CN102335586A - 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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- CN102335586A CN102335586A CN2011102680190A CN201110268019A CN102335586A CN 102335586 A CN102335586 A CN 102335586A CN 2011102680190 A CN2011102680190 A CN 2011102680190A CN 201110268019 A CN201110268019 A CN 201110268019A CN 102335586 A CN102335586 A CN 102335586A
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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 of treatment of dyeing wastewater preparation methods, 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.The absorption method of discovering in recent years is to handle 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.
Adobe isomery material has advantages such as large aperture and aperture homogeneous scalable, the space degree of order is high, specific area is big, but also has better mechanical stability, hydrothermal stability.General the synthetic of adobe material comprises: (1) is introduced interlayer with the organic cation surfactant as template; (2) introduce neutral inorganic precursor and in the interlayer duct 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 costs an arm and a leg, and has increased the preparation cost of adobe isomery material to a certain extent.In addition, because adobe isomery material mainly is the silica structure, its hydrophobic effect causes therefore hydrophilic dyestuff adsorption effect and bad is necessary modification is carried out on its surface.
The clam shell is the shell of ocean class animal, and harder have a protective effect, is a kind of natural calcium material that is easier to utilize; Outermost layer is made up of protein; Middle one deck is a calcite, and the inside is made up of the smooth plate shape calcium carbonate crystal of one deck, and own have certain treatment effect but unsatisfactory to dyeing waste water; But its contained calcareous modified porous clay isomery material that can be used for can make it become a kind of adsorbent of dyeing waste water preferably.
Summary of the invention
The objective of the invention is for overcoming the deficiency of prior art; A kind of treatment of dyeing wastewater preparation methods 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 the absorption affinity of this material to dyestuff.
The technical scheme that the present invention adopts 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 stirs; Process mud, use steam digestion 5 ~ 6h again, whenever stirred once therebetween at a distance from 15 minutes; Wash to pH be 4 ~ 5, concentrate, filter; 80 ℃ ~ 110 ℃ dry down and pulverizing, make powdery product;
2) be the mixed of 1:0.05 ~ 0.5 with the powdery product that makes by mass ratio with dry quick lime powder; Be added dropwise to the water of weight while stirring again, stir into pasty state, place thermostatic drying chamber for 2 ~ 2.5 times in this mixture; In temperature is 50 ~ 65 ℃ of reaction 24h ~ 48h down; 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 is that 1:50 ~ 1:150 slowly adds neutral inorganic precursor under vigorous stirring by mass ratio; Continue to stir 3 ~ 4h, said neutral inorganic precursor is a kind of in methyl silicate, ethyl orthosilicate, positive silicic acid propyl ester, the butyl silicate;
5) dry the back under the Separation of Solid and Liquid, room temperature and under air atmosphere, be warming up to 500 ℃ ~ 750 ℃ with 2 ℃/min ~ 5 ℃/min speed, 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 being adsorbed with the powder of phosphoric acid.
7) the clam shell clean is removed impurity with running water, the oven dry back is with being milled into powder, is that 10% ~ 15% acetic acid is pressed solid-liquid mass ratio 1 with this powder and concentration
:The amount of 3 ~ 1:10 is mixed, at 25 ℃ of following constant-temperature shaking reaction 5 ~ 6 h;
8) after vibration finishes, getting supernatant, is that 1:10 ~ 1:30 adds in this supernatant with the powder that is adsorbed with phosphoric acid of step 6) gained by the solid-liquid mass ratio, stirs 2 ~ 3 h, filters back 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 the absorption property of adobe isomery material dyestuff.The preparation cost of material is low, and effectively treatment of dyeing and printing is simple to operate, economical and efficient.
The specific embodiment
With concentration is that 25% ~ 35% sulfuric acid or hydrochloric acid add particle diameter in 60 orders ~ 100 orders and water content are 10 ~ 15% bentonite slurry, and sulfuric acid or hydrochloric acid and bentonite consumption are every gram dry weight bentonite adding 2 ~ 3mmol hydrochloric acid or 1 ~ 1.5mmol sulfuric acid, and sulfuric acid or hydrochloric acid and bentonite slurry fully stir; Process mud, again with steam to its digestion 5 ~ 6h, therebetween; Whenever stirred once at a distance from 15 minutes, washing then, making its pH is 4 ~ 5; Concentrate; Filter,, make powdery product 80 ℃ ~ 110 ℃ dry down and pulverizing.Is the mixed of 1:0.05 ~ 0.5 with dry quick lime powder according to mass ratio with the powdery product that makes, and obtains mixture of powders, is added dropwise to the water of weight for 2 ~ 2.5 times of this mixture of powders while stir the mixture again; Stir into pasty state; Placing thermostatic drying chamber, is 50 ~ 65 ℃ of reaction 24h ~ 48h down 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, stirs 4 ~ 5h then together, 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 duct of product, carry out interlayer hydrolysis and condensation polymerization; Method is: at room temperature; Is that 1:50 ~ 1:150 slowly adds in the neutral inorganic precursor under intense agitation with this powder by mass ratio, continues to stir 3 ~ 4h, and 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, dry the back under the room temperature under air atmosphere, be warming up to 500 ℃ ~ 750 ℃ with 2 ℃/min ~ 5 ℃/min speed, 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 being adsorbed with the powder of phosphoric acid.
The clam shell clean is removed impurity with running water, and the oven dry back is with being milled into powder, is that 10% ~ 15% acetic acid is pressed solid-liquid mass ratio 1 with this powder and concentration
:The amount of 3 ~ 1:10 is mixed, at 25 ℃ of following constant-temperature shaking reaction 5 ~ 6 h.Vibration is got supernatant after finishing, and the supernatant main component is a calcium acetate, is that 1:10 ~ 1:30 adds in this supernatant with the powder that is adsorbed with phosphoric acid by the solid-liquid mass ratio, stirs 2 ~ 3 h, filters back 105 ℃ of oven dry, promptly obtains being used for the material of treatment of dyeing wastewater.
Below provide 4 embodiment of the present invention to further specify the present invention:
Embodiment 1
With concentration is that 35% sulfuric acid adds particle diameter in 100 orders and water content are 15% bentonite slurry, and sulfuric acid and bentonite consumption are to add 1 mmol sulfuric acid, fully stirring in the bentonite of every gram dry weight; Process mud, use steam digestion 6h again, whenever stirred once therebetween at a distance from 15 minutes; Through wash to pH be 5; Concentrate, filter, drying is also pulverized under 110 ℃; The powdery product that makes.Is the mixed of 2:1 with dry quick lime powder according to mass ratio with the powdery product that makes, and is added dropwise to the water of weight for 2.5 times in this mixture while stir again, stirs into pasty state; Placing thermostatic drying chamber, is 65 ℃ of reaction 48h down 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 slowly adds neutral inorganic precursor methyl silicate in the ratio of mass ratio 1:150 under vigorous stirring, continue to stir 4h; Dry the back under the Separation of Solid and Liquid, room temperature under air atmosphere, be warming up to 750 ℃ with 5 ℃/min speed, 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 being adsorbed with the pressed powder of phosphoric acid, dry for standby.The clam shell clean is removed impurity with running water, and the oven dry back is with being milled into powder, is the amount mixing by solid-liquid mass ratio 1:10 of 15% acetic acid with this powder and concentration, reacts 6 h 25 ℃ of following constant-temperature shaking; After vibration finishes, get supernatant, with before the powder that is adsorbed with phosphoric acid of gained be soaked in this supernatant by solid-liquid mass ratio 1:30, stir 3 h, filter back 105 ℃ of oven dry, promptly obtain being used for the material of treatment of dyeing wastewater.Handle anionic dye Orange II with this material, when the dyestuff initial concentration was 300 mg/L, clearance was up to 96.9%.
Embodiment 2
With concentration is that 25% hydrochloric acid adds particle diameter in 60 orders and water content are 10% bentonite slurry, and acid is that every gram bentonite (dry weight) adds 3mmol hydrochloric acid with bentonite consumption, fully stirring; Process mud, use steam digestion 5h again, whenever stirred once therebetween at a distance from 15 minutes; Through wash to pH be 4; Concentrate, filter, drying is also pulverized under 80 ℃; Is the mixed of 1:0.05 with dry quick lime powder according to mass ratio with the powdery product that makes, and is added dropwise to the water of weight for 2 times in this mixture while stir again, stirs into pasty state; Placing thermostatic drying chamber, is 50 ℃ of reaction 24h down 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 slowly adds neutral inorganic precursor ethyl orthosilicate by mass ratio 1:50 under vigorous stirring, continue to stir 3h; Dry the back under the Separation of Solid and Liquid, room temperature under air atmosphere, be warming up to 500 ℃ with 2 ℃/min speed, 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, and the oven dry back is with being milled into powder, is that 10% acetic acid is by solid-liquid mass ratio 1 with this powder and concentration
:3 amount is mixed, at 25 ℃ of following constant-temperature shaking reaction 5h; After vibration finishes, get supernatant, with before the gained powder that is adsorbed with phosphoric acid be soaked in this supernatant by solid-liquid mass ratio 1:10, stir 2h, filter back 105 ℃ of oven dry, promptly obtain being used for the material of treatment of dyeing wastewater.Handle anionic dye Orange G with this material, when the dyestuff initial concentration was 320 mg/L, clearance was up to 91.4%.
Embodiment 3
With concentration is that 30% sulfuric acid adds particle diameter in 80 orders and water content are 12% bentonite slurry, and sulfuric acid and bentonite consumption are that every gram bentonite (dry weight) adds 1.5mmol sulfuric acid, fully stirring; Process mud, use steam digestion 5h again, whenever stirred once therebetween at a distance from 15 minutes; Through wash to pH be 5; Concentrate, filter, drying is also pulverized under 90 ℃; Is the mixed of 5:1 with dry quick lime powder according to mass ratio with the powdery product that makes, and is added dropwise to the water of weight for 2 times in this mixture while stir again, stirs into pasty state; Placing thermostatic drying chamber, is 60 ℃ of reaction 30h down 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 is that 1:100 slowly adds the positive silicic acid propyl ester of neutral inorganic precursor under vigorous stirring by mass ratio, continues to stir 4h; Dry the back under the Separation of Solid and Liquid, room temperature under air atmosphere, be warming up to 600 ℃ with 3 ℃/min speed, 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, the pressed powder that obtains being adsorbed with phosphoric acid is subsequent use.The clam shell clean is removed impurity with running water, and the oven dry back is with being milled into powder, is the amount mixing by solid-liquid mass ratio 1:5 of 12% acetic acid with this powder and concentration, reacts 6 h 25 ℃ of following constant-temperature shaking; After vibration finishes, get supernatant, with before the gained powder that is adsorbed with phosphoric acid be soaked in this supernatant by solid-liquid mass ratio 1:20, stir 2h, filter back 105 ℃ of oven dry, promptly obtain being used for the material of treatment of dyeing wastewater.Handle anionic dye Orange II with this material, when the dyestuff initial concentration was 350 mg/L, clearance was up to 95.8%.
Embodiment 4
With concentration is that 30% hydrochloric acid adds particle diameter in 70 orders and water content are 14% bentonite slurry, and hydrochloric acid and bentonite consumption are that every gram bentonite (dry weight) adds 2 mmol hydrochloric acid, fully stirring; Process mud, use steam digestion 5h again, whenever stirred once therebetween at a distance from 15 minutes; Through wash to pH be 4; Concentrate, filter, drying is also pulverized under 90 ℃; Powdery product that makes and the dry quick lime powder mass ratio according to 4:1 are 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 reaction 40h down 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 by slow neutral inorganic precursor butyl silicate, the lasting 3h that stirs of adding under vigorous stirring of mass ratio 1:130; Separation of Solid and Liquid is dried the back under air atmosphere under the room temperature again, is warming up to 700 ℃ with 4 ℃/min speed, 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, the powder that obtains being adsorbed with phosphoric acid is subsequent use.The clam shell clean is removed impurity with running water, and the oven dry back is with being milled into powder, is that 14% acetic acid is by solid-liquid mass ratio 1 with this powder and concentration
:8 amount is mixed, at 25 ℃ of following constant-temperature shaking reaction 5h; After vibration finishes, get supernatant, the supernatant main component is a calcium acetate, with before the gained powder that is adsorbed with phosphoric acid be soaked in this supernatant by solid-liquid mass ratio 1:25, stir 2h, filter back 105 ℃ of oven dry, promptly obtain being used for the material of treatment of dyeing wastewater.Handle 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 preparation methods 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 stirs; Process mud, use steam digestion 5 ~ 6h again, whenever stirred once therebetween at a distance from 15 minutes; Wash to pH be 4 ~ 5, concentrate, filter; 80 ℃ ~ 110 ℃ dry down and pulverizing, make powdery product;
2) be the mixed of 1:0.05 ~ 0.5 with the powdery product that makes by mass ratio with dry quick lime powder; Be added dropwise to the water of weight while stirring again, stir into pasty state, place thermostatic drying chamber for 2 ~ 2.5 times in this mixture; In temperature is 50 ~ 65 ℃ of reaction 24h ~ 48h down; 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 is that 1:50 ~ 1:150 slowly adds neutral inorganic precursor under vigorous stirring by mass ratio; Continue to stir 3 ~ 4h, said neutral inorganic precursor is a kind of in methyl silicate, ethyl orthosilicate, positive silicic acid propyl ester, the butyl silicate;
5) dry the back under the Separation of Solid and Liquid, room temperature and under air atmosphere, be warming up to 500 ℃ ~ 750 ℃ with 2 ℃/min ~ 5 ℃/min speed, 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 being adsorbed with the powder of phosphoric acid;
7) the clam shell clean is removed impurity with running water, the oven dry back is with being milled into powder, is that 10% ~ 15% acetic acid is pressed solid-liquid mass ratio 1 with this powder and concentration
:The amount of 3 ~ 1:10 is mixed, at 25 ℃ of following constant-temperature shaking reaction 5 ~ 6 h;
8) after vibration finishes, getting supernatant, is that 1:10 ~ 1:30 adds in this supernatant with the powder that is adsorbed with phosphoric acid of step 6) gained by the solid-liquid mass ratio, stirs 2 ~ 3 h, filters back 105 ℃ of oven dry and gets final product.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
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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 |
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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 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
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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 |