CN109778561B - Method for recycling reactive dye dyeing salt of cellulose fiber based on ectopic mineralization technology - Google Patents

Method for recycling reactive dye dyeing salt of cellulose fiber based on ectopic mineralization technology Download PDF

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CN109778561B
CN109778561B CN201910067260.3A CN201910067260A CN109778561B CN 109778561 B CN109778561 B CN 109778561B CN 201910067260 A CN201910067260 A CN 201910067260A CN 109778561 B CN109778561 B CN 109778561B
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dyeing
residual liquid
cellulose fiber
acid
reactive dye
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CN109778561A (en
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邢建伟
徐成书
沈兰萍
苏广召
欧阳磊
魏欣月
郑文婷
李超
同晓妮
段喜莹
苏小桦
马靖
王志刚
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Xian Polytechnic University
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Abstract

The invention discloses a method for recycling dyeing salt of a cellulose fiber reactive dye based on an ectopic mineralization technology, which comprises the steps of firstly discharging dyeing residual liquid of the cotton fiber reactive dye and collecting the dyeing residual liquid to water storage equipment; carrying out ex-situ mineralization treatment on the dyeing residual liquid to obtain ex-situ mineralization residual liquid; subsequently conditioning the ex-situ mineralized raffinate in step 2; and finally, adding the ectopic mineralized residual liquid serving as dyeing water into dyeing equipment, and dyeing the textile to be dyed with reactive dye. The invention enables the inorganic salt for dyeing to be recycled continuously, remarkably reduces the discharge of the inorganic salt in the dyeing process and realizes the aim of the ectopic mineralization ultralow salt dyeing of the cellulose fiber reactive dye; the invention has important significance for further realizing green dyeing of the cellulose fiber reactive dye, reducing the dyeing processing cost and reducing the harm of inorganic salt to the environment.

Description

Method for recycling reactive dye dyeing salt of cellulose fiber based on ectopic mineralization technology
Technical Field
The invention belongs to the technical field of textile dyeing and finishing methods, and particularly relates to a method for recycling reactive dye dyeing salt of cellulose fibers based on an ectopic mineralization technology.
Background
During the dyeing process of the cellulose fiber reactive dye, a large amount of inorganic salt (generally anhydrous sodium sulphate or common salt) is required to be added to promote the dye to dye the fiber. After dyeing is finished, the inorganic salt is discharged together with dyeing residual liquid and enters a sewage treatment system. In the sewage treatment link, inorganic salts are difficult to remove and are often discharged along with treated water, thereby causing serious harm to the environment. Therefore, how to recover and reuse the inorganic salts is an important research topic.
Chinese patent ZL201510106886.2 discloses specific dyeing post-treatment method and related auxiliaries adopted in the method, and the disclosed dyeing method is actually a cellulose fiber reactive dye in-situ mineralization dyeing method.
A new cellulose fiber in-situ mineralization dyeing technology is introduced in a paper 'reactive dye in-situ mineralization dyeing of viscose wool tops' (printing and dyeing, 2017, No.19, p 17-21). The method specifically comprises the following steps: after the dyeing is finished, under the condition that the dyed fiber and the dyeing residual liquid coexist, the dyeing residual liquid is subjected to the in-situ mineralization treatment, so that the organic pollutants on the dyed fiber and in the dyeing residual liquid including the waste dye are converted into CO2And water, but the in-situ mineralization link cannot perform digestion on the waste inorganic salt in the dyeing residual liquid, and the waste inorganic salt enters the sewage treatment system along with the in-situ mineralization residual liquid.
In order to solve the problems, a Chinese patent 'ultra-low salt in-situ mineralization dyeing method for cellulose fiber reactive dyes' (application number: 201810298606.6) discloses a method for conditioning in-situ mineralization residual liquid and then using the conditioned in-situ mineralization residual liquid for subsequent dyeing of cellulose fibers. By adopting the method, the inorganic salt in the conditioned in-situ mineralized residual liquid can be recycled in the subsequent dyeing, thereby realizing the ultra-low salt dyeing processing.
It should be noted that in some dyeings with a more difficult-to-control shade (so-called "sensitive-color" dyeings), in-situ mineralization of the residual bath in the presence of the substrate often leads to a certain degree of variation in the shade of the finished dyeings, which leads to problems of the accuracy of the shade of the finished dyeings.
Disclosure of Invention
The invention aims to provide a recycling method of cellulose fiber reactive dye dyeing salt, which solves the problem that the recycling method of the dyeing salt in the Chinese patent 'cellulose fiber reactive dye ultra-low salt in-situ mineralization dyeing method' (application number: 201810298606.6) is easy to cause poor color accuracy of 'sensitive color' dyed products.
The technical scheme adopted by the invention is that the method for recycling the reactive dye dyeing salt of the cellulose fiber based on the ectopic mineralization technology comprises the following steps:
step 1, discharging cotton fiber reactive dye dyeing residual liquid and collecting the cotton fiber reactive dye dyeing residual liquid to water storage equipment;
step 2, carrying out ex-situ mineralization treatment on the dyeing residual liquid collected in the step 1 to obtain ex-situ mineralization residual liquid;
step 3, conditioning and recycling the ectopic mineralization residual liquid in the step 2;
step 4, adding the ectopic mineralization residual liquid treated in the step 3 into dyeing equipment as dyeing water, and dyeing the textile to be dyed with reactive dye;
and 5, collecting the residual liquid dyed in the step 4, and repeating the steps 1-4 to enable the ectopic mineralized residual liquid to be circularly used for subsequent reactive dye dyeing processing.
The present invention is also characterized in that,
the water storage device used in step 1 is any container or water pool with general acid-base resistance (the pH value is 2.5-12.0) and oxidation resistance.
The step 2 specifically comprises the following operations:
step 2.1, adjusting the temperature of the dyeing residual liquid discharged and collected in the step 1 to be 20-95 ℃;
step 2.2, adding an acid agent into the dyeing residual liquid obtained in the step 2.1, and adjusting the pH value of the dyeing residual liquid to 2.0-4.0;
step 2.3, adding a cellulose fiber dyeing post-treatment auxiliary agent XBC and a cellulose fiber dyeing post-treatment auxiliary agent XYC into the dyeing residual liquid treated in the step 2.2 in sequence;
and 2.4, circulating the dyeing residual liquid treated in the step 2.3 for 5-60 min in any mode to obtain the ectopic mineralized residual liquid.
The acid agent in step 2.2 is specifically: any one of sulfuric acid, hydrochloric acid, nitric acid, formic acid, acetic acid and citric acid or any combination of six acid agents.
In the step 2.3, the addition amount of the processing aid XBC after the cellulose fiber dyeing is 0.01-5.0% (w/w).
In the step 2.3, the addition amount of the cellulose fiber dyeing post-treatment auxiliary agent XYC is 0.01-10.0% (w/w).
The step 3 is specifically operated as follows:
step 3.1, adding an alkaline agent into the ex-situ mineralized residual liquid obtained in the step 2, wherein the pH range of the ex-situ mineralized residual liquid can be adjusted to 6.0-12.0 according to the principle of adding the alkaline agent;
step 3.2, filtering the ex-situ mineralized residual liquid after the treatment in the step 3.1, and filtering solid residues in the residual liquid;
step 3.3, after the treatment of the step 3.2, adding an acid agent into the ectopic mineralization residual liquid to adjust the pH value of the residual liquid to 6.0-8.0;
and 3.4, after the step 3.3, testing the content of the inorganic salt in the ex-situ mineralized residual liquid, and adjusting the content of the inorganic salt by supplementing the inorganic salt or water, wherein the principle of supplementing the inorganic salt or the water is that the concentration of the inorganic salt meets the requirement of the subsequent ex-situ mineralized dyeing of the cellulose fiber reactive dye.
The alkaline agent in step 3.1 is any one or the combination of any two or three of NaOH, KOH and Na2CO 3.
The acid agent added in the step 3.3 is specifically: any one of sulfuric acid, hydrochloric acid, nitric acid, formic acid, acetic acid and citric acid or any combination of six acid agents.
The method for recycling the reactive dye dyeing salt of the cellulose fiber based on the ectopic mineralization technology has the beneficial effects that: after the reactive dye for the cellulose fiber is dyed,discharging and collecting residual dyeing liquid, and ectopically mineralizing the residual dyeing liquid in water storage equipment or device to convert all organic pollutants including waste dye into CO2And water while retaining the dyeing inorganic salt contained therein; then conditioning the ex-situ mineralized residual liquid, filtering a small amount of flocculate and solid impurities, adjusting the flocculate and solid impurities to be neutral in acid and alkali, and applying the flocculate and solid impurities to subsequent dyeing of the cellulose fiber active dye to realize continuous recycling of inorganic salt for dyeing, remarkably reduce the discharge of inorganic salt in the dyeing processing process and realize the aim of dyeing the cellulose fiber active dye by the ex-situ mineralized ultralow salt; the method has important significance for further realizing green dyeing of the cellulose fiber reactive dye, reducing the dyeing processing cost and reducing the harm of inorganic salt to the environment.
Detailed Description
The present invention will be described in detail with reference to examples.
Aiming at the problem of color accuracy of the existing dyed products, the invention carries out dyeing processing on certain dyed products with difficult color control, discharges and stores dyeing raffinate after the dyeing link is finished, carries out ectopic mineralization on the dyeing raffinate under the condition that the dyeing raffinate is separated from the dyed products, and converts organic impurities including waste dyes in the dyeing raffinate into CO2And water, so that inorganic salt for dyeing is reserved, and then the residual liquid is conditioned, so that the residual liquid can be applied to the subsequent dyeing of the cellulose fiber reactive dye, and the recycling of the inorganic salt is realized.
The invention relates to a method for recycling cellulose fiber reactive dye dyeing salt based on an ectopic mineralization technology, which comprises the following steps:
step 1, discharging cotton fiber reactive dye dyeing residual liquid and collecting the cotton fiber reactive dye dyeing residual liquid to water storage equipment; specifically, the patent numbers: ZL201510106886.2, namely a dyeing residual liquid obtained in the step 1-2 in the cellulose fiber in-situ mineralization deep water-saving emission-reduction dyeing post-treatment method and auxiliary agent is discharged and enters a water storage device.
The water storage device used in step 1 is any container or water pool with general acid-base resistance (the pH value is 2.5-12.0) and oxidation resistance.
And 2, carrying out ex-situ mineralization treatment on the dyeing residual liquid collected in the step 1 to obtain the ex-situ mineralization residual liquid. The method specifically comprises the following steps:
step 2.1, adjusting the temperature of the dyeing residual liquid discharged and collected in the step 1 to be 20-95 ℃;
step 2.2, adding an acid agent into the dyeing residual liquid obtained in the step 2.1, and adjusting the pH of the dyeing residual liquid to 2.0-4.0, wherein the acid agent is specifically: any one of sulfuric acid, hydrochloric acid, nitric acid, formic acid, acetic acid and citric acid or any combination of six acid agents;
step 2.3, adding a cellulose fiber dyeing post-treatment auxiliary agent XBC and a cellulose fiber dyeing post-treatment auxiliary agent XYC into the dyeing residual liquid treated in the step 2.2 in sequence; the addition amount of the cellulose fiber dyeing post-treatment auxiliary agent XBC is 0.01-5.0% (w/w), and the addition amount of the cellulose fiber dyeing post-treatment auxiliary agent XYC is 0.01-10.0% (w/w);
wherein the cellulose fiber dyeing post-processing auxiliary agent XBC and the cellulose fiber dyeing post-processing auxiliary agent XYC are specifically disclosed in the patent numbers: ZL201510106886.2, named as 'cellulose fiber in-situ mineralization deep water-saving emission-reduction dyeing post-treatment method and auxiliary agent'.
And 2.4, circulating the dyeing residual liquid treated in the step 2.3 for 5-60 min in any mode to obtain the ectopic mineralized residual liquid.
And 3, conditioning and recycling the ectopic mineralization residual liquid in the step 2. And (3) carrying out in-situ mineralization and dyeing on the ex-situ mineralization residual liquid according to a patent of a cellulose fiber reactive dye ultralow salt in-situ mineralization dyeing method and an application number: 201810298606.6, conditioning and recycling the in-situ mineralized residual liquid in the steps 1-2.3.
The method specifically comprises the following steps:
step 3.1, adding an alkaline agent into the ex-situ mineralized residual liquid obtained in the step 2, wherein the pH range of the ex-situ mineralized residual liquid can be adjusted to 6.0-12.0 according to the principle of adding the alkaline agent; the alkaline agent is NaOH, KOH or Na2CO3Any one or a combination of any two or three of them.
Step 3.2, filtering the ex-situ mineralized residual liquid after the treatment in the step 3.1, and filtering solid residues in the residual liquid; the adopted filtering device is various liquid-solid filtering and separating devices with general acid-base resistance (pH is 2.5-12.0);
step 3.3, after the treatment of the step 3.2, adding an acid agent into the ectopic mineralization residual liquid to adjust the pH value of the residual liquid to 6.0-8.0;
and 3.4, after the step 3.3, testing the content of the inorganic salt in the ex-situ mineralized residual liquid, and adjusting the content of the inorganic salt by supplementing the inorganic salt or water, wherein the principle of supplementing the inorganic salt or the water is that the concentration of the inorganic salt meets the requirement of the subsequent ex-situ mineralized dyeing of the cellulose fiber reactive dye.
The adopted test method for the content of the inorganic salt is any existing test method, and the supplemented inorganic salt is anhydrous sodium sulphate or salt.
Step 4, adding the ectopic mineralization residual liquid treated in the step 3 into dyeing equipment as dyeing water, and dyeing the textile to be dyed with reactive dye;
and 5, collecting the residual liquid dyed in the step 4, and repeating the steps 1-4 to ensure that the ectopic mineralized residual liquid can be circularly used in the subsequent reactive dye dyeing processing to finish recycling.
Example 1
Discharging the dyeing residual liquid obtained in the steps 1-2 in the in-situ mineralization deep water-saving emission-reduction dyeing post-treatment method and the auxiliary agent of the cellulose fiber (patent number: ZL201510106886.2) into a water storage device, adjusting the temperature of the discharged and collected dyeing residual liquid to 60 ℃ through pipeline heat exchange, adding 0.7% (w/w) dilute sulfuric acid (30%, w/w) to the residual dyeing liquid under stirring to make the pH value of the residual dyeing liquid 3.0, mixing uniformly, adding 3.0% (w/w) of cellulose fiber dyeing auxiliary agent XBC into the dyeing residual liquid, mixing uniformly, adding cellulose fiber dyeing post-treatment auxiliary agent XYC into the dyeing residual liquid, wherein the adding amount is 5.0% (w/w), and carrying out ectopic mineralization reaction under the stirring condition for 30 min. After the ectopic mineralization reaction is finished, adding an alkaline agent NaOH into the obtained ectopic mineralization residual liquid, and adjusting the pH value of the ectopic mineralization residual liquid to be 10.0; filtering to remove solid residue in the residual liquid; sulfuric acid was added to the above filtrate to adjust the pH of the filtrate to 7.0. And testing the content of the inorganic salt in the filtrate, and adjusting the content of the inorganic salt by supplementing anhydrous sodium sulphate or water, wherein the principle of supplementing the inorganic salt or the water is that the concentration of the inorganic salt meets the requirement of the subsequent ex-situ mineralization dyeing of the cellulose fiber reactive dye.
Example 2
Discharging residual dyeing liquid obtained in the step 1-2 in a patent of cellulose fiber in-situ mineralization deep water-saving emission-reduction dyeing post-treatment method and auxiliary agent (patent number: ZL201510106886.2) into a water storage device, adjusting the temperature of the discharged and collected residual dyeing liquid to 70 ℃ through pipeline heat exchange, adding 0.8% (w/w) of hydrochloric acid into the residual dyeing liquid under the stirring condition to enable the pH value of the residual dyeing liquid to be 2.5, adding a cellulose fiber dyeing post-treatment auxiliary agent XBC into the residual dyeing liquid after uniform mixing in an amount of 3.5% (w/w), adding a cellulose fiber dyeing post-treatment auxiliary agent XYC into the residual dyeing liquid after uniform mixing in an amount of 6.0% (w/w), and carrying out mineralization ex-situ reaction under the stirring condition for 35 min. Adding an alkaline agent KOH into the obtained ectopic mineralization residual liquid, and adjusting the pH value of the ectopic mineralization residual liquid to 12.0; filtering to remove solid residue in the residual liquid; hydrochloric acid was added to the above filtrate to adjust the pH of the filtrate to 7.5. And testing the content of the inorganic salt in the filtrate, and adjusting the content of the inorganic salt by supplementing anhydrous sodium sulphate or water, wherein the principle of supplementing the inorganic salt or the water is that the concentration of the inorganic salt meets the requirement of the subsequent ex-situ mineralization dyeing of the cellulose fiber reactive dye.
Example 3
Discharging residual dyeing liquid obtained in the step 1-2 recorded in the 'cellulose fiber in-situ mineralization deep water-saving emission-reduction dyeing post-treatment method and auxiliary agent' (patent number: ZL201510106886.2) in a patent into water storage equipment, adjusting the temperature of the discharged and collected residual dyeing liquid to 75 ℃ through pipeline heat exchange, adding 0.3% (w/w) nitric acid into the residual dyeing liquid under stirring to enable the pH value of the residual dyeing liquid to be 2.3, and after uniform mixing, adding cellulose fiber into the residual dyeing liquidAdding 2.5% (w/w) of cellulose fiber dyeing post-treatment auxiliary agent XBC into the dyeing residual liquid after uniformly mixing, adding 4.0% (w/w) of cellulose fiber dyeing post-treatment auxiliary agent XYC into the dyeing residual liquid, and carrying out ectopic mineralization reaction under the stirring condition for 25 min. Adding an alkaline agent Na into the obtained ex-situ mineralized residual liquid2CO3Adjusting the pH value of the ectopic mineralization residual liquid to be 10.5; filtering to remove solid residue in the residual liquid; adding nitric acid into the filtrate, and adjusting the pH value of the filtrate to be 6.5; and testing the content of the inorganic salt in the filtrate, and adjusting the content of the inorganic salt by supplementing anhydrous sodium sulphate or water, wherein the principle of supplementing the inorganic salt or the water is that the concentration of the inorganic salt meets the requirement of the subsequent ex-situ mineralization dyeing of the cellulose fiber reactive dye.
Example 4
Discharging residual dyeing liquid obtained in the step 1-2 in a cellulose fiber in-situ mineralization deep water-saving emission-reduction dyeing treatment method and auxiliary agent (patent number: ZL201510106886.2) in a patent into a water storage device, adjusting the temperature of the discharged and collected residual dyeing liquid to 80 ℃ through pipeline heat exchange, adding 2.5% (w/w) of formic acid into the residual dyeing liquid under the stirring condition to enable the pH value of the residual dyeing liquid to be 2.8, adding a cellulose fiber dyeing post-treatment auxiliary agent XBC into the residual dyeing liquid after uniform mixing in an amount of 3.2% (w/w), adding a cellulose fiber dyeing post-treatment auxiliary agent XYC into the residual dyeing liquid after uniform mixing in an amount of 3.5% (w/w), and carrying out ex-situ mineralization reaction under the stirring condition for 40 min. Adding alkaline agents NaOH and Na into the obtained ex-situ mineralized residual liquid2CO3Adjusting the pH value of the ectopic mineralization residual liquid to be 11.5; filtering to remove solid residue in the residual liquid; adding formic acid into the filtrate, and adjusting the pH of the filtrate to 7.5; and testing the content of the inorganic salt in the filtrate, adjusting the content of the inorganic salt by supplementing salt or water, wherein the principle of supplementing the inorganic salt or the water is to ensure that the concentration of the inorganic salt meets the requirement of the subsequent ex-situ mineralization dyeing of the cellulose fiber reactive dye.
Example 5
Will be recorded in the patent "cellulose fibersThe dyeing residual liquid obtained in the step 1-2 in an in-situ mineralization deep water-saving emission-reduction dyeing post-treatment method and the auxiliary agent (patent number: ZL201510106886.2) is discharged into a water storage device, the temperature of the discharged and collected dyeing residual liquid is adjusted to 78 ℃ through pipeline heat exchange, 3.0% (w/w) of glacial acetic acid is added into the dyeing residual liquid under the stirring condition, the pH value of the dyeing residual liquid is 3.5, after uniform mixing, a cellulose fiber dyeing post-treatment auxiliary agent XBC is added into the dyeing residual liquid, the adding amount is 2.8% (w/w), after uniform mixing, a cellulose fiber dyeing post-treatment auxiliary agent XYC is added into the dyeing residual liquid, the adding amount is 3.2% (w/w), and ex-situ mineralization reaction is carried out under the stirring condition, and the reaction time is 45 min. Adding alkaline agents KOH and Na into the obtained ex-situ mineralized residual liquid2CO3Adjusting the pH value of the ectopic mineralization residual liquid to be 10.5; filtering to remove solid residue in the residual liquid; adding acetic acid into the filtrate, and adjusting the pH value of the filtrate to be 7.0; and testing the content of the inorganic salt in the filtrate, adjusting the content of the inorganic salt by supplementing salt or water, wherein the principle of supplementing the inorganic salt or the water is to ensure that the concentration of the inorganic salt meets the requirement of the subsequent ex-situ mineralization dyeing of the cellulose fiber reactive dye.
Example 6
Discharging residual dyeing liquid obtained in the step 1-2 in a cellulose fiber in-situ mineralization deep water-saving emission-reduction dyeing treatment method and auxiliary agent (patent number: ZL201510106886.2) in a patent into a water storage device, adjusting the temperature of the discharged and collected residual dyeing liquid to 65 ℃ through pipeline heat exchange, adding 2.5% (w/w) of citric acid into the residual dyeing liquid under the stirring condition to enable the pH value of the residual dyeing liquid to be 3.2, adding a cellulose fiber dyeing treatment auxiliary agent XBC into the residual dyeing liquid after uniform mixing in an amount of 4.0% (w/w), adding a cellulose fiber dyeing treatment auxiliary agent XYC into the residual dyeing liquid after uniform mixing in an amount of 7.0% (w/w), and carrying out ex-situ mineralization reaction under the stirring condition for 50 min. Adding alkaline agents NaOH and KOH into the obtained ectopic mineralization residual liquid, and adjusting the pH value of the ectopic mineralization residual liquid to be 11.5; filtering to remove solid residue in the residual liquid; adding formic acid and acetic acid into the filtrate, and adjusting the pH of the filtrate to be 7.0; and testing the content of the inorganic salt in the filtrate, adjusting the content of the inorganic salt by supplementing salt or water, wherein the principle of supplementing the inorganic salt or the water is to ensure that the concentration of the inorganic salt meets the requirement of the subsequent ex-situ mineralization dyeing of the cellulose fiber reactive dye.
In actual production, dyeing residual liquid obtained in the step 1-2 of the 'cellulose fiber in-situ mineralization deep water-saving emission-reduction dyeing post-treatment method and auxiliary agent (patent number: ZL 201510106886.2)' invented in China is discharged and collected, the method is adopted to carry out ex-situ mineralization on the residual liquid, then the ex-situ mineralization residual liquid is conditioned, the concentration of inorganic salt is adjusted, and then the obtained product is recycled in cellulose fiber reactive dye dyeing. Compared with the common dyeing method, the dosage of the inorganic salt for dyeing is obviously reduced. The relationship between the reduction of the dyed anhydrous sodium sulphate and the number of times the ectopically mineralized residual liquid is reused for dyeing is shown in table 1:
TABLE 1 relationship between reduction of anhydrous sodium sulfate and the number of times of ectopic mineralization residual liquid used for dyeing
Number of times of reuse (times) 1 2 3 4
Percentage (%) of decrease in the amount of anhydrous sodium sulfate 40 60 70 75

Claims (5)

1. The method for recycling the reactive dye dyeing salt of the cellulose fiber based on the ectopic mineralization technology is characterized by comprising the following steps of:
step 1, discharging cotton fiber reactive dye dyeing residual liquid and collecting the cotton fiber reactive dye dyeing residual liquid to water storage equipment;
step 2, carrying out ex-situ mineralization treatment on the dyeing residual liquid collected in the step 1 to obtain ex-situ mineralization residual liquid;
step 2.1, adjusting the temperature of the dyeing residual liquid discharged and collected in the step 1 to be 20-95 ℃;
step 2.2, adding an acid agent into the dyeing residual liquid obtained in the step 2.1, and adjusting the pH value of the dyeing residual liquid to 2.0-4.0;
step 2.3, adding a cellulose fiber dyeing post-treatment auxiliary agent XBC and a cellulose fiber dyeing post-treatment auxiliary agent XYC into the dyeing residual liquid treated in the step 2.2 in sequence;
the addition amount of the cellulose fiber dyeing post-treatment auxiliary agent XBC is 0.01-5.0% (w/w); the addition amount of the cellulose fiber dyeing post-treatment auxiliary agent XYC is 0.01-10.0% (w/w);
step 2.4, circulating the dyeing residual liquid treated in the step 2.3 for 5-60 min in any mode to obtain ectopic mineralized residual liquid;
step 3, conditioning the ectopic mineralization residual liquid in the step 2;
step 3.1, adding an alkaline agent into the ex-situ mineralized residual liquid obtained in the step 2, wherein the pH range of the ex-situ mineralized residual liquid can be adjusted to 6.0-12.0 according to the principle of adding the alkaline agent;
step 3.2, filtering the ex-situ mineralized residual liquid after the treatment in the step 3.1, and filtering solid residues in the residual liquid;
step 3.3, after the treatment of the step 3.2, adding an acid agent into the ectopic mineralization residual liquid to adjust the pH value of the residual liquid to 6.0-8.0;
step 3.4, after the step 3.3, testing the content of inorganic salt in the ex-situ mineralized residual liquid, and adjusting the content of the inorganic salt by supplementing the inorganic salt or water, wherein the principle of supplementing the inorganic salt or the water is that the concentration of the inorganic salt meets the requirement of the subsequent ex-situ mineralized dyeing of the cellulose fiber reactive dye;
step 4, adding the ectopic mineralization residual liquid treated in the step 3 into dyeing equipment as dyeing water, and dyeing the textile to be dyed with reactive dye;
and 5, collecting the residual liquid dyed in the step 4, and repeating the steps 1-4 to enable the ectopic mineralized residual liquid to be circularly used for subsequent reactive dye dyeing processing.
2. The method for recycling the dyeing salt of the cellulose fiber based on the ectopic mineralization technology as claimed in claim 1, wherein the water storage facility adopted in the step 1 is any container with acid and alkali resistance and oxidation resistance, and the acid and alkali resistance has a pH value of 2.5-12.0.
3. The method for recycling the dyeing salt of the cellulose fiber reactive dye based on the ectopic mineralization technology as claimed in claim 1, wherein the acid agent in the step 2.2 is specifically: any one of sulfuric acid, hydrochloric acid, nitric acid, formic acid, acetic acid and citric acid or any combination of six acid agents.
4. The method for recycling dyeing salt of cellulose fiber reactive dye based on ectopic mineralization technology as claimed in claim 1, wherein the alkaline agent in step 3.1 is NaOH, KOH or Na2CO3Any one or a combination of any two or three of them.
5. The method for recycling the dyeing salt of the cellulose fiber reactive dye based on the ectopic mineralization technology as claimed in claim 1, wherein the acid agent added in the step 3.3 is specifically: any one of sulfuric acid, hydrochloric acid, nitric acid, formic acid, acetic acid and citric acid or any combination of six acid agents.
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