CN110002563A - A kind of preparation method of high molecular weight paper mill sludge base organic cation flocculating agent - Google Patents
A kind of preparation method of high molecular weight paper mill sludge base organic cation flocculating agent Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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Abstract
The present invention relates to a kind of preparation methods of high molecular weight paper mill sludge base organic cation flocculating agent, this method uses the paper mill sludge generated in alkali paper-making production process for raw material, under the action of initiator potassium persulfate and disodium ethylene diamine tetraacetate, graft copolymerization occurs with MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, generate the macromonomer copolymer with branched structure, obtained product charge density is high, molecular weight is big, and there is branching backbone, Zeta potential is 50.1-63.1mV, charge density is 4500-4763 μ eq/L, molecular weight is 10000kDa~20000kDa；It is big that flocculant generates wadding body, it is bigger with the contact probability of contaminant particle, traditional flocculant is better than to the adsorption bridging effect of small wadding body, while the flocculant charge density is higher, so absorption charge neutrality ability is stronger, non-cationic flocculant is better than to the removal effect of anionic impurity in water.Have the advantages that flocculation performance is higher, is convenient for purification, is suitable for field of waste water treatment.
Description
Technical field
The present invention relates to a kind of preparation methods of high molecular weight paper mill sludge base organic cation flocculating agent, belong to solid
Waste resource recovery utilizes and technical field of water treatment chemical.
Background technique
Coagulation sedimentation is a kind of not only economic but also easy water treatment method, is widely used to domestic and international water pollution and controls
In reason, sludge dewatering and water-saving reuse purified treatment engineering field.And the performance superiority and inferiority of flocculant is to determine coagulation efficiency, technique
The key factor of operating cost and purification of water quality quality.Cationic organic polymer coargulator can pass through its positive charge
Charge neutrality effect between group and anionic contaminant group reduces the hydrophily of pollutant, and has in turn by cationic
The removal to pollutant is realized in the adsorption bridging effect of machine high polymer coagulant.
Currently, cationic organic polymer coargulator has two major classes, first is that artificial synthesized organic high molecular polymer, two
Being is new and effective organic polymer coargulator made from raw material are modified to biomass；Artificial synthesized organic polymer is poly-
Closing object includes: cationic-type polyacrylamide, polydimethyl diallyl ammonium chloride, epichlorohydrin-dimethylamine copolymer etc.,
Have dosage few in these artificial synthesized cationic organic polymer coargulator applications, agglomeration speed is fast, and wadding body is big and hard
The advantages that tough, but the monomer toxicity for Synthetical Organic Polymeric Flocculants is stronger, product difficult for biological degradation and cost
It is higher, therefore its application in water and wastewater treatment field is restricted.
In today that environmental consciousness is increasingly enhanced, since biomass organic polymer coargulator has, toxicity is low, raw material is next
The advantages such as source is wide, easily biological-degradable, price are low, are generallyd use the second class organic polymer coargulator, are especially using biomass
Agriculture and industry waste is modified the flocculant that (etherificate, esterification, sulfonation, graft copolymerization etc.) obtains, Ji Keshi as raw material
The comprehensive utilization of existing waste resource, and the preparation and application cost of flocculant can be reduced.Therefore, carry out biomass-based flocculant
Research is of great practical significance and application value.
Paper mill sludge is the end product of wastewater treatment in paper-making process, and one ton of paper of every production will generate 150kg or more
Dewatered sludge, be 5-10 times of same size municipal sewage plant.Paper mill sludge has complicated component, water content height, processing
The disadvantages of difficulty is big, disposal costs are high, therefore paper mill sludge processing disposition has become the problem of puzzlement paper industry development.Papermaking
Sewage sludge biomass rich content, wherein organic matter accounts for 50%-65%, predominantly lignin and a small amount of cellulose, hemicellulose
Element.Therefore, how paper mill sludge biomass as resources comprehensive utilization is carried out to be of great practical significance.Based on can hold
The theory of supervention exhibition, recycling sludge is ideal Disposal Measures, has not only realized the effective use of resource in sludge, but also reduce
Unreasonable processing method of disposal is endangered caused by the mankind and environment, has important theory significance and realistic meaning, pole
Has popularization and application foreground.
Currently, also about the report for being used to prepare flocculant document using paper mill sludge, be mostly using acrylamide,
Dimethyl diallyl ammonium chloride (DMDAAC) is monomer, and the obtained generally existing molecular weight of product is small, usually less than
1000kDa, wadding body is small, small with pollutant contact probability, and the deficiency of at high cost, efficiency is not high enough etc. is not able to satisfy sewage
Processing requirement, therefore, the big cationic high-molecular flocculant of research and development high molecule mass, high-cation conversion ratio, wadding body
Product has great importance to meet domestic market demand.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of high molecular weight paper mill sludge base organic cation flocculating agent
Preparation method, the flocculant charge density that the method for the present invention obtains is high, generates that wadding body is big, and molecular weight is big, and have branching long
Chain structure.
Raw material explanation
The raw material that the present invention uses is the paper mill sludge generated in dry alkali paper-making production process, and pH value is
6.62, content of ashes 30-35wt%, content of organic matter 65-70wt%, content of lignin 40-45wt%, cellulose contain
Amount is 8-12wt%, residue rate 60-65wt%.
The present invention is achieved through the following technical solutions:
A kind of preparation method of high molecular weight paper mill sludge base organic cation flocculating agent, was produced using alkali paper-making
The paper mill sludge generated in journey is made for raw material, and obtained flocculant Zeta potential is 50.1-63.1mV, and charge density is
4500-4763 μ eq/L, molecular weight are 10000kDa~20000kDa；
Preparation step is as follows:
(1) paper mill sludge is added in deionized water, the quality of paper mill sludge and the volume ratio of deionized water are as follows: 5:(150
~250), unit: g/mL adjusts pH to 12.0-13.0, is thoroughly mixed uniformly, and centrifugation takes supernatant, adjusts supernatant
PH is 7.5~8.5；
(2) supernatant after adjusting pH is heated to 65-75 DEG C, is continually fed into high flow rate nitrogen, stir 15-30min, row
Except the air in rugose wood element liquid, potassium persulfate and disodium ethylene diamine tetraacetate are added into system, it is stirred to react 10~
30min adds the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution that mass concentration is 70~85%, paper mill sludge quality
With the volume ratio of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution are as follows: 5:(2~30), unit: g/mL, it is stirred to react 2~
6h；
(3) after reaction, it is cooled to room temperature, evolution reaction product, filters, take filter residue dry after Soxhlet extraction, i.e.,
Secure satisfactory grades sub- amount paper mill sludge base organic cation flocculating agent.
Above-mentioned preparation method, it is preferred that in step (1), the water content of paper mill sludge is 5-15%, paper mill sludge and go from
The mass volume ratio of sub- water is 5: (170~200) g/mL, and concentration is used to adjust the pH of mixed liquor for the NaOH solution of 0.1mol/L
To 12.0-13.0, it is preferred that the pH of mixed liquor is 12.3.
Above-mentioned preparation method, it is preferred that concentration is used to adjust supernatant for the HCl solution of 0.1mol/L in step (1)
PH to 7.5-8.5, it is preferred that the pH of supernatant is 7.8.
Above-mentioned preparation method, it is preferred that in step (2), supernatant heating temperature is 70 DEG C, and high flow rate nitrogen is passed through flow velocity
For 300-400mL/min.
Above-mentioned preparation method, it is preferred that in step (2), the additional amount of potassium persulfate and the mass ratio of paper mill sludge are
(0.005~0.1): 5, it is preferred that the mass ratio of the additional amount of potassium persulfate and paper mill sludge is 0.05:5.
Above-mentioned preparation method, it is preferred that in step (2), the additional amount of disodium ethylene diamine tetraacetate and the matter of paper mill sludge
Amount is than being (0.005~0.1): 5, it is preferred that the mass ratio of the additional amount of disodium ethylene diamine tetraacetate and paper mill sludge is 0.05:
5。
Above-mentioned preparation method, it is preferred that in step (2), the quality of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution
Concentration is 75wt%.
Above-mentioned preparation method, it is preferred that in step (2), paper mill sludge and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
Solution quality volume ratio are as follows: 5:(20~30), unit: g/mL.
It is highly preferred, paper mill sludge and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution quality volume ratio are as follows: 5:
20, unit: g/mL.
Above-mentioned preparation method, it is preferred that in step (2), after MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is added
Reaction temperature is 70 DEG C, and being stirred to react the time is 4h.
Above-mentioned preparation method, it is preferred that in step (2), MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is in three times
It is added dropwise in system.
Above-mentioned preparation method, it is preferred that in step (3), reagent used in evolution reaction product is acetone, and dry is vacuum
Dry, drying temperature is 50 DEG C.
The application for the high molecular weight paper mill sludge base organic cation flocculating agent that above-mentioned preparation method obtains is used for waste water
Processing, dosage 5-18mg/L, it is preferred that dosage 14-18mg/L.
The principle of the present invention:
The present invention is being drawn using the alkali lignin in paper mill sludge with MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride monomer
Under the action of sending out agent, grafting occurs for functional group's (phenolic hydroxyl group) and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride on lignin altogether
Poly- reaction, generates the macromonomer copolymer with branched structure, and obtained product charge density is high, and molecular weight is big, and has branch
Change backbone, Zeta potential 50.1-63.1mV, charge density be 4500-4763 μ eq/L, molecular weight be 10000kDa~
20000kDa；Obtained flocculant generation wadding body is big, bigger with the contact probability of contaminant particle, to the adsorptive racks of small wadding body
Bridge effect is better than traditional flocculant, while the flocculant charge density is higher, so absorption charge neutrality ability is stronger, to negative in water
The removal effect of ionic impurity is better than non-cationic flocculant.Have the advantages that flocculation performance is higher, is convenient for purification, is suitable for
Field of waste water treatment.
Compared with prior art, excellent results of the invention are:
1, the present invention is existed using the alkali lignin in paper mill sludge with MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride monomer
Under the action of initiator, graft copolymerization occurs, generates the flocculant with branched structure, obtained product charge density
Height, molecular weight is big, and has branching backbone, Zeta potential 63.1mV, and charge density is 4763 μ eq/L, and molecular weight is about
10000kDa~20000kDa is, it can be achieved that efficient removal to anionic pollutant.
2, flocculant made from preparation method of the invention, wadding body partial size is big, bigger with the contact probability of contaminant particle,
Traditional flocculant is better than to the adsorption bridging effect of small wadding body, while the flocculant charge density is higher, so in absorption electricity
It is stronger with ability, non-cationic flocculant, cationic flocculant viscosity are better than to the removal effect of anionic impurity in water
High, cationic degree height, has a wide range of application.
3, the flocculant product flocculation efficiency that the present invention obtains is more preferable compared to existing lignin-base flocculant product, adds
Amount is in 20mg/l or so, so that it may reach 96% or more chroma removal rate.
4, preparation method simple production process of the invention, by-product is few, and device requirement is few, it is easy to accomplish industrial metaplasia
It produces.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but not limited to this.Raw material used in embodiment is dry
The paper mill sludge generated in dry alkali paper-making production process, pH value 6.62, content of ashes 34wt%, the content of organic matter
For 66wt%, content of lignin 45wt%, content of cellulose 10wt%, residue rate 62wt%.
The preparation of disperse yellow dye waste water is simulated in embodiment:
It weighs 0.1g disperse yellow powder to be dissolved in 1L water, stir evenly.Test the concentration of water sample, pH, Zeta potential and suction
Luminosity is respectively 100mg/L, 8.05 ± 0.02, -29.0 ± 1.0mV and 8.00 ± 0.02.
Disperse yellow dye waste water is simulated, finally water treatment efficiency is indicated out with chroma removal rate (%).
Embodiment 1.
A kind of preparation method of high molecular weight paper mill sludge base organic cation flocculating agent, comprises the following steps that
(1) the dry paper mill sludge of 5g is weighed, 170mL deionized water is added, is adjusted using 0.1mol/L NaOH solution mixed
The pH of liquid is closed, stirring stablizes pH 12.3 or so, is centrifuged 6min in 10000rpm；Take supernatant adjust pH be 7.8 to get
Lignin crude liquid.
(2) lignin crude liquid is transferred in reactor, is put into 70 DEG C of water-baths, is continually fed into high pure nitrogen, makes wood
It is full of bubble in quality crude liquid, adjusts mixing speed and is 120rpm and stirs 20min.
(4) in the case where nitrogen protection, 50mg potassium persulfate is added into reactor, after activating 20min, is added
50mg disodium ethylene diamine tetraacetate reacts 5min, the methylacryoyloxyethyl trimethyl chlorine of 75wt% is added dropwise in three times
Change ammonium salt solution 20mL, continues logical nitrogen 25min, the reaction was continued at 70 DEG C 4h；
(5) after reaction, it being cooled to room temperature, 250mL acetone is added, product is precipitated, filter residue is dried in vacuo in 50 DEG C,
Up to high molecular weight paper mill sludge base organic cation flocculating agent e, high molecular weight paper mill sludge base cationic organic-flocculation
Agent molecule amount is 7.23 × 106Da。
Experimental example 1:
Change 1 MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution of embodiment additional amount, additional amount be respectively 2mL,
5mL, 10mL, 15mL, 20mL, 30mL, respectively obtain different flocculant a1, b1, c1, d1, f1, test a1, b1, c1, d1,
The Zeta potential of e1, f1, as a result see the table below 1-1, by a1, b1, c1, d1, e1, f1 to simulation disperse yellow dye waste water with different
Dosage is handled, and processing result see the table below shown in 1-2.
Table 1-1.Zeta current potential (mV)
Table 1-2. chroma removal rate removal rate (%)
By table 1-1, table 1-2 can be seen that MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride dosage be 20mL when, wadding
The current potential of solidifying agent is maximum, and with the increase of the dosage of flocculant, chroma removal rate removal rate increases, and is 18mg/L in dosage
When chroma removal rate it is maximum but increasing with dosage, there is downward trend instead in chroma removal rate removal rate, because
And flocculant dosage of the invention be 14-18mg/L when high treating effect.
Experimental example 2:
Change 1 potassium persulfate of embodiment additional amount, additional amount be respectively 5mg, 10mg, 15mg, 20mg, 50mg,
100mg respectively obtains different flocculant a2, b2, c2, d2, f2, tests the Zeta potential of a2, b2, c2, d2, e, f2, as a result
It see the table below 2-1, a2, b2, c2, d2, e, f2 handle simulation disperse yellow dye waste water with different dosages, processing knot
Fruit see the table below shown in 2-2.
Table 2-1.Zeta current potential (mV)
Table 2-2. chroma removal rate removal rate (%)
When by table 2-1, table 2-2, to can be seen that potassium persulfate dosage be 50mg, the current potential of flocculant is maximum, with
The increase of the dosage of flocculant, chroma removal rate removal rate increase, when dosage is 18mg/L, chroma removal rate is maximum,
But increasing with dosage, there is downward trend instead in chroma removal rate removal rate, thus, flocculant of the invention
High treating effect when dosage is 14-18mg/L.
Experimental example 3:
Change 1 disodium ethylene diamine tetraacetate of embodiment additional amount, additional amount be respectively 5mg, 10mg, 15mg, 20mg,
50mg, 100mg respectively obtain different flocculant a3, b3, c3, d3, f3, test the Zeta potential of a3, b3, c3, d3, e, f3,
As a result it see the table below 3-1, a3, b3, c3, d3, e, f3 handle simulation disperse yellow dye waste water with different dosages, locate
Reason result see the table below shown in 3-2.
Table 3-1.Zeta current potential (mV)
Table 3-2. chroma removal rate removal rate (%)
By table 3-1, table 3-2 can be seen that disodium ethylene diamine tetraacetate dosage be 50mg when, the current potential of flocculant is most
Greatly, with the increase of the dosage of flocculant, chroma removal rate removal rate increases, the chroma removal rate when dosage is 18mg/L
Maximum, but it is increasing with dosage, and there is downward trend instead in chroma removal rate removal rate, thus, of the invention
High treating effect when flocculant dosage is 14-18mg/L.
Application example 4:
Change the reaction temperature of embodiment 1, temperature is respectively 50 DEG C, 60 DEG C, 80 DEG C, 90 DEG C, respectively obtains different waddings
Solidifying agent a4, b4, c4, d4, test the Zeta potential of a4, b4, c4, d4, e, as a result see the table below 4-1, by a4, b4, c4, d4, e to mould
Quasi- disperse yellow dye waste water is handled with different dosages, and processing result see the table below shown in 4-2.
Table 4-1.Zeta current potential (mV)
Table 4-2. chroma removal rate removal rate (%)
Application example 5:
The addition manner for changing the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of embodiment 1 is changed to disposably quickly add
Enter, test Zeta potential, as a result see the table below 5-1, then simulation disperse yellow dye waste water is handled with different dosages,
Processing result see the table below shown in 5-2.
Table 5-1.Zeta current potential (mV)
Table 5-2. chroma removal rate removal rate (%)
The preparation of 1 lignin of comparative example-dimethyl diallyl ammonium chloride flocculant
(1) 5.0g paper mill sludge is weighed, the NaOH solution of 170mL deionized water and 10wt% is added, stirring stablizes pH
12.0 or so, it is centrifuged 15min in 8000rpm, supernatant is taken to be placed in reactor, adjusting pH is 7.5；
(2) reactor is put into 70 DEG C of water-baths, stirs 15min, addition potassium persulfate quality is 50mg, leads to nitrogen
After activating 20min, it is respectively 50mg that disodium ethylene diamine tetraacetate quality, which is added, reacts 5min, and the diformazan of 20mL 60wt% is added
Base diallyl ammonium chloride solution, continues logical nitrogen 25min, the reaction was continued at 70 DEG C 4h；
(3) after reaction, it is cooled to room temperature, 200mL acetone is added, product is precipitated, filter, filter residue is in 60 DEG C of vacuum
Drying is to get lignin-dimethyl diallyl ammonium chloride flocculant.
Flocculant prepared by comparative example is used for the processing of dye wastewater by contrast effect, and treatment effect is listed in the table below
6。
6 chroma removal rate of table (%)
The effect of comparative example is compared with the effect of application example 1 of the present invention, can intuitively be found out by comparing,
Monomer dosage is flocculant made from 20mL, and flocculant dosage of the invention is the simulated wastewater color removal of 10mg/L
Rate is 54.8%, and the simulated wastewater chroma removal rate that the flocculant dosage of comparative example 1 is 10mg/L is 12.6%, the present invention
Flocculant dosage be 20mg/L simulated wastewater chroma removal rate be 95.1%, and the flocculant dosage of comparative example 1 is
The simulated wastewater chroma removal rate of 20mg/L is 46.8%, and under identical dosage, flocculant of the invention is to simulated wastewater
Removal rate it is higher, the flocculant charge density in the present invention is higher, has stronger charge neutrality effect, coagulation effect is brighter
Aobvious, therefore, in actual application, flocculant of the invention can be in the case where seldom dosage, and treatment effect is more preferable,
Cost is lower.
Claims (10)
1. a kind of preparation method of high molecular weight paper mill sludge base organic cation flocculating agent, using alkali paper-making production process
The paper mill sludge of middle generation is made for raw material, and obtained flocculant Zeta potential is 50.1-63.1mV, charge density 4500-
4763 μ eq/L, molecular weight are 10000kDa~20000kDa；
Preparation step is as follows:
(1) paper mill sludge is added in deionized water, the quality of paper mill sludge and the volume ratio of deionized water are as follows: 5:(150~
250), unit: g/mL adjusts pH to 12.0-13.0, is thoroughly mixed uniformly, and centrifugation takes supernatant, adjusts supernatant pH
It is 7.5~8.5；
(2) supernatant after adjusting pH is heated to 65-75 DEG C, is continually fed into high flow rate nitrogen, stir 15-30min, excluded thick
Potassium persulfate and disodium ethylene diamine tetraacetate are added into system, is stirred to react 10~30min for air in lignin liquid,
Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution that mass concentration is 70~85%, paper mill sludge quality and methyl
The volume ratio of acrylyl oxy-ethyl-trimethyl salmiac solution are as follows: 5:(2~30), unit: g/mL is stirred to react 2~6h；
(3) after reaction, it is cooled to room temperature, evolution reaction product, filters, filter residue is taken to dry after Soxhlet extraction to get height
Molecular weight paper mill sludge base organic cation flocculating agent.
2. preparation method according to claim 1, which is characterized in that the water content of paper mill sludge is 5- in step (1)
15%, the mass volume ratio of paper mill sludge and deionized water is 5: (170~200) g/m L to use concentration for 0.1mol/L's
The pH to 12.0-13.0 of NaOH solution adjusting mixed liquor.
3. preparation method according to claim 1, which is characterized in that use concentration for the HCl of 0.1mol/L in step (1)
The pH to 7.5-8.5 of solution adjusting supernatant.
4. preparation method according to claim 1, which is characterized in that in step (2), supernatant heating temperature is 70 DEG C,
It is 300-400mL/min that high flow rate nitrogen, which is passed through flow velocity,.
5. preparation method according to claim 1, which is characterized in that in step (2), the additional amount of potassium persulfate with make
The mass ratio of paper sludge is (0.005~0.1): 5, it is preferred that the additional amount of potassium persulfate and the mass ratio of paper mill sludge are
0.05:5.
6. preparation method according to claim 1, which is characterized in that in step (2), the addition of disodium ethylene diamine tetraacetate
The mass ratio of amount and paper mill sludge is (0.005~0.1): 5, it is preferred that the additional amount of disodium ethylene diamine tetraacetate and papermaking are dirty
The mass ratio of mud is 0.05:5.
7. preparation method according to claim 1, which is characterized in that in step (2), methylacryoyloxyethyl trimethyl
The mass concentration of ammonium chloride solution is 75wt%, paper mill sludge and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution quality body
Product ratio are as follows: 5:(20~30), unit: g/mL；It is highly preferred, paper mill sludge and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
Solution quality volume ratio are as follows: 5:20, unit: g/mL.
8. preparation method according to claim 1, which is characterized in that in step (2), methylacryoyloxyethyl trimethyl
Reaction temperature is 70 DEG C after ammonium chloride solution is added, and being stirred to react the time is 4h, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
Solution is added dropwise in system in three times.
9. preparation method according to claim 1, which is characterized in that in step (3), reagent used in evolution reaction product
Dry to be dried in vacuo for acetone, drying temperature is 50 DEG C.
10. the high molecular weight paper mill sludge base organic cation flocculating agent that preparation method described in claim 1 obtains is answered
With for wastewater treatment, dosage 14-18mg/L.
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| KANGYING GUO等: "Evaluation of molecular weight, chain architectures and charge densities of various lignin-based flocculants for dye wastewater treatment", 《CHEMOSPHERE》 * |
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