CN102335586B - Preparation method of printing and dyeing wastewater treating material - Google Patents
Preparation method of printing and dyeing wastewater treating material Download PDFInfo
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- CN102335586B CN102335586B CN 201110268019 CN201110268019A CN102335586B CN 102335586 B CN102335586 B CN 102335586B CN 201110268019 CN201110268019 CN 201110268019 CN 201110268019 A CN201110268019 A CN 201110268019A CN 102335586 B CN102335586 B CN 102335586B
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Abstract
The invention discloses a preparation method of a printing and dyeing wastewater treating material. The method comprises the following steps of: adding hydrochloric acid or sulfuric acid into bentonite to obtain slurry, mixing the slurry and quicklime powder, adding the mixture into sodium dodecyl benzene sulphonate solution, precipitating for separation, drying and milling to obtain powder; slowly adding the obtained powder into a neutral inorganic precursor with intensive stirring, baking, and thus obtaining porous clay heterogeneous material powder; soaking in phosphoric acid solution to obtain phosphoric acid-adsorbed powder; and mixing clam shells and acetic acid to react, extracting supernatant fluid, adding the obtained phosphoric acid-adsorbed powder into the supernatant fluid, stirring, filtering and drying. In the preparation method, a common cheap anionic surfactant is used for preparing a porous clay heterogeneous material, the clam shells are used for dissolving calcium acetate out, the calcium acetate is reacted with phosphoric acid which is adsorbed on the surface of the porous clay heterogeneous material, and calcium phosphate is generated on the surface of the porous clay heterogeneous material through sedimentation, so that the dye adsorbing performance of the porous clay heterogeneous material is improved, and printing and dyeing wastewater can be effectively treated.
Description
Technical field
The present invention relates to a kind for the treatment of of dyeing wastewater material preparation method, belong to technical field of sewage in the environmental protection.
Background technology
Contain multiple dyestuff in the industrial wastewater of textile printing and dyeing industry, these industrial wastewater characteristics are organic concentration height, complicated component, biodegradability is poor, colourity is high and changeable, water quality and quantity changes greatly, belong to more unmanageable industrial wastewater.In recent years research finds that absorption method is to process the effective ways of such waste water, because of low, the easy operation of cost of absorption method, insensitive to toxicant, in weak solution, also can remove pollutant fully.
The advantages such as adobe isomery material has the large aperture and the aperture homogeneous can be regulated, the space degree of order high, specific area is large, but also have better mechanical stability, hydrothermal stability.General the synthetic of adobe material comprises: (1) introduces interlayer with the organic cation surfactant as template; (2) introduce neutral inorganic precursor and in the interlayer pass of 2:1 type layered clay mineral, carry out interlayer hydrolysis and condensation polymerization; (3) remove the surfactant templates agent through roasting, obtain the adobe material.The template that adopts in the preparation process has multiple, but requisite be cationic surfactant, this reagent is expensive, has increased to a certain extent adobe isomery material preparation cost.In addition, because adobe isomery material mainly is silica structure, its hydrophobic effect causes therefore hydrophilic Dye Adsorption effect and bad is necessary its modifying surface.
The clam shell is the shell of ocean class animal; harder have a protective effect; it is a kind of natural calcium material that is easier to utilize; outermost layer is comprised of protein; middle one deck is calcite, and the inside is that itself has certain treatment effect to dyeing waste water but be unsatisfactory by the smooth plate shape calcium carbonate crystal composition of one deck; but its contained calcareous modified porous clay isomery material that can be used for can make it become a kind of preferably dyeing waste water adsorbent.
Summary of the invention
The objective of the invention is for overcoming the deficiencies in the prior art, a kind for the treatment of of dyeing wastewater material preparation method is provided, utilize the cheap synthesizing porous clay isomery of anion surfactant material, and utilize the natural calcium material that the phosphatization modification is carried out on its surface, strengthen this material to the absorption affinity of dyestuff.
The technical solution used in the present invention is to adopt following steps:
1) be that 25% ~ 35% sulfuric acid or hydrochloric acid add particle diameter in 60 orders ~ 100 orders and water content are 10 ~ 15% bentonite slurry with concentration, every gram bentonite adds 2 ~ 3mmol hydrochloric acid or 1 ~ 1.5mmol sulfuric acid, fully stir, make mud, use again steam digestion 5 ~ 6h, stirred once every 15 minutes therebetween, wash to pH be 4 ~ 5, concentrated, filter, 80 ℃ ~ 110 ℃ lower dry and pulverizing, make powdery product;
2) be the ratio mixing of 1:0.05 ~ 0.5 in mass ratio with powdery product and the dry quick lime powder that makes, be added dropwise to the water that weight is 2 ~ 2.5 times in this mixture while stirring again, stir into pasty state, place thermostatic drying chamber, reaction 24h ~ 48h under temperature is 50 ~ 65 ℃, wash 4 ~ 5 times, oven dry is milled;
3) will mill that to add concentration be in the neopelex solution of 50 mg/L ~ 300 mg/L for the product that obtains, the solid-liquid mass ratio is 1:1000 ~ 1:10000, stirs 4 ~ 5h, precipitate and separate, and oven dry is milled into powder;
4) at room temperature, the powder that step 3) is obtained slowly adds neutral inorganic precursor for 1:50 ~ 1:150 in mass ratio under vigorous stirring, continue to stir 3 ~ 4h, described neutral inorganic precursor is a kind of in methyl silicate, ethyl orthosilicate, positive silicic acid propyl ester, the butyl silicate;
5) be warming up to 500 ℃ ~ 750 ℃ with 2 ℃/min ~ 5 ℃/min speed after drying under the Separation of Solid and Liquid, room temperature under air atmosphere, roasting 5 ~ 10 h obtain faint yellow adobe isomery material powder:
6) this adobe isomery material powder being soaked in concentration is 5 ~ 6 h in 5% ~ 10% the phosphoric acid solution, and solid-to-liquid ratio is 1:100 ~ 1:500, filters, and with the solid oven dry, obtains adsorbing the powder that phosphoric acid is arranged.
7) the clam shell clean being removed impurity with running water, with being milled into powder, is that 10% ~ 15% acetic acid is pressed solid-liquid mass ratio 1 with this powder and concentration after the oven dry
:The amount of 3 ~ 1:10 is mixed, at 25 ℃ of lower constant temperature oscillation reaction 5 ~ 6 h;
8) after vibration finishes, get supernatant, it is that 1:10 ~ 1:30 adds in this supernatant by the solid-liquid mass ratio that the absorption of step 6) gained is had the powder of phosphoric acid, stirs 2 ~ 3 h, filters rear 105 ℃ of oven dry and gets final product.
The present invention utilizes cheap common anion surfactant to prepare adobe isomery material and utilizes cheap clam shell stripping to obtain calcium acetate, with calcium acetate and the phosphatase reaction that is adsorbed on adobe isomery material surface, generate calcium phosphate at its surface deposition, improve adobe isomery material to the absorption property of dyestuff.The material preparation cost is low, and effectively treatment of dyeing and printing is simple to operate, economical and efficient.
The specific embodiment
Be that 25% ~ 35% sulfuric acid or hydrochloric acid add particle diameter in 60 orders ~ 100 orders and water content are 10 ~ 15% bentonite slurry with concentration, sulfuric acid or hydrochloric acid and bentonite consumption are that every gram dry weight bentonite adds 2 ~ 3mmol hydrochloric acid or 1 ~ 1.5mmol sulfuric acid, sulfuric acid or hydrochloric acid and bentonite slurry fully stir, make mud, again with steam to its digestion 5 ~ 6h, therebetween, stirred once every 15 minutes, then washing, making its pH is 4 ~ 5, concentrated, filters, 80 ℃ ~ 110 ℃ lower dry and pulverizing, make powdery product.Be that the ratio of 1:0.05 ~ 0.5 is mixed with the powdery product that makes and dry quick lime powder according to mass ratio, obtain mixture of powders, be added dropwise to again weight while stirring the mixture and be the water of 2 ~ 2.5 times of this mixture of powders, stir into pasty state, placing thermostatic drying chamber, is 50 ~ 65 ℃ of lower reaction 24h ~ 48h in temperature, washes 4 ~ 5 times, oven dry is milled.
It is in the neopelex solution of 50 mg/L ~ 300 mg/L that the product that obtains milling adds concentration, the mill product that obtains and the solid-liquid mass ratio of neopelex solution is 1:1000 ~ 1:10000, then stir together 4 ~ 5h, like this, just the anion surfactant of neopelex is introduced the interlayer of the product that obtains of milling as template, precipitate and separate is dried again, is milled into powder.Then, in the interlayer pass of product, carry out interlayer hydrolysis and condensation polymerization, method is: at room temperature, be that 1:50 ~ 1:150 slowly adds in the neutral inorganic precursor under intense agitation in mass ratio with this powder, continue to stir 3 ~ 4h, neutral inorganic precursor is a kind of in methyl silicate, ethyl orthosilicate, positive silicic acid propyl ester, the butyl silicate.Carry out Separation of Solid and Liquid again, under air atmosphere, be warming up to 500 ℃ ~ 750 ℃ with 2 ℃/min ~ 5 ℃/min speed after drying under the room temperature, roasting 5 ~ 10 h obtain faint yellow adobe isomery material powder to remove the anion surfactant template.It is 5 ~ 6 h in 5% ~ 10% the phosphoric acid solution that this adobe isomery material powder is soaked in concentration, and its solid-to-liquid ratio is: 1:100 ~ 1:500, filter, and with the solid oven dry, obtain adsorbing the powder that phosphoric acid is arranged.
The clam shell clean is removed impurity with running water, with being milled into powder, is that 10% ~ 15% acetic acid is pressed solid-liquid mass ratio 1 with this powder and concentration after the oven dry
:The amount of 3 ~ 1:10 is mixed, at 25 ℃ of lower constant temperature oscillation reaction 5 ~ 6 h.Vibration is got supernatant after finishing, and the supernatant main component is calcium acetate, and absorption being had the powder of phosphoric acid is that 1:10 ~ 1:30 adds in this supernatant by the solid-liquid mass ratio, stirs 2 ~ 3 h, filters rear 105 ℃ of oven dry, namely obtains the material for treatment of dyeing wastewater.
Below provide 4 embodiment of the present invention to further specify the present invention:
Embodiment 1
Be that 35% sulfuric acid adds particle diameter in 100 orders and water content are 15% bentonite slurry with concentration, sulfuric acid and bentonite consumption are to add 1 mmol sulfuric acid in the bentonite of every gram dry weight, fully stir, make mud, use again steam digestion 6h, stirred once every 15 minutes therebetween, through wash to pH be 5, concentrated, filter, also pulverize 110 ℃ of lower dryings; The powdery product that makes.Be that the ratio of 2:1 is mixed with the powdery product that makes and dry quick lime powder according to mass ratio, stir again on one side and be added dropwise to the water that weight is 2.5 times in this mixture, stir into pasty state, placing thermostatic drying chamber, is 65 ℃ of lower reaction 48h in temperature, washes 5 times, oven dry is milled; It is in the neopelex solution of 300 mg/L that the product that obtains milling adds concentration, and the solid-liquid mass ratio is 1:10000, stirs 4 ~ 5h, precipitate and separate, and oven dry is milled, and anion surfactant is introduced the interlayer of the product that obtains of milling as template; At room temperature, the powder that obtains milling the in mass ratio ratio of 1:150 slowly adds neutral inorganic precursor methyl silicate under vigorous stirring, continue to stir 4h; Under air atmosphere, be warming up to 750 ℃ with 5 ℃/min speed after drying under the Separation of Solid and Liquid, room temperature, roasting 10 h obtain faint yellow adobe isomery material powder to remove surfactant templates; It is 6 h in 5% the phosphoric acid solution that this adobe isomery material powder is soaked in concentration, and adobe isomery material powder and phosphoric acid solution solid-to-liquid ratio are: 1:500, filter, and obtain adsorbing the pressed powder that phosphoric acid is arranged, dry for standby.The clam shell clean is removed impurity with running water, after the oven dry with being milled into powder, with this powder and concentration be 15% acetic acid by the amount mixing of solid-liquid mass ratio 1:10, react 6 h at 25 ℃ of lower constant temperature oscillations; Vibration is got supernatant after finishing, and the before absorption of gained is had the powder of phosphoric acid be soaked in this supernatant by solid-liquid mass ratio 1:30, stirs 3 h, filters rear 105 ℃ of oven dry, namely obtains the material for treatment of dyeing wastewater.Process anionic dye Orange II with this material, when the dyestuff initial concentration was 300 mg/L, clearance was up to 96.9%.
Embodiment 2
Be that 25% hydrochloric acid adds particle diameter in 60 orders and water content are 10% bentonite slurry with concentration, acid and bentonite consumption are that every gram bentonite (dry weight) adds 3mmol hydrochloric acid, fully stir, make mud, use again steam digestion 5h, stirred once every 15 minutes therebetween, through wash to pH be 4, concentrated, filter, also pulverize 80 ℃ of lower dryings; Be that the ratio of 1:0.05 is mixed with the powdery product that makes and dry quick lime powder according to mass ratio, stir again on one side and be added dropwise to the water that weight is 2 times in this mixture, stir into pasty state, placing thermostatic drying chamber, is 50 ℃ of lower reaction 24h in temperature, washes 4 times, oven dry is milled; It is in the neopelex solution of 50 mg/L that the product that obtains milling adds concentration, and the solid-liquid mass ratio is 1:1000, stirs 4h, precipitate and separate, and oven dry is milled; At room temperature, the powder that obtains milling in mass ratio 1:50 slowly adds neutral inorganic precursor ethyl orthosilicate under vigorous stirring, continue to stir 3h; Under air atmosphere, be warming up to 500 ℃ with 2 ℃/min speed after drying under the Separation of Solid and Liquid, room temperature, roasting 5h obtains pale yellow powder to remove the surfactant templates agent; It is 5 h in 10% the phosphoric acid solution that this powder is soaked in concentration, and powder and phosphoric acid solution solid-to-liquid ratio are: 1:100, filter, with the solid dry for standby.The clam shell clean is removed impurity with running water, with being milled into powder, is that 10% acetic acid is by solid-liquid mass ratio 1 with this powder and concentration after the oven dry
:3 amount is mixed, at 25 ℃ of lower constant temperature oscillation reaction 5h; Vibration is got supernatant after finishing, and has the powder of phosphoric acid to be soaked in this supernatant by solid-liquid mass ratio 1:10 before gained absorption, stirs 2h, filters rear 105 ℃ of oven dry, namely obtains the material for treatment of dyeing wastewater.Process anionic dye Orange G with this material, when the dyestuff initial concentration was 320 mg/L, clearance was up to 91.4%.
Embodiment 3
Be that 30% sulfuric acid adds particle diameter in 80 orders and water content are 12% bentonite slurry with concentration, sulfuric acid and bentonite consumption are that every gram bentonite (dry weight) adds 1.5mmol sulfuric acid, fully stir, make mud, use again steam digestion 5h, stirred once every 15 minutes therebetween, through wash to pH be 5, concentrated, filter, also pulverize 90 ℃ of lower dryings; Be that the ratio of 5:1 is mixed with the powdery product that makes and dry quick lime powder according to mass ratio, stir again on one side and be added dropwise to the water that weight is 2 times in this mixture, stir into pasty state, placing thermostatic drying chamber, is 60 ℃ of lower reaction 30h in temperature, washes 4 times, oven dry is milled; It is in the neopelex solution of 100 mg/L that the product that obtains milling adds concentration, and the solid-liquid mass ratio is 1:2000, stirs 4h, precipitate and separate, and oven dry is milled, and anion surfactant is introduced the interlayer of the product that obtains of milling as template.At room temperature, the powder that obtains milling slowly adds the positive silicic acid propyl ester of neutral inorganic precursor for 1:100 in mass ratio under vigorous stirring, continue to stir 4h; Under air atmosphere, be warming up to 600 ℃ with 3 ℃/min speed after drying under the Separation of Solid and Liquid, room temperature, roasting 6 h obtain faint yellow adobe isomery material powder to remove surfactant templates; It is 6 h in 6% the phosphoric acid solution that this powder is soaked in concentration, and powder and phosphoric acid solution solid-to-liquid ratio are: 1:300, filter, and with this solid oven dry, obtain adsorbing and have the pressed powder of phosphoric acid for subsequent use.The clam shell clean is removed impurity with running water, after the oven dry with being milled into powder, with this powder and concentration be 12% acetic acid by the amount mixing of solid-liquid mass ratio 1:5, react 6 h at 25 ℃ of lower constant temperature oscillations; Vibration is got supernatant after finishing, and has the powder of phosphoric acid to be soaked in this supernatant by solid-liquid mass ratio 1:20 before gained absorption, stirs 2h, filters rear 105 ℃ of oven dry, namely obtains the material for treatment of dyeing wastewater.Process anionic dye Orange II with this material, when the dyestuff initial concentration was 350 mg/L, clearance was up to 95.8%.
Embodiment 4
Be that 30% hydrochloric acid adds particle diameter in 70 orders and water content are 14% bentonite slurry with concentration, hydrochloric acid and bentonite consumption are that every gram bentonite (dry weight) adds 2 mmol hydrochloric acid, fully stir, make mud, use again steam digestion 5h, stirred once every 15 minutes therebetween, through wash to pH be 4, concentrated, filter, also pulverize 90 ℃ of lower dryings; The powdery product that makes and the dry quick lime powder mass ratio according to 4:1 is mixed, stir again on one side and be added dropwise to the water that weight is 2 times in this mixture, stir into pasty state, placing thermostatic drying chamber, is 55 ℃ of lower reaction 40h in temperature, washes 4 times, oven dry is milled; It is in the neopelex solution of 200 mg/L that the product that obtains milling adds concentration, and the solid-liquid mass ratio is 1:8000, stirs 4h, the anion surfactant of neopelex is introduced the interlayer of the product that obtains of milling as template, precipitate and separate is dried again, mills.At room temperature, the powder that obtains milling is the neutral inorganic precursor butyl silicate of slow adding under vigorous stirring of 1:130 in mass ratio, continues to stir 3h; Separation of Solid and Liquid under air atmosphere, is warming up to 700 ℃ with 4 ℃/min speed after drying under the room temperature again, and roasting 8h obtains pale yellow powder to remove surfactant templates; It is 5 h in 8% the phosphoric acid solution that this powder is soaked in concentration, and powder and phosphoric acid solution solid-to-liquid ratio are: 1:400, filter, and with the solid oven dry, obtain adsorbing and have the powder of phosphoric acid for subsequent use.The clam shell clean is removed impurity with running water, with being milled into powder, is that 14% acetic acid is by solid-liquid mass ratio 1 with this powder and concentration after the oven dry
:8 amount is mixed, at 25 ℃ of lower constant temperature oscillation reaction 5h; Vibration is got supernatant after finishing, and the supernatant main component is calcium acetate, has the powder of phosphoric acid to be soaked in this supernatant by solid-liquid mass ratio 1:25 before gained absorption, stirs 2h, filters rear 105 ℃ of oven dry, namely obtains the material for treatment of dyeing wastewater.Process the anionic dye reactive red with this material, when the dyestuff initial concentration was 280 mg/L, clearance was up to 97.1%.
Claims (1)
1. treatment of dyeing wastewater material preparation method is characterized in that in turn including the following steps:
1) be that 25% ~ 35% sulfuric acid or hydrochloric acid add particle diameter in 60 orders ~ 100 orders and water content are 10 ~ 15% bentonite slurry with concentration, every gram bentonite adds 2 ~ 3mmol hydrochloric acid or 1 ~ 1.5mmol sulfuric acid, fully stir, make mud, use again steam digestion 5 ~ 6h, stirred once every 15 minutes therebetween, wash to pH be 4 ~ 5, concentrated, filter, 80 ℃ ~ 110 ℃ lower dry and pulverizing, make powdery product;
2) be the ratio mixing of 1:0.05 ~ 0.5 in mass ratio with powdery product and the dry quick lime powder that makes, be added dropwise to the water that weight is 2 ~ 2.5 times in this mixture while stirring again, stir into pasty state, place thermostatic drying chamber, reaction 24h ~ 48h under temperature is 50 ~ 65 ℃, wash 4 ~ 5 times, oven dry is milled;
3) will mill that to add concentration be in the neopelex solution of 50 mg/L ~ 300 mg/L for the product that obtains, the solid-liquid mass ratio is 1:1000 ~ 1:10000, stirs 4 ~ 5h, precipitate and separate, and oven dry is milled into powder;
4) at room temperature, the powder that step 3) is obtained slowly adds neutral inorganic precursor for 1:50 ~ 1:150 in mass ratio under vigorous stirring, continue to stir 3 ~ 4h, described neutral inorganic precursor is a kind of in methyl silicate, ethyl orthosilicate, positive silicic acid propyl ester, the butyl silicate;
5) be warming up to 500 ℃ ~ 750 ℃ with 2 ℃/min ~ 5 ℃/min speed after drying under the Separation of Solid and Liquid, room temperature under air atmosphere, roasting 5 ~ 10 h obtain faint yellow adobe isomery material powder;
6) this adobe isomery material powder being soaked in concentration is 5 ~ 6 h in 5% ~ 10% the phosphoric acid solution, and solid-to-liquid ratio is 1:100 ~ 1:500, filters, and with the solid oven dry, obtains adsorbing the powder that phosphoric acid is arranged;
7) the clam shell clean being removed impurity with running water, with being milled into powder, is that 10% ~ 15% acetic acid is pressed solid-liquid mass ratio 1 with this powder and concentration after the oven dry
:The amount of 3 ~ 1:10 is mixed, at 25 ℃ of lower constant temperature oscillation reaction 5 ~ 6 h;
8) after vibration finishes, get supernatant, it is that 1:10 ~ 1:30 adds in this supernatant by the solid-liquid mass ratio that the absorption of step 6) gained is had the powder of phosphoric acid, stirs 2 ~ 3 h, filters rear 105 ℃ of oven dry and gets final product.
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| CN104276693A (en) * | 2014-10-09 | 2015-01-14 | 常州大学 | Method for treating congo red in printing and dyeing waste water |
| CN107597067A (en) * | 2017-10-10 | 2018-01-19 | 孙祎 | A kind of preparation method for the treatment of of dyeing/printing wastewaters |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4780215A (en) * | 1987-06-08 | 1988-10-25 | Carlson Russell L | Water purification device |
| CN1673108A (en) * | 2005-03-24 | 2005-09-28 | 浙江大学 | Prepn process of magnetic composite organic bentonite as water treating material |
| CN1843951A (en) * | 2006-04-19 | 2006-10-11 | 浙江大学 | Method for treating printing/dyeing waste water |
| CN101254925A (en) * | 2008-03-25 | 2008-09-03 | 江苏工业学院 | Bentonite reclaiming utilization method |
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2011
- 2011-09-13 CN CN 201110268019 patent/CN102335586B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4780215A (en) * | 1987-06-08 | 1988-10-25 | Carlson Russell L | Water purification device |
| CN1673108A (en) * | 2005-03-24 | 2005-09-28 | 浙江大学 | Prepn process of magnetic composite organic bentonite as water treating material |
| CN1843951A (en) * | 2006-04-19 | 2006-10-11 | 浙江大学 | Method for treating printing/dyeing waste water |
| CN101254925A (en) * | 2008-03-25 | 2008-09-03 | 江苏工业学院 | Bentonite reclaiming utilization method |
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Effective date of registration: 20151030 Address after: Daitou town of Liyang City Ferry Street 213311 Jiangsu city of Changzhou province 8-2 No. 7 Patentee after: Liyang Chang Technology Transfer Center Co., Ltd. Address before: Gehu Lake Road Wujin District 213164 Jiangsu city of Changzhou province No. 1 Patentee before: Changzhou University |