protein fiber is dyed is 0.001-10% owf;

the temperature is raised to 60-95 ℃, and the heat preservation time is 5-60 min.

8. The in-situ mineralization dyeing method of natural protein fiber high-color-fastness dyeings according to claim 1, wherein the temperature rise in step 6 is to 40 ℃ to 60 ℃, and the cyclic treatment is performed for 5min to 60min.

9. The in-situ mineralization dyeing method of natural protein fiber high-fastness dyed products as claimed in claim 1, wherein the mass ratio of the soft dyeing water added in four times in the steps 1-5 to the textile to be dyed is 7-11: 1.

Technical Field

The invention belongs to the technical field of fiber dyeing methods, and particularly relates to an in-situ mineralization dyeing method for a natural protein fiber high-color-fastness dye product.

Background

Chinese patent No. 20150311, No. CN201510107510.3, No. 20161207, No. CN104711872B discloses a method for in-situ mineralization and deep water-saving emission-reducing dyeing post-treatment of residual bath and dyed fiber after dyeing of natural protein fiber, and also discloses related auxiliary agents, such as XAM (natural protein fiber dyeing post-treatment auxiliary), XBM (natural protein fiber dyeing post-treatment auxiliary) and XYM (natural protein fiber dyeing post-treatment auxiliary).

Chinese patent No. 20160623; application No. CN 201610466482.9; publication No. 20181204; publication No. CN106120404B) discloses an auxiliary agent for separating dye and fiber in protein fiber in-situ mineralization dyeing, and discloses a composition and a using method of the auxiliary agent XFL for separating dye and fiber.

The new technology of in-situ mineralization dyeing of wool top reactive dyes (wool spinning technology, volume 43, phase 10, 10 months 2015) describes a process of in-situ mineralization dyeing of wool fibers for worsted fabrics.

The core contents of the above publications and patents are: under the condition of coexistence of dyed fiber and dyeing residual bath, organic pollutants on a dyed product and in the residual bath are digested into CO through in-situ mineralization₂And water is mixed, so that water for cleaning dyed products is reduced, the pollution load of discharged wastewater is reduced, and the aim of saving energy can be fulfilled by shortening the dyeing process flow.

Meanwhile, the disclosed technology is suitable for dyeing high-quality (relatively high-purity) wool reactive dyes. In fact, when dyeing with reactive dyes for wool of medium or low quality (i.e. relatively low purity), the soaping fastness of the dyeings obtained is low due to the presence of a large amount of colored impurities in such dyes. The low-medium quality wool reactive dye has relatively low price and is widely applied to domestic enterprises. Therefore, in order to make the in-situ mineralization dyeing technology of natural protein fibers suitable for dyeing of reactive dyes for all quality wool, a corresponding dyeing process needs to be developed, so that various color fastness of corresponding dyed products can meet the requirements of product quality, and meanwhile, the in-situ mineralization water-saving emission-reduction dyeing technology can be widely applied.

Disclosure of Invention

The invention aims to provide an in-situ mineralization dyeing method for a natural protein fiber high-color fastness dye, which solves the problem that the existing dyeing method is not suitable for low-medium-quality (namely relatively low-purity) wool reactive dyes.

The technical scheme adopted by the invention is that the in-situ mineralization dyeing method of the natural protein fiber high-color-fastness dye comprises the following steps:

step 1, preparation link before dyeing

Putting the textile to be dyed into dyeing equipment, adding soft water for the first time, and keeping the dye bath circulation;

step 2, dyeing processing and post-treatment links

Dyeing the textile to be dyed in the step 1 according to a method for dyeing natural protein fibers by using common reactive dyes for wool, and after dyeing is finished, temporarily not discharging dyeing residual liquid;

step 3, cooling the dyeing residual liquid in the step 2 in a heat exchange mode, then adding an auxiliary agent XFL for dye and fiber separation for heat preservation circulation, and discharging the first residual liquid;

step 4, adding soft water into the dyeing equipment treated in the step 3 for the second time, performing heating circulation treatment, and discharging second residual liquid;

step 5, adding soft water into the dyeing equipment treated in the step 4 for the third time, sequentially adding a natural protein fiber dyeing post-treatment auxiliary XBM and a natural protein fiber dyeing post-treatment auxiliary XYM, uniformly circulating, heating and preserving heat, and then discharging a third residual liquid;

and 6, adding soft water into the dyeing equipment treated in the step 5 for the fourth time, performing circulating treatment after heating, then discharging the residual liquid for the fourth time, and finishing dyeing.

The present invention is also characterized in that,

the dyeing equipment in the step 1 is any one of a loose fiber dyeing machine, a top dyeing machine, a cheese dyeing machine, a hank dyeing machine, a garment dyeing machine, a jig dyeing machine, an overflow dyeing machine or an airflow dyeing machine.

The textile to be dyed in the step 1 is any one of wool fiber, cashmere fiber, camel fiber, yakwool fiber, mohair fiber, alpaca fiber, rabbit hair fiber, fox wool fiber, silk fiber, yarn spun by the fibers and fabric woven by the fibers.

The temperature of the dyeing soft water added for four times in the steps 1 to 6 is 25 to 35 ℃.

Cooling the dyeing residual liquid to 70-90 ℃ in the step 3;

the dosage of the auxiliary agent XFL for separating the dye and the fiber is 0.001-10% owf, and the heat preservation circulation is 1-30 min.

In the step 4, the temperature is raised to 70-90 ℃, and the circulating treatment time is 1-30 min.

In the step 5, the dosage of the processing aid XBM after the natural protein fiber is dyed is 0.001-10% owf; the dosage of the treatment auxiliary agent XYM after the natural protein fiber is dyed is 0.001-10% owf;

the temperature is raised to 60-95 ℃, and the heat preservation time is 5-60 min.

In step 6, the temperature is raised to 40-60 ℃, and the circulation treatment is carried out for 5-60 min.

The mass ratio of the soft water added in the steps 1 to 6 to the textile to be dyed is 7-11: 1.

The invention has the beneficial effects that: the in-situ mineralization dyeing method of the natural protein fiber high-color-fastness dyed product utilizes the natural protein fiber dyeing post-treatment auxiliary agent XBM and the natural protein fiber dyeing post-treatment auxiliary agent XYM to carry out in-situ mineralization treatment on the dyed product, and through the improvement of the dyeing process and the dyeing process, the related color fastness index of the dyed product obtained by adopting the lower-quality wool reactive dye can reach the quality requirement; through the implementation of the in-situ mineralization dyeing method, on the premise of ensuring the relevant color fastness index of the dyed product, compared with the traditional dyeing process, the purpose of saving water by about 50 percent is achieved, the dyeing process is obviously shortened, the production efficiency is improved, and meanwhile, the energy-saving effect is realized.

Drawings

FIG. 1 is a graph of temperature rise of a conventional dyeing method;

wherein A represents acetic acid and leveling agent, B represents reactive dye for wool, C represents first soda ash, D represents first detergent, E represents second soda ash, F represents second detergent, and G represents last acetic acid;

FIG. 2 is a graph of the temperature rise of the dyeing process of the present invention;

wherein A is^lDenotes acetic acid, microsuspension dyeing assistant, B^lDenotes a reactive dye for wool, C^lAuxiliary XFL, D for dye and fibre separation^lDenotes the natural protein fiber dyeing auxiliary agent XYM, E^lRepresents a natural protein fiber dyeing post-treatment assistant XYM.

Detailed Description

The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.

As shown in fig. 1, the vertical direction represents temperature, and the horizontal direction represents time, which are temperature rise graphs of the conventional dyeing method. In the dyeing process of adopting the traditional dyeing method of natural protein fibers, firstly adding dyeing auxiliary agents (such as acetic acid and leveling agent represented by A) and dyes (such as reactive dyes for wool represented by B), heating the dyeing bath to 90-98 ℃ at the heating rate of 0.5-1.0 ℃/min, preserving the temperature for 60-90 min, and then discharging dyeing residual liquid; then adding fresh water, respectively adding soda ash (shown as C in figure 1) and detergent (shown as D in figure 1), circulating uniformly, heating the treatment bath to 80 deg.C, treating for 20min, and discharging residual liquid; adding new water again, heating the treatment bath to 80 ℃, treating for 20min, and discharging residual liquid; adding fresh water for the fourth time, respectively adding soda ash (shown as E in figure 1) and detergent (shown as F in figure 1), circulating uniformly, heating the treatment bath to 80 deg.C, treating for 20min, and discharging residual liquid; adding new water for the fifth time, heating the treatment bath to 80 ℃, treating for 10min, and discharging residual liquid; then washing 2 times at 80 deg.C (i.e. repeating the fourth and fifth times); finally, acetic acid (shown as G in FIG. 1) is added, and the dyeing process is finished after the treatment is carried out for 10min at 50 ℃.

Therefore, the dyeing process has more links, larger water consumption and discharge capacity, high consumption and low efficiency, and is not beneficial to the sustainable development of the textile dyeing and finishing industry.

The invention relates to an in-situ mineralization dyeing method of a natural protein fiber high-color-fastness dye product, which comprises the following steps:

step 1, a preparation link before dyeing: placing the textile to be dyed into dyeing equipment, adding soft water with the temperature of 25-35 ℃ for the first time, and keeping the dye bath circulation.

The dyeing equipment is any one of loose fiber dyeing machine, top dyeing machine, cheese dyeing machine, hank dyeing machine, garment dyeing machine, jig dyeing machine, overflow dyeing machine and airflow dyeing machine.

The textile to be dyed is any one of wool fiber, cashmere fiber, camel hair fiber, yak hair fiber, mohair fiber, alpaca fiber, rabbit hair fiber, fox hair fiber, silk fiber, yarn spun by the fibers and woven fabric.

The mass ratio of the soft water for dyeing to the textile to be dyed is 7-11: 1.

Step 2, dyeing processing and post-treatment links

And (3) dyeing the textile to be dyed treated in the step (1), and after dyeing is finished, temporarily not discharging dyeing residual liquid. The dyeing process specifically comprises the following steps: the textile to be dyed in step 1 is dyed according to a method of dyeing natural protein fibers by using a general reactive dye for wool.

Step 3, cooling the dyeing residual liquid in the step 2 to 70-90 ℃ in a heat exchange mode, then adding 0.001-10% owf of dye and fiber separation auxiliary agent XFL, performing heat preservation circulation for 1-30 min, and discharging the first residual liquid; XFL is added to ensure that waste dye on a dyed product enters dyeing residual liquid; the mass ratio of the soft water for dyeing to the textile to be dyed is 7-11: 1.

Step 4, adding soft water into the dyeing equipment treated in the step 3 for the second time, heating to 70-90 ℃, circularly treating for 1-30 min, and discharging second residual liquid; the mass ratio of the soft water for dyeing to the textile to be dyed is 7-11: 1.

Step 5, adding soft water into the dyeing equipment treated in the step 4 for the third time, sequentially adding a natural protein fiber dyeing post-treatment auxiliary agent XBM with 0.001% -owf and 10% -owf and a natural protein fiber dyeing post-treatment auxiliary agent XYM with 0.001% -owf and 10% -owf, uniformly stirring, raising the temperature to 60-95 ℃, preserving the temperature for 5-60 min, and then discharging a third residual liquid; the mass ratio of the soft water for dyeing to the textile to be dyed is 7-11: 1.

The XBM and XYM are added to simultaneously carry out in-situ mineralization treatment on the dye and the residual bath, so that organic pollutants including waste dyes on the dye and the residual bath are mainly digested into CO₂And water.

And 6, adding soft water into the dyeing equipment treated in the step 5 for the fourth time, heating to 40-60 ℃, circularly treating for 5-60 min, discharging the fourth residual liquid, and finishing dyeing.

As shown in FIG. 2, the temperature rise curve of the dyeing method of the present invention is shown in the horizontal direction for time and in the vertical direction for temperature. By comparison with conventional dyeing processes and methods, it can be seen that: the dyeing process and the method can obviously reduce the water consumption in the dyeing process of the natural protein fibers, and can obviously reduce the pollution load of discharged residual liquid by implementing an in-situ mineralization method; due to the reduction of cleaning links, the dyeing time can be shortened, the processing efficiency is improved, and the energy-saving effect is realized.