CN101053824A - Method for embedding lead ion poly (m-phenylene diamine) adsorbent - Google Patents
Method for embedding lead ion poly (m-phenylene diamine) adsorbent Download PDFInfo
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- CN101053824A CN101053824A CN 200710037913 CN200710037913A CN101053824A CN 101053824 A CN101053824 A CN 101053824A CN 200710037913 CN200710037913 CN 200710037913 CN 200710037913 A CN200710037913 A CN 200710037913A CN 101053824 A CN101053824 A CN 101053824A
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Abstract
The invention relates to a waste water treatment art, especially relates to an embedding method for poly(m-phenylenediamine) as a lead iron sorbent to embed the poly(m-phenylenediamine) powder into a ball by cross linking reacting of polyvinyl alcohol as an embedding medium and boracic acid as a cross linker. The method of the invention with simple operation and low cost has fine mechanical property and adsorption property of the embedded ball, which is capable of continuously operating in an adsorption condition.
Description
Technical field
The invention belongs to the technology for treating industrial waste water field, be specifically related to the embedding method of adsorbent for heavy metal poly m-phenylene diamine.
Background technology
Lead ion itself has sizable toxicity as a kind of heavy metal ion, will cause very big harm to environment if will contain the direct discharging of waste liquid of lead ion, therefore need handle the waste liquid of discharging.This seminar adopts the synthetic poly m-phenylene diamine of chemical oxidative polymerization that lead ion is had good adsorption performance (Mei-Rong Huang, Qian-Yun Peng, Xin-Gui Li.Rapid and Effective Adsorption of Lead Ions on Fine PolyphenylenediamineMicroparticles.Chemistry, A European Journal, 2006,12,4341-4350.Huang Meirong, cloud use of Pb ion absorbent of polyphenylene diamine before the Li upstart, Peng, publication number: CN1840235).But, the nascent polymer that generates has inconvenience because originally as Powdered, directly using.Therefore, be necessary its embedding is become the above particle of millimeter level, so that Separation of Solid and Liquid makes it have real practical application potentiality in the Industrial Wastewater Treatment field.
Embedding medium commonly used has sodium alginate, polyvinyl alcohol, polyacrylamide, gelatin, carragheen etc.Wherein polyvinyl alcohol is a kind of novel fixation support, have intensity height, good, the antimicrobial capacity of decomposition of chemical stability strong, to series of advantages such as microorganism are nontoxic, cheap, be a kind of embedded material with practical potentiality.At home and abroad obtained in recent years than extensive studies.Yet at present polyvinyl alcohol is used for immobilization embedded to microorganism and cell more, and the embedding of adsorbent for heavy metal is seen in the also few of report, and because the physical barrier of embedding medium, the adsorption capacity of adsorbent descends greatly after the embedding.For example, polyvinyl alcohol embedding adsorbents for lead ion pyrolytic streptomyces rimosus such as Zhang Li, compare with the streptomyces rimosus of not embedding, adsorbent after the embedding has descended 47.1% to the lead ion saturated extent of adsorption, lost nearly half adsorption capacity (Zhang Li, Tong Mingrong, Yu Yaoting. the polyvinyl alcohol embedding streptomyces rimosus is to Pb in the water
2+The research of absorption property.Ion-exchange and absorption, 2000,16 (6): 534-539).On the contrary, during polyvinyl alcohol embedding organic substance adsorbent, because the sorption effect of itself, adsorption capacity will rise to some extent, for example, usefulness polyvinyl alcohol such as Zhang Lingyan are that embedding medium, BAS are the spherical adsorbent of montmorillonite of crosslinking agent embedding, clearance to low-concentration ammonia-nitrogen waste water can reach 68.3%, it only is 60.0% Powdered montmorillonite adsorbent (Zhang Lingyan that effect is better than adsorption rate, Yu Jia, Lin Xiuling. Preparation of Montmorillonite Granule Adsorbent [J]. urban environment and urban ecology, 2006,19 (6): 24-25).
The present invention is an embedding medium with the polyvinyl alcohol, is crosslinking agent with boric acid, with adsorbents for lead ion pyrolytic poly (m-phenylenediamine) powder embedding balling-up, is significant in the application of water treatment field for the exploitation poly m-phenylene diamine.Correlative study does not appear in the newspapers.
Summary of the invention
Purpose of the present invention just provides a kind of embedding method of operating adsorbents for lead ion pyrolytic polyphenyl diamines simple and easy, with low cost.
Poly m-phenylene diamine be prepared as prior art, adopt chemical oxidative polymerization polymerization in aqueous medium to prepare the poly m-phenylene diamine powder.
The embedding method of the adsorbents for lead ion pyrolytic poly (m-phenylenediamine) that the present invention proposes is that concrete steps are as follows by embedding medium polyvinyl alcohol and crosslinking agent boric acid cross-linking reaction embedding poly m-phenylene diamine powder:
Polyvinyl alcohol is dissolved in the 80-100 ℃ of hot water, is 2 according to poly m-phenylene diamine and polyvinyl alcohol: 1-1: 2 weight proportion, in above-mentioned poly-vinyl alcohol solution, add the poly m-phenylene diamine powder, and stir; Add sodium alginate again, stir; Should mix the liquid syringe of packing into and dropwise be extruded into bead, splash in the saturated BAS that contains 1-3wt% calcium chloride cross-linking reaction, 18-30 hour, take out bead, with the boric acid and the calcium chloride of distilled water flush away surface attachment, dry the adsorbent poly m-phenylene diamine bead of polyvinyl alcohol embedding.
Poly m-phenylene diamine adds the balling property that sodium alginate can improve polyvinyl alcohol effectively during by the embedding balling-up, plays the effect that prevents adhesion.But too much sodium alginate can be separated out in the follow-up use of embedding bead, causes bead to disintegrate.The consumption of sodium alginate is 0.1～0.4wt% of adsorbent and embedding medium, and preferable amount is 0.2wt%.
Poly m-phenylene diamine by the embedding balling-up after, the mechanical property of bead and lead ion absorption property all change with the embedding process condition.Among the present invention, the concentration of polyvinyl alcohol is 6%--10%, and preferable amount is 8%; The weight ratio of poly m-phenylene diamine and polyvinyl alcohol is 1: 2-2: 1, and preferable amount is 1/1; Cross-linking reaction time is 18 hours-30 hours, and the preferred time is 24 hours.The particle diameter of bead is 2-6mm.
Among the present invention, additive calcium carbonate can increase the permeability of polyvinyl alcohol gel particle, and then increases the lead ion absorption property, can also improve the intensity and the physical property of bead in addition.Calcium carbonate is joined respectively in the mixed liquor of adsorbent poly m-phenylene diamine and embedding medium polyvinyl alcohol among the present invention, or add in the borate cross-linking agent saturated solution.The addition of calcium carbonate is the 1-3wt% of mixed liquor or boric acid saturated solution.
In the said method, before mixed liquor is extruded into bead, also can carry out ultrasonic processing, time 5-25 minute, make mixture more even mixed liquor.
The breakage rate of poly m-phenylene diamine powder sorbent embedding bead of the present invention, adopt following method to measure:
Accurately take by weighing 0.10g adsorbent bead and be put in the 50mL distilled water, in 30 ℃ water bath with thermostatic control, stir 24h, filter, take out and weigh after intact bead dries naturally, calculate breakage rate according to the weight change before and after handling.Get its mean value by twice parallel laboratory test.
The method of adsorbent of poly m-phenylene diamine bead adsorpting lead ion of the present invention adopts static adsorptive method, and concrete steps are as follows:
To contain 25mL-100mL concentration be 492.7mgL than taking by weighing the adsorbent bead that contains the 50mg poly m-phenylene diamine, placing according to embedding
-1The conical flask of lead nitrate solution in, at 20-40 ℃ of following stirring and adsorbing 1-30 hour, filter, with compleximetry (when plumbum ion concentration greater than 20mg.L
-1The time) or the inductive coupling plasma method (when plumbum ion concentration less than 20mg.L
-1The time) measure remaining Pb in the filtrate
2+Concentration C '.Calculate adsorbents adsorb capacity Q (mg g respectively according to formula (1) and (2)
-1) and clearance q (%).
Beneficial effect of the present invention: the m-phenylene diamine (MPD) low price is the raw material of industry of dyestuff, medicine and coatings industry, and price is 2～30,000 yuan/ton, and is with low cost by its synthetic adsorbent.Utilize polyvinyl alcohol-boric acid embedding poly m-phenylene diamine to become the adsorbent bead, operation is simple, with low cost.Bead satisfactory mechanical property after the embedding, bead intensity can satisfy the continued operation under the adsorption conditions, and the embedding bead absorption property of poly m-phenylene diamine is still good.Take all factors into consideration cost of material, cost of manufacture and absorption property, adsorbent of poly m-phenylene diamine embedding bead has very big potential actual application value.
The specific embodiment
Embodiment 1
0.08mol (8.652g) monomer m-phenylene diamine (MPD) is dissolved in the 200mL distilled water, ultrasonic 3～5 minutes, impel it fully to dissolve, then monomer solution is placed 30 ℃ of water-baths, balance half an hour.The oxidant ammonium persulfate of 0.08mol (18.256g) is dissolved in the 100mL distilled water, also it is maintained 30 ℃.This ammonium persulfate solution is added in the above-mentioned monomer solution.Reacted 24 hours, suction filtration, and with distilled water wash products in funnel, until using BaCl
2Solution check sulfate radical-free ion.Drain after cleaning, product was descended dry 3 days at 50 ℃, obtain poly m-phenylene diamine, productive rate 80.6%.
Embodiment 2
The 4g polyvinyl alcohol is dissolved in 90 ℃ of left and right sides hot water of 46mL, after waiting to dissolve it is cooled to about 40 ℃, be mixed with the poly-vinyl alcohol solution that weight concentration is 8wt%.Measure this poly-vinyl alcohol solution of 10mL to the 200mL beaker, add 0.8g poly m-phenylene diamine powder, add the 0.0016g sodium alginate after stirring again, stirring also with glass bar again, ultrasonic processing impelled the three to mix about 20 minutes.This mixed liquid is transferred in the syringe of 10mL, it dropwise is extruded into the bead of the about 2mm of particle diameter, splash in the saturated BAS that contains 1.5wt% calcium chloride under 30 ℃.And under this temperature, keep cross-linking reaction and carried out 24 hours.Take out bead, the boric acid of usefulness distilled water flush away surface attachment and calcium chloride etc. dry naturally, get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, and bead is not too even, and the adhesion tendency is arranged, and yield is 80%.
Repeat aforesaid operations, but use the 0.0033g sodium alginate instead, get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, bead is smooth evenly, no adhesion tendency, and yield is 96%.
Repeat aforesaid operations, but use the 0.0050g sodium alginate instead, get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, bead is even, no adhesion tendency, and yield is 96%.
Repeat aforesaid operations, but use the 0.0067g sodium alginate instead, get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, bead does not have the adhesion tendency, but in use is easy to disintegrate, and yield is 96%.
Therefore, consider that from embedding cost and the effect that will reach it is that 0.2wt% carries out that following embodiment all selects sodium alginate concentration for use.
Embodiment 3
The 5g polyvinyl alcohol is dissolved in 90 ℃ of left and right sides hot water of 45mL, after waiting to dissolve it is cooled to about 40 ℃, be mixed with the poly-vinyl alcohol solution that weight concentration is 10wt%.Measure this poly-vinyl alcohol solution of 10mL to the 100mL beaker, add 1g poly m-phenylene diamine powder, making the embedding ratio is 1: 1, adds the 0.0041g sodium alginate after stirring again, stirring also with glass bar again, ultrasonic processing impelled the three to mix about 20 minutes.This mixed liquid is transferred in the syringe of 10mL, it dropwise is extruded into the bead that particle diameter is about 5mm, splash in the saturated BAS that contains 2wt% calcium chloride under 30 ℃.And under this temperature, keep cross-linking reaction and carried out 30 hours.Take out bead, the boric acid of usefulness distilled water flush away surface attachment and calcium chloride etc. dry naturally, get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, and mixed in such cases liquid balling property is better, and gained bead intensity height, bead breakage rate only are 9.9%.Is 492.7mgL with this bead to concentration
-1Lead ion solution carry out static adsorption operations, adsorption capacity is 99.1mg/g, adsorption rate is 40.2%.
Repeat aforesaid operations, but use 0.5g poly m-phenylene diamine powder instead, making the embedding ratio is 1: 2, and cross-linking reaction was carried out 18 hours.Get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, mixed in such cases liquid balling property is better, and bead intensity height, bead breakage rate only are 10.0%.Is 492.7mgL with this bead to concentration
-1Lead ion solution carry out static adsorption operations, adsorption capacity is 91.7mg/g, adsorption rate is 37.2%.
Repeat aforesaid operations, but use 2g poly m-phenylene diamine powder instead, making the embedding ratio is 2: 1, and cross-linking reaction was carried out 24 hours.Get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, mixed in such cases liquid balling property is better, and bead intensity is higher, and the bead breakage rate is 14.2%.Is 492.7mgL with this bead to concentration
-1Lead ion solution carry out static adsorption operations, adsorption capacity is 120.3mg/g, adsorption rate is 48.8%.
Embodiment 4
The 4g polyvinyl alcohol is dissolved in 90 ℃ of left and right sides hot water of 46mL, after waiting to dissolve it is cooled to about 40 ℃, be mixed with the poly-vinyl alcohol solution that weight concentration is 8wt%.Measure this poly-vinyl alcohol solution of 10mL to the 100mL beaker, add 0.8g poly m-phenylene diamine powder, making the embedding ratio is 1: 1, adds the 0.0033g sodium alginate after stirring again, stirring also with glass bar again, ultrasonic processing impelled the three to mix about 20 minutes.This mixed liquid is transferred in the syringe of 10mL, it dropwise is extruded into the bead that particle diameter is about 3mm, splash in the saturated BAS that contains 2wt% calcium chloride under 30 ℃.And under this temperature, keep cross-linking reaction and carried out 24 hours.Take out bead, the boric acid of usefulness distilled water flush away surface attachment and calcium chloride etc. dry naturally, get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, and mixed in such cases liquid balling property is good, and gained bead intensity is higher, and the bead breakage rate only is 9.6%.Is 492.7mgL with this bead to concentration
-1Lead ion solution carry out static adsorption operations, adsorption capacity is 129.1mg/g, adsorption rate is 52.4%.
Repeat aforesaid operations, but use 0.4g poly m-phenylene diamine powder instead, making the embedding ratio is 1: 2, and cross-linking reaction was carried out 30 hours.Get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, mixed in such cases liquid balling property is good, and bead intensity is higher, and the bead breakage rate only is 9.3%.Is 492.7mgL with this bead to concentration
-1Lead ion solution carry out static adsorption operations, adsorption capacity is 87.5mg/g, adsorption rate is 35.5%.
Repeat aforesaid operations, but use 1.6g poly m-phenylene diamine powder instead, making the embedding ratio is 2: 1, and cross-linking reaction was carried out 18 hours.Get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, mixed in such cases liquid balling property is better, but bead intensity is relatively poor, and the bead breakage rate is 15.5%.Is 492.7mgL with this bead to concentration
-1Lead ion solution carry out static adsorption operations, adsorption capacity is 120.1mg/g, adsorption rate is 48.8%.
Embodiment 5
The 3g polyvinyl alcohol is dissolved in 90 ℃ of left and right sides hot water of 47mL, after waiting to dissolve it is cooled to about 40 ℃, be mixed with the poly-vinyl alcohol solution that weight concentration is 6wt%.Measure this poly-vinyl alcohol solution of 10mL to the 100mL beaker, add 0.6g poly m-phenylene diamine powder, making the embedding ratio is 1: 1, adds the 0.0025g sodium alginate after stirring again, stirring also with glass bar again, ultrasonic processing impelled the three to mix about 20 minutes.This mixed liquid is transferred in the syringe of 10mL, it dropwise is extruded into the bead that particle diameter is about 5mm, splash in the saturated BAS that contains 2wt% calcium chloride under 30 ℃.And under this temperature, keep cross-linking reaction and carried out 18 hours.Take out bead, the boric acid of usefulness distilled water flush away surface attachment and calcium chloride etc. dry naturally, get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, and mixed in such cases liquid balling property is relatively poor, and bead intensity is relatively poor, and the bead breakage rate is 23.4%.Is 492.7mgL with this bead to concentration
-1Lead ion solution carry out static adsorption operations, adsorption capacity is 113.4mg/g, adsorption rate is 46.0%.
Repeat aforesaid operations, but use 0.3g poly m-phenylene diamine powder instead, making the embedding ratio is 1: 2, and cross-linking reaction was carried out 24 hours.Get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, mixed in such cases liquid balling property is relatively poor, and bead intensity is relatively poor, and the bead breakage rate is 12.2%.Is 492.7mgL with this bead to concentration
-1Lead ion solution carry out static adsorption operations, adsorption capacity is 99.1mg/g, adsorption rate is 40.2%.
Repeat aforesaid operations, but use 1.2g poly m-phenylene diamine powder instead, making the embedding ratio is 2: 1, and cross-linking reaction was carried out 30 hours.Get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, mixed in such cases liquid balling property is relatively poor, and bead intensity difference, bead breakage rate are 18.4%.Is 492.7mgL with this bead to concentration
-1Lead ion solution carry out static adsorption operations, adsorption capacity is 104.6mg/g, adsorption rate is 42.5%.
Embodiment 6
The 4g polyvinyl alcohol is dissolved in 90 ℃ of left and right sides hot water of 46mL, after waiting to dissolve it is cooled to about 40 ℃, be mixed with the poly-vinyl alcohol solution that weight concentration is 8wt%.Measure this poly-vinyl alcohol solution of 10mL to the 100mL beaker, add 0.8g poly m-phenylene diamine powder, making the embedding ratio is 1: 1, adds 0.0043g sodium alginate and 0.033g calcium carbonate after stirring again, stirring also with glass bar again, ultrasonic processing impelled blend to mix about 20 minutes.This mixed liquid is transferred in the syringe of 10mL, it dropwise is extruded into the bead that particle diameter is about 5mm, splash in the saturated BAS that contains 2wt% calcium chloride under 30 ℃.And under this temperature, keep cross-linking reaction and carried out 24 hours.Take out bead, the boric acid of usefulness distilled water flush away surface attachment and calcium chloride etc. dry naturally, get the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, mixed in such cases liquid balling property is better, gained bead intensity height, hardness is big, and the bead breakage rate only is 7.2%.Is 492.7mgL with this bead to concentration
-1Lead ion solution carry out static adsorption operations, adsorption capacity is 152.2mg/g, adsorption rate is 61.8%.
Repeat aforesaid operations, but 2g calcium carbonate joins in the saturated BAS, the adsorbent of poly m-phenylene diamine bead of polyvinyl alcohol embedding, mixed in such cases liquid balling property is good, bead intensity height, hardness is big, the bead breakage rate is 9.1%.Is 492.7mgL with this bead to concentration
-1Lead ion solution carry out static adsorption operations, adsorption capacity is 203.2mg/g, adsorption rate is 82.5%.
By above embodiment as seen, by polyvinyl alcohol embedding method embedding polyphenyl diamines powder, make coccoid adsorbent, embedding method is simple, and is with low cost.Bead satisfactory mechanical property after the embedding, bead intensity can satisfy the continued operation under the adsorption conditions, and the embedding bead absorption property of poly m-phenylene diamine is still good.Take all factors into consideration cost of material, cost of manufacture and absorption property, adsorbent of poly m-phenylene diamine embedding bead has very big potential actual application value.
Claims (3)
1, a kind of embedding method of adsorbents for lead ion pyrolytic poly (m-phenylenediamine) is characterized in that it being that concrete steps are as follows by embedding medium polyvinyl alcohol and crosslinking agent boric acid cross-linking reaction embedding poly m-phenylene diamine powder:
Polyvinyl alcohol is dissolved in the 80-100 ℃ of hot water, is 2 according to poly m-phenylene diamine and polyvinyl alcohol: 1-1: 2 weight proportion, in above-mentioned poly-vinyl alcohol solution, add the poly m-phenylene diamine powder, and stir; Add sodium alginate again, stir; Should mix the liquid syringe of packing into and dropwise be extruded into bead, splash in the saturated BAS that contains 1-3wt% calcium chloride, cross-linking reaction 18-30 hour, take out bead, with the boric acid and the calcium chloride of distilled water flush away surface attachment, dry the adsorbent poly m-phenylene diamine bead of polyvinyl alcohol embedding.
2, the embedding method of adsorbents for lead ion pyrolytic poly (m-phenylenediamine) according to claim 1, the concentration that it is characterized in that described polyvinyl alcohol is 6%-10%.
3, adsorbents for lead ion pyrolytic poly (m-phenylenediamine) according to claim 1 embedding method, it is characterized in that mixed liquor is carried out ultrasonic processing 15-25 minute before being extruded into bead.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103193315A (en) * | 2013-04-12 | 2013-07-10 | 北京工业大学 | Method for preparing bioactive filler through immobilization of anaerobic ammonia oxidizing bacterium |
| CN104190382A (en) * | 2014-08-11 | 2014-12-10 | 湖北师范学院 | Preparation method and application of PVA supported ionic liquid adsorbing material |
| CN105366816A (en) * | 2015-11-05 | 2016-03-02 | 中国科学院广州地球化学研究所 | Slow-release type fulvic acid material and preparation method thereof |
| CN109589780A (en) * | 2019-01-03 | 2019-04-09 | 广州供电局有限公司 | Hydrogen fluoride gas adsorbent and preparation method thereof |
-
2007
- 2007-03-08 CN CN 200710037913 patent/CN101053824A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103193315A (en) * | 2013-04-12 | 2013-07-10 | 北京工业大学 | Method for preparing bioactive filler through immobilization of anaerobic ammonia oxidizing bacterium |
| CN103193315B (en) * | 2013-04-12 | 2014-05-07 | 北京工业大学 | Method for preparing bioactive filler through immobilization of anaerobic ammonia oxidizing bacterium |
| CN104190382A (en) * | 2014-08-11 | 2014-12-10 | 湖北师范学院 | Preparation method and application of PVA supported ionic liquid adsorbing material |
| CN105366816A (en) * | 2015-11-05 | 2016-03-02 | 中国科学院广州地球化学研究所 | Slow-release type fulvic acid material and preparation method thereof |
| CN109589780A (en) * | 2019-01-03 | 2019-04-09 | 广州供电局有限公司 | Hydrogen fluoride gas adsorbent and preparation method thereof |
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