CN103964557B - A kind of method utilizing paper mill sludge to prepare positively charged ion organic floculant - Google Patents
A kind of method utilizing paper mill sludge to prepare positively charged ion organic floculant Download PDFInfo
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Abstract
The present invention relates to a kind of method utilizing paper mill sludge to prepare positively charged ion organic floculant, comprise and raw material is directly dissolved with alkali lye, centrifugation goes out supernatant liquor, regulator solution pH, is placed in reactor and under being heated to certain temperature, add Potassium Persulfate, disodium ethylene diamine tetraacetate, logical nitrogen, stir-activating certain hour, then in reactor, add acrylamide and dimethyl diallyl ammonium chloride solution, continue logical nitrogen, stirring reaction; Then pour in acetone, reaction product is separated out, filter residue vacuum-drying, obtains flocculant product.When gained flocculation agent is for the treatment of simulated water sample, dosage is at 2mg/l, UV
254clearance reaches about 85%, DOC clearance and reaches about 70%.Present invention process is simple, and equipment requirements is low, is beneficial to industrial production application, not only achieves the recycling of paper making waste, and the flocculant product environment-protecting asepsis of preparation, and efficiency is high, reduces the cost of water treatment.
Description
Technical field
The present invention relates to and utilize the mud produced in alkali paper-making process to be main raw material, synthesize a kind of method of cation high molecular organic floculant, belong to changing waste into resources and utilize and water treatment flocculant technical field.
Technical background
Along with the violent growth of China's population and the sustainable development of industrial or agricultural, the demand of water resources increases day by day.The water source, many places of China is subject to pollution in various degree simultaneously, and this also exacerbates the contradiction of shortage of water resources further.Water resources has become one of important factor of restriction our people's standard of living and Economic development.
After water resource pollution problem occurs, the method for multiple waste water control is also arisen at the historic moment, and experienced by a fast-developing process.Chemical coagulation process has economy, the advantage such as efficient, easy, has become one of method extensively used in waste water treatment.The performance quality adding flocculation agent is the key factor determining coagulating treatment effect.The main direction of studying of relevant chemical Coagulation Method concentrates on exploitation that is novel, efficient, cheap, environmental protection flocculant both at home and abroad at present, and this also has very important actual application value to improving China's water quality.
Paper mill sludge is one of main waste of paper industry generation, there is complicated component, water ratio be high, output is large, intractability high, therefore to its follow-up important factor be manipulated so to limit paper industry development, also bring huge pressure to environment simultaneously.Domesticly generally select burning, the mode of landfill processes, but easily cause secondary pollution, aggravation environmental problem.Therefore, people, according to the composition of paper mill sludge, are constantly devoted to carry out recycling to it.
The recycling of current paper mill sludge mainly prepares gac, produce organic fertilizer, material of construction, chemical dispersant etc., Chinese patent document CN102205964A, CN102249745A, CN102503361A and CN1614142A individually disclose and utilize paper mill sludge to prepare the technical schemes such as gac, fertilizer, brick material, but about utilize paper mill sludge for the report of Material synthesis flocculation agent less, and the coagulation mechanism of product is confined to adsorption bridging effect.Through retrieval, take paper mill sludge as the correlation technique of Material synthesis cation high molecular organic floculant, have not yet to see report.
Summary of the invention
In order to make the paper mill sludge of paper industry realize changing waste into resources, realizing the Sustainable development of paper industry, alleviating environmental stress, the invention provides a kind of paper mill sludge that utilizes and prepare the method for positively charged ion organic floculant for raw material.
Raw material explanation
The raw material that the present invention adopts is the paper mill sludge produced in dried alkali paper-making production process, wherein content of lignin 35 ~ 45wt%, and Mierocrystalline cellulose is 8 ~ 10wt%, water ratio 5 ~ 10wt%, and all the other are earth, the grains of sand and plurality of inorganic salt impurity.
Technical scheme of the present invention is as follows:
A kind of method utilizing paper mill sludge to prepare positively charged ion organic floculant, comprise and use the paper mill sludge produced in alkali paper-making production process to be raw material, described paper mill sludge content of lignin 35 ~ 45wt%, content of cellulose 8 ~ 10wt%, water ratio 5 ~ 10wt%; Step is as follows:
(1) be dissolved in deionized water by described paper mill sludge, the quality of paper mill sludge is 2 with the ratio of the volume of deionized water: (50 ~ 60) g/ml; Drip NaOH solution under stirring, control pH, 11.0 ~ 12.0, stirs 30 ~ 50min, when pH is constant 11.5 time, centrifugal, gets supernatant liquor, pours in reactor, regulates pH to be 7.0 ~ 8.0;
(2) reactor water-bath is heated to 70 DEG C ~ 80 DEG C, stir 5 ~ 10min, add Potassium Persulfate, the mass ratio of paper mill sludge and Potassium Persulfate is 2:(0.04 ~ 0.07), logical nitrogen reaction 10 ~ 15min; Add disodium ethylene diamine tetraacetate again, the mass ratio of paper mill sludge and disodium ethylene diamine tetraacetate is 2:(0.04 ~ 0.07), logical nitrogen reaction 3 ~ 5min; And then add the dimethyl diallyl ammonium chloride solution that acrylamide and concentration are 60wt%, the mass ratio of paper mill sludge and acrylamide is 2:(1.5 ~ 3.0), the quality of paper mill sludge is 2:(6 ~ 10 with the ratio of the volume of dimethyl diallyl ammonium chloride solution) g/ml, after logical nitrogen 3 ~ 5min, stirring reaction 3 ~ 4h, temperature of reaction 70 DEG C ~ 80 DEG C;
(3) after reaction terminates, be cooled to room temperature, add acetone evolution reaction product, filter, get filter residue vacuum-drying, obtain product.
According to the present invention, preferably, described in step (1), get supernatant liquor, pour in reactor, regulate pH to be 7.5.
According to the present invention, preferably, the mass ratio of the paper mill sludge described in step (2) and Potassium Persulfate is 2:0.05;
Preferably, described paper mill sludge and the mass ratio of disodium ethylene diamine tetraacetate are 2:(0.05 ~ 0.06), preferred 2:0.06 further;
Preferably, the quality of described paper mill sludge and the volume ratio of dimethyl diallyl ammonium chloride solution are 2:(7 ~ 9) g/ml, further preferred 2:8g/ml.
According to the present invention, preferably, in step (3), vacuum-drying temperature is 60 ~ 65 DEG C.
According to the present invention, preferred scheme is as follows:
1) getting paper mill sludge 2.0g adds in 50ml deionized water, and stir the lower NaOH solution dripping mass concentration 10%, control pH, 11.5, fully stirs, and with the centrifugation 15min of 8000rpm, gets supernatant liquor in reactor, regulates pH to be 7 ~ 8;
2) reactor water-bath is heated to 70 ~ 80 DEG C, logical nitrogen gas stirring 5min, adds Potassium Persulfate 40 ~ 50mg, continues stirring and Potassium Persulfate is activated, soak time 10min; Add disodium ethylene diamine tetraacetate 60 ~ 70mg, soak time 5min, add the dimethyl diallyl ammonium chloride 8 ~ 10ml of acrylamide 2.0 ~ 3.0g and 60wt%, continue logical nitrogen 5min, stirring reaction 4 ~ 5h, temperature of reaction 70 DEG C ~ 80 DEG C;
3) after reaction terminates, be cooled to room temperature, add 200ml acetone and reaction product is separated out, filter, get filter residue vacuum-drying, vacuum-drying temperature 60 C, obtains product.
Principle of the present invention:
What the present invention utilized is alkali lignin in paper mill sludge, with acrylamide and dimethyldiallylammonchloride chloride monomer under the effect of initiator, there is graft copolymerization, generate the macromole with linear structure, performance throwing out can be combined by the colloidalmaterial in water.Product prepared by the inventive method belongs to xylogen-acrylamide-dimethyl diallyl ammonium chloride flocculation agent (L-AM-N), and after measured, current potential is+20 ~ 30mV, and molecular weight is about 500kDa ~ 2000kDa.The molecular weight of this product is large, and there is wire backbone, traditional flocculant is better than to the adsorption bridging effect of small flco, zeta current potential is higher simultaneously, charge neutrality effect can be played fully, non-cationic flocculation agent is better than to the organic removal effect in water, also add the effect of removing anionic impurity simultaneously, there is the advantage that productive rate is higher, be convenient to purification, be applicable to the fields such as feedwater, wastewater treatment.
Treated humic acid-Kaolin water sample experiment test, the flocculant dosage of gained of the present invention, when about 2mg/l, just can make UV
254clearance, DOC clearance reach 85% and 70% respectively.Content specifically will be illustrated in the examples below.
Compared with prior art, excellent results of the present invention is:
1. method of the present invention reaches the effect of changing waste into resources, not only reduces the discharge of solid waste, and provides new thinking for the sound development of paper industry.
2. flocculant product flocculation efficiency of the present invention is higher, and dosage, at about 2mg/l, just can make UV
254clearance, DOC clearance reach 85% and 70% respectively.
3. flocculant product toxicological harmless of the present invention, production technique is simple, and device requirement is few, is easy to realize suitability for industrialized production.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but be not limited thereto.The raw material paper mill sludge used in embodiment produces in the alkali paper-making process of paper mill, wherein content of lignin 35 ~ 45wt%, and Mierocrystalline cellulose is 8 ~ 10wt%, water ratio 5 ~ 10wt%, and all the other are earth, the grains of sand and plurality of inorganic salt impurity.
The preparation of the positively charged ion organic floculant (L-AM-N) of the different disodium ethylene diamine tetraacetate addition of embodiment 1.
(1) take 2.0g paper mill sludge, add the NaOH solution of 60ml deionized water and 10wt%, stir, make pH be stabilized in about 11.5, in the centrifugal 15min of 8000rpm, get supernatant liquor and be placed in reactor, regulate pH to be 7.5;
(2) reactor is put into 70 DEG C of water-baths, stir 5min, adding Potassium Persulfate quality is 50mg, after logical nitrogen activation 10min, add disodium ethylene diamine tetraacetate quality and be respectively 40mg, 50mg, 60mg, 70mg, reaction 5min, add 2g acrylamide monomer, add the dimethyl diallyl ammonium chloride solution of 8ml60wt%, continue logical nitrogen 5min, at 70 DEG C, continue reaction 4h;
(3) after reaction terminates, be cooled to room temperature, add 200ml acetone, product is separated out, filter, filter residue, in 60 DEG C of vacuum-dryings, obtains four products that disodium ethylene diamine tetraacetate dosage is different.
The preparation of the positively charged ion organic floculant (L-AM-N) of the different dimethyl diallyl ammonium chloride addition of embodiment 2.
(1) take 2.0g paper mill sludge, add the NaOH solution of 60ml deionized water and 10wt%, stir, make pH be stabilized in about 11.5, in the centrifugal 15min of 8000rpm, get supernatant liquor and be placed in reactor, regulate pH to be 7.5;
(2) reactor is put into 70 DEG C of water-baths, stir 5min, adding Potassium Persulfate quality is 50mg, after logical nitrogen activation 10min, add 60mg disodium ethylene diamine tetraacetate, reaction 5min, add 2g acrylamide monomer, the volume adding the dimethyl diallyl ammonium chloride solution of 60wt% is respectively 4ml, 6ml, 8ml, 10ml, continues logical nitrogen 5min, continues reaction 4h at 70 DEG C;
(3) after reaction terminates, be cooled to room temperature, add 200ml acetone, product is separated out, filter, filter residue, in 60 DEG C of vacuum-dryings, obtains four products that dimethyl diallyl ammonium chloride dosage is different.
The preparation of the positively charged ion organic floculant (L-AM-N) of the different acrylamide addition of embodiment 3.
Described step is identical with embodiment 2, difference is that in step (2), the volume of dimethyl diallyl ammonium chloride solution is fixed as 8ml, the amount of acrylamide is respectively 1.5g, 2.0g, 2.5g, 3.0g, obtains the positively charged ion organic floculant product that acrylamide addition is different.
The preparation of the positively charged ion organic floculant (L-AM-N) of the different Potassium Persulfate addition of embodiment 4.
Described step is identical with embodiment 3, difference is that in step (2), the amount of acrylamide is fixed as 2.5g, the addition of Potassium Persulfate is respectively 40mg, 50mg, 60mg, 70mg, obtains the positively charged ion organic floculant product that Potassium Persulfate addition is different.
The preparation of positively charged ion organic floculant (L-AM-N) under embodiment 5. difference synthesis pH environment
Described step is identical with embodiment 4, difference is that in step (2), the amount of Potassium Persulfate is fixed as 50mg, in step (1), supernatant liquor pH is adjusted to 3.5,5.5,7.5,9.5 respectively, obtains the positively charged ion organic floculant product under differential responses pH environment.
The preparation of positively charged ion organic floculant (L-AM-N) under embodiment 6. differing temps
Described step is identical with embodiment 5, and difference is that in step (1), pH is fixed as 7.5, and in step (2), temperature of reaction is respectively 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, obtains the positively charged ion organic floculant product at differential responses temperature.
The preparation of embodiment 7. differential responses time positively charged ion organic floculant (L-AM-N)
Identical with described in embodiment 6, difference is that temperature of reaction is fixed as 70 DEG C in step (2), and the reaction times is respectively 2h, 3h, 4h, 5h, obtains reaction times different positively charged ion organic floculant product.
The preparation of comparative example xylogen-acrylamide flocculating agent (L-AM)
(1) take 2.0g paper mill sludge, add the NaOH solution of 60ml deionized water and 10wt%, stir, make pH be stabilized in about 11.5, in the centrifugal 15min of 8000rpm, get supernatant liquor, regulate pH to be 7.5;
(2) reactor is put into 70 DEG C of water-baths, stir 5min, adding Potassium Persulfate quality is 50mg, after logical nitrogen activation 10min, adds 2g acrylamide monomer, continues logical nitrogen 5min, continues reaction 4h at 70 DEG C;
(3), after reaction terminates, be cooled to room temperature, add 200ml acetone, product is separated out, vacuum filtration, filter residue, in 60 DEG C of vacuum-dryings, obtains xylogen-acrylamide flocculating agent (L-AM).
Application test: the preparation of humic acid-Kaolin water sample:
Humic acid storing solution: take 1.0g humic acid and 0.4g sodium hydroxide, add in the deionized water of about about 800ml, Keep agitation 0.5h, is settled to 1L, is namely made into the humic acid storing solution of 1g/L.
Aqueous suspension ofkaolin: take 5.0g kaolin, adds Keep agitation 0.5h in the deionized water of 1L, is transferred in the graduated cylinder of 1L, static 0.5h, gets top 500ml suspension liquid with for subsequent use.
The preparation of coagulation experiment humic acid-Kaolin water sample: get deionized water and tap water that volume ratio is 1:1, add above-mentioned humic acid storing solution and aqueous suspension ofkaolin wherein, make humic acid concentration be 10mg/L, turbidity is 15.0 ± 0.5NTU.
Do flocculation agent process humic acid-Kaolin water sample with product of the present invention, finally go out water treatment efficiency and represent with UV254 clearance (%) and DOC clearance (%).
Positively charged ion organic floculant (L-AM-N) product in embodiment 1-7 and the xylogen-acrylamide flocculating agent (L-AM) in comparative example are processed humic acid-Kaolin water sample, and experiment effect is as follows:
Application example 1: L-AM-N flocculation agent embodiment 1 prepared is used for the process of humic acid-Kaolin water sample, treatment effect is listed in the table below 1-1 and 1-2.
Table 1-1.UV
245clearance (%)
The clearance (%) of table 1-2.DOC
As can be seen from the above two tables, the quality of amount on product of disodium ethylene diamine tetraacetate has impact, and disodium ethylene diamine tetraacetate, as a kind of initiator, can increase the activity of hydroxyl in xylogen, thus improve the percentage of grafting of dimethyl diallyl ammonium chloride, improve the quality of product.The present invention take 60mg as optimum.
The L-AM-N flocculant product that embodiment 2 is prepared by application example 2. is used for the process of humic acid-Kaolin water sample, and treatment effect sees following table 2-1 and 2-2.
Table 2-1.UV
245clearance (%)
The clearance (%) of table 2-2.DOC
As can be seen from the above two tables, the coagulation effect of the amount energy remarkably influenced sintetics of dimethyl diallyl ammonium chloride.Dimethyl diallyl ammonium chloride, by being grafted on the hydroxyl of xylogen, reducing negative group in xylogen, introduces amine groups simultaneously, changes the electrical of product, improves the charge neutrality effect of product in actual coagulation process, affect coagulation effect.The present invention take 8ml as optimum.
Application example 3: L-AM-N flocculation agent embodiment 3 prepared is used for the process of humic acid-Kaolin water sample, treatment effect is listed in the table below 3-1 and 3-2.
Table 3-1.UV
245clearance (%)
The clearance (%) of table 3-2.DOC
As can be seen from two tables, the quality of the amount energy remarkably influenced sintetics of acrylamide, acrylamide is best with the coagulation effect of 2.5g synthetic flocculant.Acrylamide is under certain scope that adds, and the polymerization degree of product increases along with monomer mass and increases, thus improves coagulation effect.
Application example 4: L-AM-N flocculation agent embodiment 4 prepared is used for the process of humic acid-Kaolin water sample, treatment effect is listed in the table below 4-1 and 4-2.
Table 4-1.UV
245clearance (%)
The clearance (%) of table 4-2.DOC
As can be seen from the above two tables, the quality of amount on product of initiator Potassium Persulfate has impact, and the present invention take 50mg as optimum.
The L-AM-N flocculant product that embodiment 5 is prepared by application example 5. is for the treatment of humic acid-Kaolin water sample, and treatment effect sees following table 5-1 and 5-2 respectively.
Table 5-1.UV
245clearance (%)
The clearance (%) of table 5-2.DOC
Above two tables can be found out, the pH environmental influence combined coefficient of reaction soln, mild alkaline conditions (pH=7.5) is optimum reaction condition.
The L-AM-N flocculant product that embodiment 6 is prepared by application example 6. is for the treatment of humic acid-Kaolin water sample, and treatment effect is listed in the table below 6-1 and 6-2.
Table 6-1.UV
245clearance (%)
The clearance (%) of table 6-2.DOC
Too low too high the carrying out all being unfavorable for reacting of temperature of reaction as can be seen from the above two tables, the present invention is optimum with 70 DEG C.
The L-AM-N flocculation agent that embodiment 7 is prepared by application example 7. is used for the process of humic acid-Kaolin water sample, and treatment effect is listed in the table below 7-1 and 7-2.
Table 7-1.UV
245clearance (%)
The clearance (%) of table 7-2.DOC
Reaction times of the present invention should not be too short as can be seen from the above two tables, and take 4h as optimum, reaction times long quality product has decline by a small margin.
The L-AM flocculation agent that comparative example is prepared by application example 8. is used for the process of humic acid-Kaolin water sample, and treatment effect is listed in the table below 8.
Table 8
Contrast with the coagulation effluent index of L-AM, the UV of the coagulation water outlet of L-AM-N product
245, DOC clearance raise to some extent, clearance under identical dosage increases by 10 ~ 20%.Cationic flocculant L-AM-N has stronger charge neutrality effect than L-AM, and coagulation effect is more obvious.
Claims (6)
1. utilize paper mill sludge to prepare a method for positively charged ion organic floculant, comprise and use the paper mill sludge produced in alkali paper-making production process to be raw material, described paper mill sludge content of lignin 35 ~ 45wt%, content of cellulose 8 ~ 10wt%, water ratio 5 ~ 10wt%;
Step is as follows:
(1) be dissolved in deionized water by described paper mill sludge, the quality of paper mill sludge is 2 with the ratio of the volume of deionized water: (50 ~ 60) g/ml; Drip NaOH solution under stirring, control pH, 11.0 ~ 12.0, stirs 30 ~ 50min, when pH is constant 11.5 time, centrifugal, gets supernatant liquor, pours in reactor, regulates pH to be 7.0 ~ 8.0;
(2) reactor water-bath is heated to 70 DEG C ~ 80 DEG C, stir 5 ~ 10min, add Potassium Persulfate, the mass ratio of paper mill sludge and Potassium Persulfate is 2:(0.04 ~ 0.07), logical nitrogen reaction 10 ~ 15min; Add disodium ethylene diamine tetraacetate again, the mass ratio of paper mill sludge and disodium ethylene diamine tetraacetate is 2:(0.04 ~ 0.07), logical nitrogen reaction 3 ~ 5min; And then add the dimethyl diallyl ammonium chloride solution that acrylamide and concentration are 60wt%, the mass ratio of paper mill sludge and acrylamide is 2:(1.5 ~ 3.0), the quality of paper mill sludge is 2:(6 ~ 10 with the ratio of the volume of dimethyl diallyl ammonium chloride solution) g/ml, after logical nitrogen 3 ~ 5min, stirring reaction 3 ~ 4h, temperature of reaction 70 DEG C ~ 80 DEG C;
(3) after reaction terminates, be cooled to room temperature, add acetone evolution reaction product, filter, get filter residue vacuum-drying, obtain product.
2. the method utilizing paper mill sludge to prepare positively charged ion organic floculant according to claim 1, is characterized in that, gets supernatant liquor described in step (1), pours in reactor, regulates pH to be 7.5.
3. the method utilizing paper mill sludge to prepare positively charged ion organic floculant according to claim 1, is characterized in that, the mass ratio of the paper mill sludge described in step (2) and Potassium Persulfate is 2:0.05.
4. the method utilizing paper mill sludge to prepare positively charged ion organic floculant according to claim 1, is characterized in that, in step (2), the mass ratio of paper mill sludge and disodium ethylene diamine tetraacetate is 2:(0.05 ~ 0.06).
5. the method utilizing paper mill sludge to prepare positively charged ion organic floculant according to claim 1, is characterized in that, the quality of the paper mill sludge described in step (2) and the volume ratio of dimethyl diallyl ammonium chloride solution are 2:(7 ~ 9) g/ml.
6. the method utilizing paper mill sludge to prepare positively charged ion organic floculant according to claim 1, is characterized in that, in step (3), vacuum-drying temperature is 60 ~ 65 DEG C.
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| CN104261651B (en) * | 2014-09-19 | 2015-12-30 | 山东瑞特精细化工有限公司 | A kind of polyacrylamide sludge dehydrating agent and preparation method thereof |
| CN104774290B (en) * | 2015-03-27 | 2017-10-10 | 南京师范大学 | A kind of pH, temperature dual sensitiveness chitosan flocculant and its preparation method and application |
| CN105001381B (en) * | 2015-07-14 | 2018-01-02 | 山东大学 | A kind of preparation method of paper mill sludge base Amphiphatic high polymer coagulant |
| CN105384231B (en) * | 2015-12-22 | 2018-06-29 | 山东大学 | A kind of polyaluminum ferric chloride-paper mill sludge based polyalcohol composite flocculation agent and preparation method thereof |
| CN109280174B (en) * | 2018-08-31 | 2020-09-22 | 华南理工大学 | Hyperbranched lignin grafted cationic polyacrylamide flocculant and preparation method thereof |
| CN109205955B (en) * | 2018-10-31 | 2021-03-19 | 浙江工业大学上虞研究院有限公司 | Method for treating ammonia nitrogen-containing wastewater by chemical precipitation method and biological method |
| CN109292941B (en) * | 2018-11-30 | 2021-09-28 | 山东大学 | Preparation method of high-grafting-rate paper mill sludge-based organic polymeric flocculant |
| CN110002563A (en) * | 2019-04-17 | 2019-07-12 | 山东大学 | A kind of preparation method of high molecular weight paper mill sludge base organic cation flocculating agent |
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