CN113562919A - System for recycling salt in dyeing raffinate of reactive dye based on fiber ectopic mineralization technology - Google Patents

System for recycling salt in dyeing raffinate of reactive dye based on fiber ectopic mineralization technology Download PDF

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CN113562919A
CN113562919A CN202110921334.2A CN202110921334A CN113562919A CN 113562919 A CN113562919 A CN 113562919A CN 202110921334 A CN202110921334 A CN 202110921334A CN 113562919 A CN113562919 A CN 113562919A
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salt
dyeing
value conditioning
raffinate
ectopic mineralization
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徐成书
邢建伟
沈兰萍
苏广召
欧阳磊
任燕
王立
陆少锋
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Xi'an Wanzi Fine Chemical Technology Co ltd
Xian Polytechnic University
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Xi'an Wanzi Fine Chemical Technology Co ltd
Xian Polytechnic University
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5281—Installations for water purification using chemical agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F2001/007—Processes including a sedimentation step
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions

Abstract

The invention discloses a system for recycling dyeing raffinate salt of an active dye based on a cellulose fiber ectopic mineralization technology, which comprises a dyeing raffinate collecting device, an ectopic mineralization reaction device, a first pH value conditioning device, a first filtering device, a second pH value conditioning device, a second filtering device and a pure brine storage device which are sequentially connected through pipelines, wherein a first turbid liquid outlet is arranged at the bottom of the first pH value conditioning device and communicated with an inlet of a first precipitate shunting collecting device, a second turbid liquid outlet is arranged at the bottom of the second pH value conditioning device and communicated with an inlet of a second precipitate shunting collecting device, and power devices are arranged among the devices, so that the purification treatment of the dyeing raffinate of the active dye can be realized through the system, the recycling of the dyeing raffinate salt of the active dye by the cellulose fiber ectopic mineralization treatment can be realized, the content of inorganic salt in the sewage generated by dyeing processing is obviously reduced.

Description

System for recycling salt in dyeing raffinate of reactive dye based on fiber ectopic mineralization technology
Technical Field
The invention belongs to the technical field of water saving and emission reduction in textile printing and dyeing processing, and particularly relates to a system for recycling salt in dyeing residual liquid of reactive dye based on a fiber ectopic mineralization technology.
Background
In the application process of the reactive dye, the dye molecules usually contain water-soluble groups such as sulfonic sodium salt, hydroxyl, amino and the like so as to have water solubility, and the groups are ionized in the dyeing process so that the dye is negatively charged. Removal of hydrogen ions from the hydroxyl groups of cellulose macromolecules to form Cell-O－So that the fiber itself is also negatively charged, and the fiber are charged in the same way, so that electrostatic repulsion exists, and the reactive dye is prevented from dyeing the cellulose fiber. In order to improve the utilization rate of the reactive dye, a large amount of inorganic salt (sodium chloride or sodium sulfate, generally 10-100g/L) is required to be added during dyeing, sodium ions ionized by the inorganic salt shield negative charges of cellulose fibers, the adsorption and dyeing of the dye on the fibers are promoted, and the adsorption rate and the balanced adsorption capacity of the reactive dye are improved.
After the inorganic salt dyeing promotion is finished, an alkaline agent is added for color fixation (0.5-4.0 g/L of substitute alkali or 5-30g/L of soda ash). The fixation alkaline agent can enable hydroxyl on cellulose macromolecules to perform leaving reaction to form cellulose anions, at the moment, the active groups of the dye can perform nucleophilic reaction (nucleophilic substitution or nucleophilic addition reaction) with the cellulose macromolecules, so that the active dye and the cellulose macromolecules are covalently combined, and the other part of the dye can perform hydrolysis reaction.
Figure BDA0003207514270000011
Dye-SO2CH2CH20SO3Na+NaOH→Dye-SO2CH＝CH2+Na2SO4+H2O
Dye+SO2CH＝CH2+Na2SO4+Cell-OH→Dye-SO2CH2CH2Cell (nucleophilic addition)
The utilization rate of the reactive dye is low due to the characteristics of the reactive dye, the fixation rate is generally 50% -70%, so that the chromatic value of the dyeing residual liquid of the reactive dye is large, the pollutant content is high, a large amount of inorganic salt (containing basic salt) exists in the dyeing residual liquid, the inorganic salt cannot be effectively treated during sewage treatment, the discharge of the dyeing wastewater tends to destroy the surrounding ecological environment, soil salt and alkalization are caused, the ecological system is seriously destroyed, and based on the problems existing in the treatment of the dyeing residual liquid of the reactive dye, the method for recycling the salt of the dyeing residual liquid of the reactive dye based on the cellulose fiber ectopic mineralization technology is provided. If the existing brine recycling system based on the acid regulating system, the oil removing system and the back extraction system is used, the pH value of dyeing residual liquid is regulated to be below 3.0 in the acid regulating system in the application process, then an extracting agent and the acidified dyeing residual liquid are fully mixed in an extraction tower, a cationized extracting agent adsorbs active dye molecules and enters oil phase components of the extracting agent, but the extraction system cannot overcome the acting force between the active dye molecules and water molecules, the chroma of the acidic dyeing residual liquid in the extraction tower is still obvious, the chroma of brine prepared at a water outlet of the extraction tower is higher, and the separation efficiency of the oil phase extracting agent and the dye molecules separated in the extraction tower is not high, so that the brine recycling system has many defects in the practical application process and can only meet the recycling dyeing requirements of deep color products.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a system for recycling salt of dyeing raffinate of reactive dye based on a fiber ectopic mineralization technology, which provides a set of complete system and equipment for recycling salt of dyeing raffinate of cellulose fiber reactive dye, purifies the dyeing raffinate of the cellulose fiber reactive dye, and recycles the obtained pure brine for subsequent dyeing processing to realize the recycling of inorganic salt.
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides an active dyestuff dyeing raffinate salt recycling system based on fibre ectopic mineralization technique, includes dyeing raffinate collection device, ectopic mineralization reaction unit, first pH value conditioning device, first filter equipment, second pH value conditioning device, second filter equipment and net salt water storage device that connect gradually through the pipeline, first pH value conditioning device bottom sets up first turbid liquid export, first turbid liquid export and first precipitate reposition of redundant personnel collection device's import intercommunication, second pH value conditioning device bottom sets up turbid liquid export under the second, turbid liquid export and second precipitate reposition of redundant personnel collection device's entry intercommunication under the second, all dispose power device between the above-mentioned device.
Further, the ectopic mineralization reaction device comprises a temperature measuring device, a steam heating device, a stirring shaft, a dyeing raffinate inlet and an ectopic mineralization raffinate outlet; the temperature measuring device is arranged on the inner wall of the ectopic mineralization reaction device and is used for monitoring the temperature of the ectopic mineralization reaction system; the steam heating device is arranged at the bottom of the ectopic mineralization reaction device and is used for heating the ectopic mineralization system; the connecting end of the stirring shaft is rotationally connected with the top of the ectopic mineralization reaction device; the dyeing residual liquid inlet is arranged at the top of the ectopic mineralization reaction device and is communicated with the outlet of the dyeing residual liquid collection device through a pipeline; and the ectopic mineralization residual liquid outlet is arranged at the bottom of the ectopic mineralization reaction device and is communicated with the inlet of the first pH value conditioning device through a pipeline.
Further, the ectopic mineralization reaction device is provided in plurality.
Further, the first pH value conditioning device comprises a liquid internal circulation power device, an aeration device, an ectopic mineralized residual liquid inlet, a first turbid liquid outlet and a first supernatant liquid outlet, wherein an opening is formed in the bottom of the side surface of the first pH value conditioning device, and the opening is provided with the liquid internal circulation power device used for liquid circulation during pH value adjustment; the aeration device is arranged at the bottom of the first pH value conditioning device and is used for accelerating the liquid circulation in the first pH value conditioning device; the ex-situ mineralized raffinate inlet is arranged at the top of the first pH value conditioning device and is communicated with the ex-situ mineralized raffinate outlet; the first turbid liquid outlet is arranged at the bottom of the first pH value conditioning device, and the first supernatant liquid outlet is arranged on the side wall of the upper part of the first pH value conditioning device and is communicated with the inlet of the first filtering device to filter the first supernatant liquid.
Further, the power device for internal circulation of liquid comprises a pipeline and a power pump, wherein the pipeline is communicated with the side surface and the upper opening of the first pH value conditioning device, and the power pump is arranged on the pipeline and is used for realizing internal circulation of liquid in the first pH value conditioning device from bottom to top.
Further, the first pH value conditioning device is used for adjusting the pH value of the ectopic mineralization residual liquid to be alkaline; the second pH value conditioning device is used for adjusting the pH value of the filtered first supernatant to be neutral.
Further, the first filtering device and the second filtering device are both bag filters, and the filtering size of the first filtering device is 5-10 μm; the second filter unit has a filter size of 1 μm to 5 μm.
Further, first deposit reposition of redundant personnel collection device and second deposit reposition of redundant personnel collection device all include subsides device and collecting pit, subside device and collecting pit pass through the pipeline intercommunication, set up control flap on the pipeline, subside the device and be arranged in subsiding again of deposit under first turbid liquid and the second turbid liquid, the collecting pit is used for collecting the deposit that subsides again.
Further, the first and second split-flow collecting devices for the precipitate are made of salt-resistant and alkali-resistant materials.
Furthermore, the dyeing residual liquid collecting device and the corresponding connecting pipelines meet the material requirements of salt resistance, alkali resistance and high temperature; the ectopic mineralization reaction device and the corresponding connecting pipeline meet the requirements of materials for salt resistance, acid resistance, alkali resistance, high temperature resistance and oxidation resistance; the first pH value conditioning device, the second pH value conditioning device and the corresponding connecting pipelines meet the requirements of salt resistance, acid resistance, alkali resistance, high temperature and oxidation resistance; the first filtering device, the second filtering device and the corresponding connecting pipelines all meet the material requirements of salt resistance and alkali resistance; the pure brine storage device and the corresponding connecting pipeline meet the requirement of salt-resistant materials.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention provides a recycling system of active dye dyeing raffinate salt based on a fiber ectopic mineralization technology, which realizes the purification treatment of active dye dyeing raffinate under the combined action of an ectopic mineralization reaction device, a first pH value conditioning device, a first precipitate shunting collection device, a first filtering device, a second pH value conditioning device, a second precipitate shunting collection device and a second filtering device, wherein the obtained brine after treatment can meet the recycling requirement of subsequent dyeing; the method has important significance for further realizing clean dyeing of the cellulose fiber reactive dye, reducing the dyeing processing cost and reducing the harm of inorganic salt to the ecological environment.
In the ectopic mineralization reaction device and the ectopic mineralization reaction system, the active dyeing residual liquid in the dyeing workshop is uniformly collected by a residual liquid collecting device; adding reaction agent into the ectopic mineralization reaction device, starting a liquid circulation and heat supply device to promote the ectopic mineralization reaction, and converting organic pollutants in the dyeing residual liquid into CO in the ectopic mineralization reaction device2And water, the inorganic salt for dyeing contained in it is retained; in the first pH value conditioning device, the pH value conditioning is carried out on the obtained ectopic mineralized residual liquid, so that the residual auxiliary agent in the residual liquid can form a three-dimensional net structure, micro impurities in the ectopic mineralized residual liquid are captured, larger granular floccule precipitates are formed, the separate collection of the precipitates is facilitated, and the floccule and solid impurities in the precipitate can be conveniently filtered(ii) a The filtrate is conveyed to a second pH conditioning device through a first filtering device, and the first filtering device can filter out cellulose short fibers and a small amount of residual mineralized auxiliary agent; and adjusting the pH value of the treatment liquid to be nearly neutral in a second pH conditioning device, and further filtering a small amount of solid impurities through a second filtering device to obtain clean brine.
Description of the drawings:
FIG. 1 is a schematic flow chart of a system for recycling salt from dyeing residual liquid of reactive dye in the ectopic mineralization technology of cellulose fibers;
FIG. 2 is a schematic view of an ectopic mineralization reactor of the present invention;
FIG. 3 is a schematic diagram of a pH conditioning system according to the present invention;
in the drawings: 1. a dyeing residual liquid collecting device; 2. an ectopic mineralization reaction device; 21. a temperature measuring device; 22. a steam heating device; 23. a stirring shaft; 24. dyeing residual liquid is imported; 25. an ectopic mineralized residual liquid outlet; 3. a first pH conditioning device; 31. a liquid internal circulation power device; 32. an aeration device; 33. an ectopic mineralized residual liquid inlet; 34. an air outlet of the aeration device; 35. a first lower turbid liquid outlet; 36. a first supernatant outlet; 4. a first precipitate shunting and collecting device; 5. a first filtering device; 6. a second pH value conditioning device; 7. a second precipitate shunting and collecting device; 8. a second filtering device; 9. a purified brine storage device.
Detailed Description
The present invention will be described in detail with reference to the following examples and drawings.
As shown in fig. 1, the present invention provides a system for recycling salt from dyeing raffinate of reactive dyes based on a fiber ectopic mineralization technology, which comprises a dyeing raffinate collection device 1, an ectopic mineralization reaction device 2, a first pH value conditioning device 3, a first filtering device 5, a second pH value conditioning device 6, a second filtering device 8, and a pure brine storage device 9, which are sequentially connected through a pipeline, wherein a first turbid solution outlet 35 is arranged at the bottom of the first pH value conditioning device 3, the first turbid solution outlet 35 is communicated with an inlet of a first precipitate shunting collection device 4, a second turbid solution outlet is arranged at the bottom of the second pH value conditioning device 6, the second turbid solution outlet is communicated with an inlet of a second precipitate shunting collection device 7, and a power device is configured between the working units.
Preferably, as shown in fig. 2, there is at least one ectopic mineralization reaction device 2, and the ectopic mineralization reaction device 2 comprises a temperature measuring device 21, a steam heating device 22, a stirring shaft 23, a dyeing raffinate inlet 24, and an ectopic mineralization raffinate outlet 25; wherein temperature measuring device 21 sets up and is used for monitoring ectopic mineralization reaction system temperature on the inner wall of dystopy mineralization reaction unit 2, steam heating device 22 sets up and is convenient for heat dystopy mineralization system in dystopy mineralization reaction unit 2 bottom, the link of (mixing) shaft 23 rotates with dystopy mineralization reaction unit 2's top to be connected, the stirring portion of (mixing) shaft 23 is apart from reaction unit bottom 30-50cm, dyeing raffinate import 24 sets up the top at dystopy mineralization reaction unit 2, export intercommunication through pipeline and dyeing raffinate collection device 1, dystopy mineralization raffinate export 25 sets up the bottom at dystopy mineralization reaction unit 2, import intercommunication through pipeline and first pH value conditioning device 3.
As shown in fig. 3, the first pH value conditioning device 3 comprises a liquid internal circulation power device 31, an aeration device 32, an ex-situ mineralized raffinate inlet 33, an aeration device air outlet 34, a first turbid liquid outlet 35 and a first supernatant outlet 36, wherein the ex-situ mineralized raffinate inlet 33 is arranged at the top of the first pH value conditioning device 3 and is communicated with the ex-situ mineralized raffinate outlet 25 through a pipeline; the first pH value conditioning device 3 is provided with an opening at the position of 80cm from the bottom at the side edge, a liquid internal circulation power device 31 is arranged at the opening, the internal circulation power device 31 comprises a pipeline for communicating the bottom and the upper opening of the first pH value conditioning device 3 and a power pump arranged on the pipeline, so that the liquid circulation during the pH value conditioning is facilitated, the internal circulation of the liquid from bottom to top is realized, and the pH value of the liquid in the system is uniform; the aeration device 32 is arranged at the bottom of the first pH value conditioning device 3 and is used for accelerating the liquid circulation in the first pH value conditioning device and accelerating the process of liquid pH value homogenization in the system by the synergistic effect of the aeration device 32 and the liquid internal circulation device 31, and an aeration device air outlet 34 is arranged on the aeration device 32; after the pH value of the liquid is uniform and stable, the power device 31 and the aeration device 32 for internal circulation of the liquid are closed for sedimentation.
The first lower turbid liquid outlet 35 is arranged at the bottom of the first pH value conditioning device 3, the first lower turbid liquid outlet 35 is connected with an inlet of the first precipitate shunting and collecting device 4 through a pipeline and is used for shunting the first supernatant liquid and the first lower turbid liquid and collecting the first lower turbid liquid mainly containing cellulose short fibers and residual mineralization auxiliaries;
the first supernatant outlet 36 is arranged on the side wall of the first pH value conditioning device 3 and is communicated with the inlet of the first filtering device 5 through a pipeline; the first supernatant in the first pH conditioning device 3 is input into a first filtering device 5 for filtering through a power pump connected with a first supernatant outlet 36, the filtered first supernatant enters a second pH conditioning device 6, a second turbid liquid outlet is arranged at the bottom of the second pH conditioning device 6, and the second turbid liquid outlet is communicated with an inlet of a second precipitate shunting and collecting device 7 through a pipeline.
Further, the second pH value conditioning device 6 has the same structure as the first pH value conditioning device 3, the second pH value conditioning device 6 adjusts the pH value of the filtered first supernatant to be nearly neutral, and after sedimentation, a second supernatant and a second turbid liquid are obtained, the second supernatant is input into the second filtering device 8 through a power pump connected with a second supernatant outlet and is filtered to obtain purified brine, and the purified brine is introduced into the purified brine storage device for storage.
Preferably, the first filtering device 5 and the second filtering device 8 are both bag filters, and the filtering size of the first filtering device 5 is 5-10 μm; the filtering size of the second filtering device 8 is 1-5 μm; the first filtering device 5 is used for rough filtering, the second filtering device 8 is used for fine filtering, and double-layer filtering is carried out on the cellulose short fibers and the residual mineralizing auxiliary agent in the saline water.
Preferably, the first sediment diversion collecting device 4 and the second sediment diversion collecting device 7 have the same structure and respectively comprise a sedimentation tank and a collection tank, the sedimentation tank and the collection tank are communicated through a pipeline, a control valve is arranged on the pipeline, the first turbid liquid and the second turbid liquid are settled again in the sedimentation tank, the control valve is opened after the settlement is completed, and the sediment is discharged into the collection tank.
Preferably, the power device is a power pump.
The purified water obtained after the treatment of the system meets the requirements of reuse dyeing, and specifically refers to the requirements of application and water quality control of reuse water in the textile dyeing and finishing industry reuse water quality (FZ/T01107-2011). Before recycling, the salt concentration in the brine needs to be calibrated, and the adopted test method for the inorganic salt concentration is any conventional test method such as a density method, conductivity instrument determination and drying and weighing method for calibrating the brine concentration.
It should be noted that: the power device and the corresponding connecting pipeline related to the dyeing residual liquid collecting device 1 need to meet the material requirements of salt resistance, alkali resistance and high temperature;
the stirring shaft 23, the steam heating device 22, the temperature measuring device 21 and corresponding connecting pipelines in the ectopic mineralization reaction device 2 need to meet the requirements of salt resistance, acid, alkali, high temperature, oxidation and the like, and comprise materials which meet the requirements of the conditions, such as stainless steel, glass fiber reinforced plastics and the like;
the first pH value conditioning device 3, the second pH value conditioning device 6, the liquid internal circulation power device 31, the aeration device 32 and corresponding connecting pipelines in the first pH value conditioning device and the second pH value conditioning device all need to meet the requirements of salt resistance, acid resistance, alkali resistance, high temperature, oxidation and the like, and the first pH value conditioning device and the second pH value conditioning device comprise materials which meet the requirements of the conditions, such as stainless steel, glass fiber reinforced plastics and the like;
the first sediment diversion and collection device 4 and the second sediment diversion and collection device 7 adopt the requirements of salt and alkali resistance of materials;
the first filtering device 5, the second filtering device 8 and corresponding connecting pipelines need to meet the requirements of salt resistance, alkali resistance and the like, and comprise materials such as stainless steel, glass fiber reinforced plastics and the like which meet the requirements of the conditions;
the pure brine storage device 9 and the corresponding connecting pipeline need to meet the requirement of salt-resistant materials.
The invention provides a use method of a salt recycling system, which comprises the following specific embodiments:
step 1, collecting and storing a cellulose fiber reactive dye dyeing residual liquid through a dyeing residual liquid collecting device 1, pumping the residual liquid into an ectopic mineralization reaction device 2 through a power pump, starting a rotating shaft 23 connected with a motor, starting a steam heating device 22 to heat an ectopic mineralization reaction system, and carrying out ectopic mineralization reaction described in patent ZL201510106886.2 to obtain an ectopic mineralization residual liquid; the temperature of the ex-situ mineralization reaction system is determined by the temperature monitoring device 21, and the rotation shaft 23 is kept running until the reaction is finished.
Step 2, enabling the ectopic mineralization residual liquid to flow out of an outlet of the ectopic mineralization reaction device 2, conveying the ectopic mineralization residual liquid to a first pH value conditioning device 3 through a power pump, adjusting the pH value of the ectopic mineralization residual liquid to be 7.0-14.0, standing and settling, and conveying the obtained first supernatant (the volume ratio is more than or equal to 95%) to a first filtering device 5; the obtained first turbid liquid (the volume ratio is less than or equal to 5%) enters a first precipitate shunting and collecting device 4;
specifically, the suspended sediment collected by the first sediment shunt collection device 4 is subjected to harmless treatment according to the printing and dyeing sludge;
specifically, the first supernatant is filtered by the first filtering device 5 and then is conveyed to the second pH value conditioning device 6.
Step 3, adjusting the pH value of the filtered first supernatant in the second pH value conditioning device 6 to be nearly neutral, standing and settling to obtain a second supernatant (the volume ratio is more than or equal to 98%) and a second lower turbid liquid (the volume ratio is less than or equal to 2%), allowing the second lower turbid liquid to enter a second precipitate shunting and collecting device 7, and allowing the second supernatant to enter a second filtering device 8 for filtering treatment;
specifically, the suspended sediment collected by the second sediment diversion and collection device 7 is subjected to harmless treatment according to the printing and dyeing sludge;
specifically, the supernatant is filtered by the second filtering device 8 and then is conveyed to the pure brine storage device 9, and the brine meets the requirement of recycling dyeing.
And adding inorganic salt or soft water into the recycled saline water in the dye vat according to the inorganic salt concentration required by the dyeing order to adjust the inorganic salt concentration.
Preferably, the treated pure saline water is used as a dyeing medium to be added into dyeing equipment, and reactive dye is carried out on cellulose fibers to be dyed; by the recycling system for the salt in the dyeing residual liquid of the reactive dye by the ectopic mineralization technology, the saline water can be recycled in the subsequent dyeing processing of the reactive dye, so that the recycling of the inorganic salt in the dyeing residual liquid of the reactive dye is realized.
Example 1
The collected cellulose fiber reactive dyeConveying the dyeing raffinate into an ex-situ mineralization reaction device 2 through a power device, keeping the room temperature, starting a stirring shaft 23 to ensure circulation of a treatment bath, adding 8g/L dilute sulfuric acid (30%) into the treatment bath, adjusting the pH value of the treatment bath to be 1.0, then adding 0.05g/L mineralized coupling agent XBC into the treatment bath, adding 3g/L mineralized coupling agent XYC into the treatment bath after the treatment bath is circulated uniformly, keeping the reaction bath circulation for 8 hours under the condition to obtain an ex-situ mineralization raffinate bath, wherein the ex-situ mineralization raffinate has extremely low chromatic value and low pollutant content, conveying the ex-situ mineralization raffinate into a first pH value conditioning device 3 through the power device, and adding 3g/L NaCO into the treatment bath3Adjusting the pH value to about 8, standing, collecting the lower turbid liquid by a first precipitate shunt collection device 4 (performing innocent treatment according to printing and dyeing sludge), filtering the supernatant by a first filtering device 5, conveying the supernatant to a second pH value conditioning device 6, adding 0.5g/L formic acid into the filtrate, adjusting the pH value of the treatment bath to be nearly neutral, collecting the residual small amount of suspended impurities in the lower layer by a second precipitate shunt collection device 7 (performing innocent treatment according to printing and dyeing sludge), filtering the supernatant by a second filtering device 8, and conveying the supernatant to a clean saline water storage device 9 for later use. And calibrating the content of inorganic salt in the purified brine, conveying the purified brine into a dye vat of a dyeing workshop, and supplementing soft water or inorganic salt by calculation to meet the requirements of recycling and dyeing.
Example 2
Conveying collected cellulose fiber active dye dyeing raffinate into an ectopic mineralization reaction device 2 through a power device, heating the dyeing raffinate to 60 ℃ through a steam heating device 22, starting a stirring shaft 23, ensuring the circulation of a treatment bath, adding 3g/L nitric acid into the treatment bath, adjusting the pH value of the treatment bath to 3.5, then adding 0.2g/L mineralized coupling agent XBC into the treatment bath, adding 4g/L mineralized coupling agent XYC after the circulation of the treatment bath is uniform, keeping the reaction bath circulation for 1.5h under the condition, obtaining the ectopic mineralization raffinate which has extremely low chroma value and low pollutant content, conveying the ectopic mineralization raffinate into a first pH value conditioning device 3 through the power device, adding 1.0g/L NaOH into the treatment bath, adjusting the pH value to be about 10, standing, collecting lower turbid liquid by a first precipitate shunt collection device 4 (performing harmless treatment by referring to printing and dyeing sludge) The supernatant is filtered by a first filtering device 5 and is conveyed to a second pH value conditioning device 6, 1g/L dilute sulfuric acid (30%) is added into the filtrate, the pH value of the treatment bath is adjusted to be nearly neutral, a small amount of suspended impurities remained in the lower layer are collected by a second precipitate shunt collection device 7 in a shunt mode (harmless treatment is carried out according to printing and dyeing sludge), and the supernatant is filtered by a second filtering device 8 and is conveyed to a pure brine storage device 9 for standby. And calibrating the content of inorganic salt in the purified brine, conveying the purified brine into a dye vat of a dyeing workshop, and supplementing soft water or inorganic salt by calculation to meet the requirements of recycling and dyeing.
Example 3
Conveying the collected cellulose fiber reactive dye dyeing residual liquid into an ex-situ mineralization reaction device 2 through a power device, heating the dyeing residual liquid to 70 ℃ through a steam heating device 22, starting a stirring shaft 23 to ensure treatment bath circulation, adding 2.5g/L hydrochloric acid into the treatment bath, adjusting the pH value of the treatment bath to 4.5, then adding 1.5g/L mineralized coupling agent XBC into the treatment bath, starting the stirring shaft 23 to ensure treatment bath circulation to be uniform, adding 5g/L mineralized coupling agent XYC, keeping the reaction bath circulation for 2h under the condition, obtaining the ex-situ mineralization residual bath, wherein the ex-situ mineralization residual liquid has extremely low chroma value and low pollutant content, conveying the ex-situ mineralization residual liquid into a first pH value conditioning device 3 through the power device, adding 1.3g/L KOH into the treatment bath, adjusting the pH value to about 11 and standing, the lower turbid liquid is collected in a shunting way through a first precipitate shunting and collecting device 4 (refer to printing and dyeing sludge for innocent treatment), the supernatant is filtered through a first filtering device 5 and is conveyed to a second pH value conditioning device 6, 2g/L citric acid is added into the filtrate, the pH value of the treatment bath is adjusted to be nearly neutral, a small amount of residual suspended impurities in the lower layer are collected in a shunting way through a second precipitate shunting and collecting device 7 (refer to printing and dyeing sludge for innocent treatment), and the supernatant is filtered through a second filtering device 8 and is conveyed to a pure brine storage device 9 for standby. And calibrating the content of inorganic salt in the purified brine, conveying the purified brine into a dye vat of a dyeing workshop, and supplementing soft water or inorganic salt by calculation to meet the requirements of recycling and dyeing.
Example 4
Conveying collected cellulose fiber reactive dye dyeing residual liquid into an ex-situ mineralization reaction device 2 through a power device, heating the dyeing residual liquid to 80 ℃ through a steam heating device 22, starting a stirring shaft 23, ensuring circulation of a treatment bath, adding 8g/L dilute sulfuric acid into the treatment bath, adjusting the pH value of the treatment bath to 3.0, then adding 0.8g/L mineralized coupling agent XBC into the treatment bath, adding 6g/L mineralized coupling agent XYC after the treatment bath is circulated uniformly, keeping the reaction bath circulation for 1.0h under the condition, obtaining the ex-situ mineralization residual liquid which has extremely low chroma value and low pollutant content, conveying the ex-situ mineralization into a first pH value conditioning device 3 through the power device, adding 1.2g/L NaOH into the treatment bath, adjusting the pH value to be about 11, standing, and collecting lower turbid liquid in a shunting way through a first precipitate collecting device 4 (carrying out innocent treatment on printing and dyeing sludge reference) ) The supernatant is filtered by a first filtering device 5 and is conveyed to a second pH value conditioning device 6, 2g/L dilute sulfuric acid (30%) is added into the filtrate, the pH value of the treatment bath is adjusted to be nearly neutral, a small amount of suspended impurities remained in the lower layer are collected by a second precipitate shunt collection device 7 in a shunt mode (harmless treatment is carried out according to printing and dyeing sludge), and the supernatant is filtered by a second filtering device 8 and is conveyed to a pure brine storage device 9 for standby. And calibrating the content of inorganic salt in the purified brine, conveying the purified brine into a dye vat of a dyeing workshop, and supplementing soft water or inorganic salt by calculation to meet the requirements of recycling and dyeing.
Example 5
Conveying the collected cellulose fiber reactive dye dyeing residual liquid into an ex-situ mineralization reaction device 2 through a power device, heating the dyeing residual liquid to 100 ℃ through a steam heating device 22, starting a stirring shaft 23, ensuring the circulation of a treatment bath, adding 4g/L formic acid into the treatment bath, adjusting the pH value of the treatment bath to 6.0, then adding 2.0g/L mineralized coupling agent XBC into the treatment bath, adding 8g/L mineralized coupling agent XYC after the circulation of the treatment bath is uniform, keeping the reaction bath circulation for 4 hours under the condition, thus obtaining the ex-situ mineralization residual bath which has extremely low chroma value and low pollutant content, conveying the ex-situ mineralization residual liquid into a first pH value conditioning device 3 through the power device, adding 2.0g/L mineralized coupling agent XYC into the treatment bath, adjusting the pH value to be about 14, standing, collecting the lower turbidity liquid by a first sediment shunt collection device 4 (performing harmless treatment by referring to sludge printing and dyeing) And filtering the supernatant through a first filtering device 5 and conveying the supernatant to a second pH value conditioning device 6, adding 4g/L of acetic acid into the filtrate, adjusting the pH value of the treatment bath to be nearly neutral, shunting and collecting a small amount of suspended impurities remained in the lower layer through a second precipitate shunting and collecting device 7 (performing harmless treatment by referring to printing and dyeing sludge), and filtering the supernatant through a second filtering device 8 and conveying the supernatant to a pure brine storage device 9 for later use. And calibrating the content of inorganic salt in the purified brine, conveying the purified brine into a dye vat of a dyeing workshop, and supplementing soft water or inorganic salt by calculation to meet the requirements of recycling and dyeing.

Claims (10)

1. A system for recycling dyeing raffinate salt of reactive dye based on a fiber ectopic mineralization technology is characterized by comprising a dyeing raffinate collecting device (1), an ectopic mineralization reaction device (2), a first pH value conditioning device (3), a first filtering device (5), a second pH value conditioning device (6), a second filtering device (8) and a pure brine storage device (9) which are sequentially connected through pipelines, a first lower turbid liquid outlet (35) is arranged at the bottom of the first pH value conditioning device (3), the first lower turbid liquid outlet (35) is communicated with the inlet of the first sediment shunting and collecting device (4), and a second lower turbid liquid outlet is arranged at the bottom of the second pH value conditioning device (6), the second lower turbid liquid outlet is communicated with an inlet of a second precipitate shunting and collecting device (7), and power devices are arranged between the devices.
2. The system for recycling dyeing raffinate salt of reactive dye based on fiber ectopic mineralization technology as claimed in claim 1, wherein the ectopic mineralization reaction device (2) comprises a temperature measuring device (21), a steam heating device (22), a stirring shaft (23), a dyeing raffinate inlet (24) and an ectopic mineralization raffinate outlet (25); wherein the temperature measuring device (21) is arranged on the inner wall of the ectopic mineralization reaction device (2) and is used for monitoring the temperature of the ectopic mineralization reaction system; the steam heating device (22) is arranged at the bottom of the ectopic mineralization reaction device (2) and is used for heating the ectopic mineralization system; the connecting end of the stirring shaft (23) is rotatably connected with the top of the ectopic mineralization reaction device (2); the dyeing residual liquid inlet (24) is arranged at the top of the ectopic mineralization reaction device (2) and is communicated with an outlet of the dyeing residual liquid collection device (1) through a pipeline; the ex-situ mineralization residual liquid outlet (25) is arranged at the bottom of the ex-situ mineralization reaction device (2) and is communicated with an inlet of the first pH value conditioning device (3) through a pipeline.
3. The system for recycling dyeing raffinate salt of reactive dye based on fiber ectopic mineralization technology as claimed in any one of claims 1 or 2, wherein a plurality of ectopic mineralization reaction devices (2) are provided.
4. The system for recycling dyeing raffinate salt of reactive dye based on the fiber ectopic mineralization technology as claimed in claim 1, wherein the first pH value conditioning device (3) comprises a liquid internal circulation power device (31), an aeration device (32), an ectopic mineralization raffinate inlet (33), a first turbid liquid outlet (35) and a first supernatant liquid outlet (36), wherein an opening is formed in the bottom of the side surface of the first pH value conditioning device (3), and the liquid internal circulation power device (31) is arranged at the opening for liquid circulation during pH value regulation; the aeration device (32) is arranged at the bottom of the first pH value conditioning device (3) and is used for accelerating the liquid circulation in the first pH value conditioning device; the ex-situ mineralized raffinate inlet (33) is arranged at the top of the first pH value conditioning device (3) and is communicated with the ex-situ mineralized raffinate outlet (25); the first lower turbid liquid outlet (35) is arranged at the bottom of the first pH value conditioning device (3), and the first supernatant liquid outlet (36) is arranged on the side wall of the upper part of the first pH value conditioning device (3) and is communicated with the inlet of the first filtering device (5) to filter the first supernatant liquid.
5. The system for recycling dyeing raffinate salt of reactive dye based on the ectopic mineralization technology of fiber as claimed in claim 4, wherein the power device (31) for internal circulation of liquid comprises a pipeline communicating the side part and the upper opening of the first pH value conditioning device (3) and a power pump arranged on the pipeline and is used for realizing internal circulation of liquid in the first pH value conditioning device (3) from bottom to top.
6. The system for recycling dyeing raffinate salt of reactive dye based on ectopic mineralization technology of claim 1, wherein the first pH value conditioning device (3) is used for adjusting the pH value of the ectopic mineralization raffinate to be alkaline; the second pH value conditioning device (6) is used for adjusting the pH value of the filtered first supernatant to be neutral.
7. The system for recycling dyeing raffinate salt of reactive dye based on the ectopic mineralization technology of fiber as claimed in claim 1, wherein the first filter device (5) and the second filter device (8) are both bag filters, and the filtering size of the first filter device (5) is 5 μm-10 μm; the second filter device (8) has a filter size of 1 μm to 5 μm.
8. The system for recycling dyeing residue and salt of reactive dyes based on the ectopic mineralization of fibers as claimed in claim 1, wherein said first and second collecting devices (4, 7) comprise a settling device and a collecting pool, said settling device and collecting pool are connected by a pipeline, said pipeline is equipped with a control valve, said settling device is used for settling the first and second sediments, and said collecting pool is used for collecting the settled sediments.
9. The system for recycling dyeing raffinate salt of reactive dye based on the ectopic mineralization technology of any one of claims 1 and 8, wherein the first and second partial sediment collecting devices (4, 7) are made of salt-resistant and alkali-resistant materials.
10. The system for recycling dyeing raffinate salt of reactive dye based on the ectopic mineralization technology of fiber as claimed in claim 1, wherein the dyeing raffinate collecting device (1) and the corresponding connecting pipeline meet the material requirements of salt tolerance, alkali tolerance and high temperature tolerance; the ectopic mineralization reaction device (2) and the corresponding connecting pipeline meet the requirements of materials for salt resistance, acid resistance, alkali resistance, high temperature resistance and oxidation resistance; the first pH value conditioning device (3), the second pH value conditioning device (6) and corresponding connecting pipelines meet the requirements of materials for salt resistance, acid resistance, alkali resistance, high temperature resistance and oxidation resistance; the first filtering device (5), the second filtering device (8) and corresponding connecting pipelines meet the requirements of salt and alkali resistance; the pure brine storage device (9) and the corresponding connecting pipeline meet the requirement of salt-resistant materials.
CN202110921334.2A 2021-08-11 2021-08-11 System for recycling salt in dyeing raffinate of reactive dye based on fiber ectopic mineralization technology Pending CN113562919A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104695253A (en) * 2015-03-11 2015-06-10 西安工程大学 Cellulosic fiber in-situ mineralization deep water-saving and emission reduction dyeing aftertreatment method and additive
CN207738523U (en) * 2017-11-29 2018-08-17 江苏中轩建设有限公司 A kind of water pollution controlling device
CN108755181A (en) * 2018-04-04 2018-11-06 西安工程大学 Cellulose fibre reactive dye low-salt original position mineralising colouring method
CN109778561A (en) * 2019-01-24 2019-05-21 西安工程大学 Based on dystopy mineralising technology cellulose fibre reactive dyeing salt reuse method
CN210559953U (en) * 2019-09-09 2020-05-19 海盐鸳鸯丝绸印染股份有限公司 Printing and dyeing process waste water purification and recovery system
WO2021077200A1 (en) * 2019-10-22 2021-04-29 Mahe Alexandre Apparatus and process for filtering and mineralizing a fluid

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104695253A (en) * 2015-03-11 2015-06-10 西安工程大学 Cellulosic fiber in-situ mineralization deep water-saving and emission reduction dyeing aftertreatment method and additive
CN207738523U (en) * 2017-11-29 2018-08-17 江苏中轩建设有限公司 A kind of water pollution controlling device
CN108755181A (en) * 2018-04-04 2018-11-06 西安工程大学 Cellulose fibre reactive dye low-salt original position mineralising colouring method
CN109778561A (en) * 2019-01-24 2019-05-21 西安工程大学 Based on dystopy mineralising technology cellulose fibre reactive dyeing salt reuse method
CN210559953U (en) * 2019-09-09 2020-05-19 海盐鸳鸯丝绸印染股份有限公司 Printing and dyeing process waste water purification and recovery system
WO2021077200A1 (en) * 2019-10-22 2021-04-29 Mahe Alexandre Apparatus and process for filtering and mineralizing a fluid

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