CN109485120A - A kind of dyeing waste water efficient process agent and preparation method thereof - Google Patents
A kind of dyeing waste water efficient process agent and preparation method thereof Download PDFInfo
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- CN109485120A CN109485120A CN201811247897.2A CN201811247897A CN109485120A CN 109485120 A CN109485120 A CN 109485120A CN 201811247897 A CN201811247897 A CN 201811247897A CN 109485120 A CN109485120 A CN 109485120A
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- 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
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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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
- 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
Abstract
The present invention is prepared for a kind of dyeing waste water efficient process agent, is made of each ingredient of following parts by weight: 32-44 parts of composite modified porous microsphere flocculant, 45-52 parts of middle polar resin adsorbent, permutite load 18-26 parts of Nanoscale Iron magnesium bimetallic, atlapulgite 14-22 parts rare earth doped.The preparation method of dyeing waste water efficient process agent of the present invention include the following steps: to take 32-44 parts of composite modified porous microsphere flocculant, 45-52 parts of middle polar resin adsorbent, permutite load 18-26 parts of Nanoscale Iron magnesium bimetallic, it is rare earth doped atlapulgite 14-22 parts after mixing, ball milling 2h, it is dried in 55 DEG C of vacuum ovens again, obtains dyeing waste water efficient process agent.Cost is relatively low for the dyeing waste water efficient process agent that the present invention is prepared, splendid to the adsorption and sedimentation and coagulation effect of dyeing waste water.
Description
Technical field
The present invention relates to chemical industry and environmental technology fields, more particularly to a kind of dyeing waste water efficient process agent and its preparation
Method.
Background technique
In recent years, with the fast development of China's printing and dyeing industry, a large amount of waste water that dyeing generates become environment guarantor
A big threat in shield.In textile dyeing, about the dyestuff of 1O%~20% forms printing and dyeing with discharge of wastewater and gives up
Water, dyeing and finishing industry is one of biggish department of pollutant discharge amount, and mainly based on contaminated wastewater, the waste water Zhan that it is discharged is total
The 35% of discharged volume of industrial waste water, the complicated component of dyeing waste water, concentration are high, coloration is high, variation water quality changes greatly, very difficulty
Reason.Especially exploitation has used some novel durable dyestuffs in recent years, the difficulty of wastewater treatment has been further exacerbated by, to printing and dyeing
The purified treatment of waste water proposes new challenge.Therefore, it is imperative to find more economical efficient treatment method of printing and dying wastewater,
On the one hand the problem of environment can be protected, the ecological balance is maintained, on the other hand can alleviate China's water resources shortage, have great
Meaning.
Summary of the invention
Technical problems to be solved:
The object of the present invention is to provide a kind of dyeing waste water efficient process agent and preparation method thereof, preferably handle coloration
Greatly, concentration is high, fluctuates big dyeing waste water.
Technical solution:
The present invention provides a kind of dyeing waste water efficient process agent, are made of each ingredient of following parts by weight:
32-44 parts of composite modified porous microsphere flocculant, 45-52 parts of middle polar resin adsorbent, permutite's load are received
It is 18-26 parts of rice iron magnesium bimetallic, atlapulgite 14-22 parts rare earth doped.
Preferably, the preparation method of the modified porous microballoon includes the following steps:
(1) oily phase is added in the reactor, adjustment revolving speed stirs 10min, is warming up to 50 DEG C, and emulsifier, stirring is added
40min is cooled to room temperature and Herba Lycopodii polysaccharide solution is added, and stirs 50min at room temperature and obtains homogeneous latex emulsion;
(2) ethyl acetate, cyclohexanol, ethylenediamine and glutaraldehyde are added into step (1) lotion, be stirred to react 7h obtain it is more
Hole microballoon;
(3) it takes porous microsphere to be added to 100mL to go from water, addition glacial acetic acid stirs evenly, and adds aluminium polychloride and sulphur
Sour magnesium, after stirring and adsorbing 3h, clean dry obtains composite modified porous microsphere flocculant.
It is further preferred that oil described in step (1) is mutually methyl-silicone oil and glycerol according to volume ratio (2-6): (1-5) is mixed
It closes.
It is further preferred that the volume ratio of oil phase, emulsifier and Herba Lycopodii polysaccharide solution described in step (1) is
(2.7-5.6):0.04:1。
It is further preferred that ethyl acetate described in step (2), cyclohexanol, ethylenediamine and glutaraldehyde volume ratio be (6-
11):(9-13):(10-14):(12-16);Porous microsphere described in step (3), glacial acetic acid, aluminium polychloride and magnesium sulfate
Weight ratio is 2:(0.8-1.4): (1.5-1.9): (1.12-1.36).
Preferably, the preparation method of the middle polar resin adsorbent, includes the following steps:
(1) 200mL deionized water, 10g sodium chloride are added in three-necked flask, 5g hydroxyethyl cellulose is warming up to 60 DEG C,
300r/min is stirred to dissolution and is obtained mixed solution A;
(2) by 23g diethylaminoethyl methacrylate, 30g acrylic acid-2-ethyl-own ester, 26g butyl acrylate and
10g divinylbenzene, 0.7-1.4g azodiisobutyronitrile, 0.24-0.66g ethylene glycol dimethacrylate stir evenly, then
6-10g 14# white oil is added, stirs evenly to obtain mixed solution B;
(3) mixed solution B is added in mixed solution A, is stirred to react 5h, then heat to 60 DEG C of heat preservation 3h, it is cooling
To room temperature, it is dried in vacuo after cleaning up to middle polar resin adsorbent.
Preferably, the permutite loads the bimetallic preparation method of Nanoscale Iron magnesium, and including the following steps: will be artificial
1000 DEG C of calcining 2h of float stone, by 1.7-2.5g FeCl3·6H2O and 1.4-2.2g Mg (NO3)2·6H2O is dissolved in 200mL
It in 10wt% ethanol solution, is subsequently placed in flask, adds the calcined permutite of 20g, stirred for 60 DEG C in nitrogen atmosphere
Reaction 30h is mixed, taking-up cleans permutite obtained by drying and loads Nanoscale Iron magnesium bimetallic.
Preferably, the preparation method of the rare earth doped atlapulgite, includes the following steps:
24g atlapulgite and 100mL deionized water are configured to mixed liquor, 900r/min is stirred continuously, and is then added
1.6-2.2g lanthana stirs 2h, and after filtering drying, 700 DEG C of calcining 2h are pulverized after cooling up to rare earth doped work
Property carclazyte.
Preferably, the preparation method of the dyeing waste water efficient process agent, includes the following steps: to take composite modified porous
32-44 parts of microballoon flocculant, 45-52 parts of middle polar resin adsorbent, permutite load 18-26 parts of Nanoscale Iron magnesium bimetallic,
Rare earth doped atlapulgite 14-22 parts after mixing, dries, is printed and dyed in ball milling 2h, then 55 DEG C of vacuum ovens
Waste water high-efficiency inorganic agent.
The utility model has the advantages that
(1) present invention preparation has the polysaccharide porous microsphere of loose webs structure, and with aluminium polychloride and magnesium sulfate pair
It is modified, and being prepared has the composite modified porous microsphere flocculant of excellent absorption property.
(2) there is porous structure in middle polar resin adsorbent prepared by the present invention, and contain ester group, surface has concurrently thin
Water and hydrophilic segment can adsorb polarity and nonpolar substance in dyeing waste water, have good suction-operated.
(3) permutite prepared by the present invention loads Nanoscale Iron magnesium bimetallic, using permutite as carrier, load
The duct of magnesium, iron, permutite has local stabilization to metallic, can reduce agglomerate, expands active constituent and sewage
Contact area, greatly improve reactivity worth, so as to restore well removal dyeing waste water in pollutant.
(4) present invention use rare earth element La doped atlapulgite, then calcined, improve atlapulgite intensity and
Stability improves its absorption property.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit this in any way
Invention.
Embodiment 1
44 parts of composite modified porous microsphere flocculant, 45 parts of middle polar resin adsorbent, permutite is taken to load Nanoscale Iron
26 parts of magnesium bimetallic, 14 parts of rare earth doped atlapulgite after mixing, dry in ball milling 2h, then 55 DEG C of vacuum ovens
It is dry, obtain dyeing waste water efficient process agent.
Modified porous microballoon is prepared by following preparation methods:
(1) 560mL oil phase is added in the reactor, adjustment revolving speed stirs 10min, is warming up to 50 DEG C, 4g sorbester p18 is added,
40min is stirred, is cooled to room temperature and 100mL 1.2g/mL Herba Lycopodii polysaccharide solution is added, 50min is stirred at room temperature and obtains uniformly
Lotion, the oil are mutually that methyl-silicone oil and glycerol are mixed according to volume ratio 4:3;
(2) 6mL ethyl acetate, 13mL cyclohexanol, 10mL ethylenediamine and 16mL glutaraldehyde are added into step (1) lotion to stir
It mixes reaction 7h and obtains porous microsphere;
(3) it takes 20g porous microsphere to be added to 100mL to go from water, addition 8g glacial acetic acid stirs evenly, and adds 19g polymerization chlorine
Change aluminium and 11.2g magnesium sulfate, after stirring and adsorbing 3h, dry 14h, is obtained composite modified porous at 5 times wash with distilled water, 90 DEG C
Microballoon flocculant.
The preparation method of middle polar resin adsorbent, includes the following steps:
(1) 200mL deionized water, 10g sodium chloride are added in three-necked flask, 5g hydroxyethyl cellulose is warming up to 60 DEG C,
300r/min is stirred to dissolution and is obtained mixed solution A;
(2) by 23g diethylaminoethyl methacrylate, 30g acrylic acid-2-ethyl-own ester, 26g butyl acrylate and
10g divinylbenzene, 1.4g azodiisobutyronitrile, 0.24g ethylene glycol dimethacrylate stir evenly, and add 10g
14# white oil stirs evenly to obtain mixed solution B;
(3) mixed solution B is added in mixed solution A, is stirred to react 5h, then heat to 60 DEG C of heat preservation 3h, it is cooling
It to room temperature, is cleaned 3 times with acetone, deionized water is cleaned 3 times, and 80 DEG C of vacuum drying 10h are up to middle polar resin adsorbent.
It is bimetallic the preparation method comprises the following steps: by 1000 DEG C of calcining 2h of permutite, by 1.7g that permutite loads Nanoscale Iron magnesium
FeCl3·6H2O and 2.2g Mg (NO3)2·6H2O is dissolved in 200mL 10wt% ethanol solution, is subsequently placed in flask, then plus
Enter the calcined permutite of 20g, be stirred to react 30h for 60 DEG C in nitrogen atmosphere, take out and use washes of absolute alcohol 3 times, go from
Sub- water cleans 3 times, and 80 DEG C of vacuum drying 12h load Nanoscale Iron magnesium bimetallic up to permutite.
Rare earth doped atlapulgite the preparation method comprises the following steps: 24g atlapulgite and 100mL deionized water are configured to mix
Liquid is closed, 900r/min is stirred continuously, and 1.6g lanthana is then added and stirs 2h, filters, by 80 DEG C of solid content dry 5h, then
700 DEG C of calcining 2h after being cooled to room temperature, pulverize up to rare earth doped atlapulgite.
Embodiment 2
32 parts of composite modified porous microsphere flocculant, 52 parts of middle polar resin adsorbent, permutite is taken to load Nanoscale Iron
18 parts of magnesium bimetallic, 22 parts of rare earth doped atlapulgite after mixing, dry in ball milling 2h, then 55 DEG C of vacuum ovens
It is dry, obtain dyeing waste water efficient process agent.
Modified porous microballoon is prepared by following preparation methods:
(1) 270mL oil phase is added in the reactor, adjustment revolving speed stirs 10min, is warming up to 50 DEG C, 4g sorbester p18 is added,
40min is stirred, is cooled to room temperature and 100mL 1.2g/mL Herba Lycopodii polysaccharide solution is added, 50min is stirred at room temperature and obtains uniformly
Lotion, the oil are mutually that methyl-silicone oil and glycerol are mixed according to volume ratio 4:3;
(2) 11mL ethyl acetate, 9mL cyclohexanol, 14mL ethylenediamine and 12mL glutaraldehyde are added into step (1) lotion to stir
It mixes reaction 7h and obtains porous microsphere;
(3) it takes 20g porous microsphere to be added to 100mL to go from water, addition 14g glacial acetic acid stirs evenly, and adds 15g polymerization chlorine
Change aluminium and 13.6g magnesium sulfate, after stirring and adsorbing 3h, dry 14h, is obtained composite modified porous at 5 times wash with distilled water, 90 DEG C
Microballoon flocculant.
The preparation method of middle polar resin adsorbent, includes the following steps:
(1) 200mL deionized water, 10g sodium chloride are added in three-necked flask, 5g hydroxyethyl cellulose is warming up to 60 DEG C,
300r/min is stirred to dissolution and is obtained mixed solution A;
(2) by 23g diethylaminoethyl methacrylate, 30g acrylic acid-2-ethyl-own ester, 26g butyl acrylate and
10g divinylbenzene, 0.7g azodiisobutyronitrile, 0.66g ethylene glycol dimethacrylate stir evenly, and add 6g 14#
White oil stirs evenly to obtain mixed solution B;
(3) mixed solution B is added in mixed solution A, is stirred to react 5h, then heat to 60 DEG C of heat preservation 3h, it is cooling
It to room temperature, is cleaned 3 times with acetone, deionized water is cleaned 3 times, and 80 DEG C of vacuum drying 10h are up to middle polar resin adsorbent.
It is bimetallic the preparation method comprises the following steps: by 1000 DEG C of calcining 2h of permutite, by 2.5g that permutite loads Nanoscale Iron magnesium
FeCl3·6H2O and 1.4g Mg (NO3)2·6H2O is dissolved in 200mL 10wt% ethanol solution, is subsequently placed in flask, then plus
Enter the calcined permutite of 20g, be stirred to react 30h for 60 DEG C in nitrogen atmosphere, take out and use washes of absolute alcohol 3 times, go from
Sub- water cleans 3 times, and 80 DEG C of vacuum drying 12h load Nanoscale Iron magnesium bimetallic up to permutite.
Rare earth doped atlapulgite the preparation method comprises the following steps: 24g atlapulgite and 100mL deionized water are configured to mix
Liquid is closed, 900r/min is stirred continuously, and 2.2g lanthana is then added and stirs 2h, filters, by 80 DEG C of solid content dry 5h, then
700 DEG C of calcining 2h after being cooled to room temperature, pulverize up to rare earth doped atlapulgite.
Embodiment 3
40 parts of composite modified porous microsphere flocculant, 47 parts of middle polar resin adsorbent, permutite is taken to load Nanoscale Iron
24 parts of magnesium bimetallic, 17 parts of rare earth doped atlapulgite after mixing, dry in ball milling 2h, then 55 DEG C of vacuum ovens
It is dry, obtain dyeing waste water efficient process agent.
Modified porous microballoon is prepared by following preparation methods:
(1) 480mL oil phase is added in the reactor, adjustment revolving speed stirs 10min, is warming up to 50 DEG C, 4g sorbester p18 is added,
40min is stirred, is cooled to room temperature and 100mL 1.2g/mL Herba Lycopodii polysaccharide solution is added, 50min is stirred at room temperature and obtains uniformly
Lotion, the oil are mutually that methyl-silicone oil and glycerol are mixed according to volume ratio 4:3;
(2) 7mL ethyl acetate, 12mL cyclohexanol, 11mL ethylenediamine and 15.4mL glutaraldehyde are added into step (1) lotion
It is stirred to react 7h and obtains porous microsphere;
(3) it takes 20g porous microsphere to be added to 100mL to go from water, addition 10g glacial acetic acid stirs evenly, and adds 18g polymerization chlorine
Change aluminium and 12g magnesium sulfate, after stirring and adsorbing 3h, dry 14h, is obtained composite modified porous micro- at 5 times wash with distilled water, 90 DEG C
Ball flocculant.
The preparation method of middle polar resin adsorbent, includes the following steps:
(1) 200mL deionized water, 10g sodium chloride are added in three-necked flask, 5g hydroxyethyl cellulose is warming up to 60 DEG C,
300r/min is stirred to dissolution and is obtained mixed solution A;
(2) by 23g diethylaminoethyl methacrylate, 30g acrylic acid-2-ethyl-own ester, 26g butyl acrylate and
10g divinylbenzene, 1.2g azodiisobutyronitrile, 0.34g ethylene glycol dimethacrylate stir evenly, and add 9g 14#
White oil stirs evenly to obtain mixed solution B;
(3) mixed solution B is added in mixed solution A, is stirred to react 5h, then heat to 60 DEG C of heat preservation 3h, it is cooling
It to room temperature, is cleaned 3 times with acetone, deionized water is cleaned 3 times, and 80 DEG C of vacuum drying 10h are up to middle polar resin adsorbent.
It is bimetallic the preparation method comprises the following steps: by 1000 DEG C of calcining 2h of permutite, by 1.9g that permutite loads Nanoscale Iron magnesium
FeCl3·6H2O and 2g Mg (NO3)2·6H2O is dissolved in 200mL 10wt% ethanol solution, is subsequently placed in flask, is added
The calcined permutite of 20g is stirred to react 30h for 60 DEG C in nitrogen atmosphere, takes out and use washes of absolute alcohol 3 times, deionization
Water cleans 3 times, and 80 DEG C of vacuum drying 12h load Nanoscale Iron magnesium bimetallic up to permutite.
Rare earth doped atlapulgite the preparation method comprises the following steps: 24g atlapulgite and 100mL deionized water are configured to mix
Liquid is closed, 900r/min is stirred continuously, and 1.7g lanthana is then added and stirs 2h, filters, by 80 DEG C of solid content dry 5h, then
700 DEG C of calcining 2h after being cooled to room temperature, pulverize up to rare earth doped atlapulgite.
Embodiment 4
36 parts of composite modified porous microsphere flocculant, 50 parts of middle polar resin adsorbent, permutite is taken to load Nanoscale Iron
20 parts of magnesium bimetallic, 19 parts of rare earth doped atlapulgite after mixing, dry in ball milling 2h, then 55 DEG C of vacuum ovens
It is dry, obtain dyeing waste water efficient process agent.
Modified porous microballoon is prepared by following preparation methods:
(1) 350mL oil phase is added in the reactor, adjustment revolving speed stirs 10min, is warming up to 50 DEG C, 4g sorbester p18 is added,
40min is stirred, is cooled to room temperature and 100mL 1.2g/mL Herba Lycopodii polysaccharide solution is added, 50min is stirred at room temperature and obtains uniformly
Lotion, the oil are mutually that methyl-silicone oil and glycerol are mixed according to volume ratio 4:3;
(2) 10mL ethyl acetate, 10mL cyclohexanol, 13mL ethylenediamine and 12.6mL penta 2 are added into step (1) lotion
Aldehyde is stirred to react 7h and obtains porous microsphere;
(3) it takes 20g porous microsphere to be added to 100mL to go from water, addition 12g glacial acetic acid stirs evenly, and adds 16g polymerization chlorine
Change aluminium and 12.8g magnesium sulfate, after stirring and adsorbing 3h, dry 14h, is obtained composite modified porous at 5 times wash with distilled water, 90 DEG C
Microballoon flocculant.
The preparation method of middle polar resin adsorbent, includes the following steps:
(1) 200mL deionized water, 10g sodium chloride are added in three-necked flask, 5g hydroxyethyl cellulose is warming up to 60 DEG C,
300r/min is stirred to dissolution and is obtained mixed solution A;
(2) by 23g diethylaminoethyl methacrylate, 30g acrylic acid-2-ethyl-own ester, 26g butyl acrylate and
10g divinylbenzene, 0.9g azodiisobutyronitrile, 0.56g ethylene glycol dimethacrylate stir evenly, and add 7g 14#
White oil stirs evenly to obtain mixed solution B;
(3) mixed solution B is added in mixed solution A, is stirred to react 5h, then heat to 60 DEG C of heat preservation 3h, it is cooling
It to room temperature, is cleaned 3 times with acetone, deionized water is cleaned 3 times, and 80 DEG C of vacuum drying 10h are up to middle polar resin adsorbent.
It is bimetallic the preparation method comprises the following steps: by 1000 DEG C of calcining 2h of permutite, by 2.3g that permutite loads Nanoscale Iron magnesium
FeCl3·6H2O and 1.6g Mg (NO3)2·6H2O is dissolved in 200mL 10wt% ethanol solution, is subsequently placed in flask, then plus
Enter the calcined permutite of 20g, be stirred to react 30h for 60 DEG C in nitrogen atmosphere, take out and use washes of absolute alcohol 3 times, go from
Sub- water cleans 3 times, and 80 DEG C of vacuum drying 12h load Nanoscale Iron magnesium bimetallic up to permutite.
Rare earth doped atlapulgite the preparation method comprises the following steps: 24g atlapulgite and 100mL deionized water are configured to mix
Liquid is closed, 900r/min is stirred continuously, and 2.1g lanthana is then added and stirs 2h, filters, by 80 DEG C of solid content dry 5h, then
700 DEG C of calcining 2h after being cooled to room temperature, pulverize up to rare earth doped atlapulgite.
Embodiment 5
38 parts of composite modified porous microsphere flocculant, 49 parts of middle polar resin adsorbent, permutite is taken to load Nanoscale Iron
22 parts of magnesium bimetallic, 18 parts of rare earth doped atlapulgite after mixing, dry in ball milling 2h, then 55 DEG C of vacuum ovens
It is dry, obtain dyeing waste water efficient process agent.
Modified porous microballoon is prepared by following preparation methods:
(1) 420mL oil phase is added in the reactor, adjustment revolving speed stirs 10min, is warming up to 50 DEG C, 4g sorbester p18 is added,
40min is stirred, is cooled to room temperature and 100mL 1.2g/mL Herba Lycopodii polysaccharide solution is added, 50min is stirred at room temperature and obtains uniformly
Lotion, the oil are mutually that methyl-silicone oil and glycerol are mixed according to volume ratio 4:3;
(2) 8.5mL ethyl acetate, 11mL cyclohexanol, 12mL ethylenediamine and 13mL glutaraldehyde are added into step (1) lotion
It is stirred to react 7h and obtains porous microsphere;
(3) it takes 20g porous microsphere to be added to 100mL to go from water, addition 11g glacial acetic acid stirs evenly, and adds 17g polymerization chlorine
Change aluminium and 12.4g magnesium sulfate, after stirring and adsorbing 3h, dry 14h, is obtained composite modified porous at 5 times wash with distilled water, 90 DEG C
Microballoon flocculant.
The preparation method of middle polar resin adsorbent, includes the following steps:
(1) 200mL deionized water, 10g sodium chloride are added in three-necked flask, 5g hydroxyethyl cellulose is warming up to 60 DEG C,
300r/min is stirred to dissolution and is obtained mixed solution A;
(2) by 23g diethylaminoethyl methacrylate, 30g acrylic acid-2-ethyl-own ester, 26g butyl acrylate and
10g divinylbenzene, 1.1g azodiisobutyronitrile, 0.45g ethylene glycol dimethacrylate stir evenly, and add 8g 14#
White oil stirs evenly to obtain mixed solution B;
(3) mixed solution B is added in mixed solution A, is stirred to react 5h, then heat to 60 DEG C of heat preservation 3h, it is cooling
It to room temperature, is cleaned 3 times with acetone, deionized water is cleaned 3 times, and 80 DEG C of vacuum drying 10h are up to middle polar resin adsorbent.
It is bimetallic the preparation method comprises the following steps: by 1000 DEG C of calcining 2h of permutite, by 2.1g that permutite loads Nanoscale Iron magnesium
FeCl3·6H2O and 1.8g Mg (NO3)2·6H2O is dissolved in 200mL 10wt% ethanol solution, is subsequently placed in flask, then plus
Enter the calcined permutite of 20g, be stirred to react 30h for 60 DEG C in nitrogen atmosphere, take out and use washes of absolute alcohol 3 times, go from
Sub- water cleans 3 times, and 80 DEG C of vacuum drying 12h load Nanoscale Iron magnesium bimetallic up to permutite.
Rare earth doped atlapulgite the preparation method comprises the following steps: 24g atlapulgite and 100mL deionized water are configured to mix
Liquid is closed, 900r/min is stirred continuously, and 1.9g lanthana is then added and stirs 2h, filters, by 80 DEG C of solid content dry 5h, then
700 DEG C of calcining 2h after being cooled to room temperature, pulverize up to rare earth doped atlapulgite.
Comparative example 1
This comparative example is not the difference from embodiment 1 is that add composite modified porous microsphere flocculant.
Comparative example 2
This comparative example is the difference from embodiment 1 is that polar resin adsorbent in not adding.
Comparative example 3
This comparative example loads Nanoscale Iron magnesium bimetallic the difference from embodiment 1 is that not adding permutite.
Comparative example 4
This comparative example is not the difference from embodiment 1 is that add rare earth doped atlapulgite.
The dyeing waste water efficient process agent being prepared in embodiment 1-5 and comparative example 1-4 is tested for the property:
Influent quality: BOD5For 400mg/L, CODCrFor 800mg/L, coloration is 500 times, SS 600mg/L, pH value
12.44。
Percent of decolourization: using UV751-GD it is ultraviolet/visible spectrophotometer measurement dyeing waste water under a certain specific wavelength
Absorbance determines its percent of decolourization.
The measurement of COD removal rate test reference GB11914-89 water chemical oxygen demand: potassium dichromate method.
The measurement of BOD removal rate test reference HJ 505-2009 water quality five-day BOD (BOD5): dilution and inoculation
Method.
The measurement of SS removal rate refers to the measurement of 89 suspended matter of GB11901-: gravimetric method.
Test result is shown in Table 1:
Table 1
Percent of decolourization/% | CODcrRemoval rate/% | BOD5Removal rate/% | SS removal rate/% | |
Embodiment 1 | 93.59 | 90.82 | 89.54 | 89.77 |
Embodiment 2 | 95.34 | 93.19 | 90.42 | 90.67 |
Embodiment 3 | 97.11 | 93.74 | 90.77 | 91.42 |
Embodiment 4 | 97.72 | 94.36 | 92.13 | 92.15 |
Embodiment 5 | 98.46 | 95.55 | 92.86 | 93.36 |
Comparative example 1 | 86.77 | 82.64 | 74.15 | 80.14 |
Comparative example 2 | 87.12 | 80.55 | 72.99 | 81.72 |
Comparative example 3 | 89.46 | 81.43 | 74.13 | 78.65 |
Comparative example 4 | 88.44 | 81.27 | 75.82 | 77.49 |
By test result it is found that the composite modified porous microsphere flocculant prepared in the present invention, middle polar resin adsorbent,
When permutite loads Nanoscale Iron magnesium bimetallic, rare earth doped atlapulgite is used in conjunction with, obtained dyeing waste water is efficient
Inorganic agent is best to the adsorption and sedimentation and coagulation effect of dyeing waste water, reaches 93.59-98.46% to sewage decoloring rate, to CODcr
Removal rate reaches 95.55-90.82%, to BOD5Removal rate reaches 89.54-92.86%, and SS removal rate reaches 89.77-
93.36%.The dyeing waste water efficient process agent being prepared in embodiment 5 in the present invention has reached optimal treatment effect.
Claims (9)
1. a kind of dyeing waste water efficient process agent, which is characterized in that be made of each ingredient of following parts by weight:
32-44 parts of composite modified porous microsphere flocculant, 45-52 parts of middle polar resin adsorbent, permutite load Nanoscale Iron
It is 18-26 parts of magnesium bimetallic, atlapulgite 14-22 parts rare earth doped.
2. dyeing waste water efficient process agent according to claim 1, which is characterized in that the system of the modified porous microballoon
Preparation Method includes the following steps:
(1) oily phase is added in the reactor, adjustment revolving speed stirs 10min, is warming up to 50 DEG C, and emulsifier is added, stirs 40min,
It is cooled to room temperature and Herba Lycopodii polysaccharide solution is added, stir 50min at room temperature and obtain homogeneous latex emulsion;
(2) ethyl acetate, cyclohexanol, ethylenediamine and glutaraldehyde are added into step (1) lotion, be stirred to react 7h obtain it is porous micro-
Ball;
(3) it taking porous microsphere to be added to 100mL to go from water, addition glacial acetic acid stirs evenly, aluminium polychloride and magnesium sulfate are added,
After stirring and adsorbing 3h, clean dry obtains composite modified porous microsphere flocculant.
3. dyeing waste water efficient process agent according to claim 2, which is characterized in that oil Xiang Weijia described in step (1)
Base silicone oil and glycerol are according to volume ratio (2-6): (1-5) is mixed.
4. dyeing waste water efficient process agent according to claim 2, which is characterized in that oil phase described in step (1), emulsification
The volume ratio of agent and Herba Lycopodii polysaccharide solution is (2.7-5.6): 0.04:1.
5. dyeing waste water efficient process agent according to claim 2, which is characterized in that ethyl acetate described in step (2),
The volume ratio of cyclohexanol, ethylenediamine and glutaraldehyde is (6-11): (9-13): (10-14): (12-16);It is more described in step (3)
Hole microballoon, glacial acetic acid, aluminium polychloride and magnesium sulfate weight ratio be 2:(0.8-1.4): (1.5-1.9): (1.12-1.36).
6. dyeing waste water efficient process agent according to claim 1, which is characterized in that the middle polar resin adsorbent
Preparation method, include the following steps:
(1) 200mL deionized water, 10g sodium chloride are added in three-necked flask, 5g hydroxyethyl cellulose is warming up to 60 DEG C,
300r/min is stirred to dissolution and is obtained mixed solution A;
(2) by 23g diethylaminoethyl methacrylate, 30g acrylic acid-2-ethyl-own ester, 26g butyl acrylate and 10g bis-
Vinyl benzene, 0.7-1.4g azodiisobutyronitrile, 0.24-0.66g ethylene glycol dimethacrylate stir evenly, and add 6-
10g 14# white oil stirs evenly to obtain mixed solution B;
(3) mixed solution B is added in mixed solution A, is stirred to react 5h, then heated to 60 DEG C of heat preservation 3h, be cooled to room
Temperature is dried in vacuo up to middle polar resin adsorbent after cleaning.
7. dyeing waste water efficient process agent according to claim 1, which is characterized in that the permutite loads nanometer
The bimetallic preparation method of iron magnesium includes the following steps: by 1000 DEG C of calcining 2h of permutite, by 1.7-2.5g FeCl3·
6H2O and 1.4-2.2g Mg (NO3)2·6H2O is dissolved in 200mL 10wt% ethanol solution, is subsequently placed in flask, is added
The calcined permutite of 20g is stirred to react 30h for 60 DEG C in nitrogen atmosphere, and permutite's load obtained by drying is cleaned in taking-up
Nanoscale Iron magnesium bimetallic.
8. dyeing waste water efficient process agent according to claim 1, which is characterized in that the rare earth doped activity
The preparation method of carclazyte, includes the following steps:
24g atlapulgite and 100mL deionized water are configured to mixed liquor, 900r/min is stirred continuously, and 1.6- is then added
2.2g lanthana stirs 2h, and after filtering drying, 700 DEG C of calcining 2h pulverize white up to rare earth doped activity after cooling
Soil.
9. a kind of preparation method of dyeing waste water efficient process agent according to claim 1-8, including walk as follows
It is rapid: 32-44 parts of composite modified porous microsphere flocculant, 45-52 parts of middle polar resin adsorbent, permutite being taken to load Nanoscale Iron
18-26 parts of magnesium bimetallic, it is rare earth doped atlapulgite 14-22 parts after mixing, ball milling 2h, then 55 DEG C of vacuum ovens
Middle drying obtains dyeing waste water efficient process agent.
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