CN110002557A - A kind of preparation method of the high grafting rate paper mill sludge base Inorganic whisker water treatment agent of inorganic coagulant- - Google Patents
A kind of preparation method of the high grafting rate paper mill sludge base Inorganic whisker water treatment agent of inorganic coagulant- Download PDFInfo
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- CN110002557A CN110002557A CN201910308950.3A CN201910308950A CN110002557A CN 110002557 A CN110002557 A CN 110002557A CN 201910308950 A CN201910308950 A CN 201910308950A CN 110002557 A CN110002557 A CN 110002557A
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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
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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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
- C02F1/56—Macromolecular compounds
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- Inorganic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Treatment Of Sludge (AREA)
Abstract
The present invention relates to a kind of preparation methods of the high grafting rate paper mill sludge base Inorganic whisker water treatment agent of inorganic coagulant-, the composite water disposal agent is compounded using polymeric aluminum chlorides solution with high grafting rate paper mill sludge base flocculant solution, utilize the alkali lignin in paper mill sludge, with MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride monomer under the action of initiator, graft copolymerization occurs for functional group's (phenolic hydroxyl group) and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride on lignin, generate the macromonomer copolymer with branched structure, the obtained composite water disposal agent formation time is short and form is coarse, wadding body is big, the composite water treatment agent not only has large increase in charge density, and there has also been significantly increase for molecular weight, therefore absorption charge neutrality effect is improved in sewage treatment, and absorption can be provided It builds bridge and net catches the volume effect of sweeping, be provided with good coagulation effect.
Description
Technical field
The present invention relates to a kind of preparations of the high grafting rate paper mill sludge base Inorganic whisker water treatment agent of inorganic coagulant-
Method belongs to Environmental Chemistry water treatment agent technical field.
Background technique
Paper mill sludge is the end product of wastewater treatment in paper-making process, according to statistics, the annual emissions point in Japan and the U.S.
Great Yue Wei not be 300 and 8,000,000 tons, and in China, discharge amount reaches 30,000,000 tons/year.Since paper mill sludge water content is high, ingredient
Complexity, to increase its processing difficulty.Currently, the disposal options that most of country and area are taken are stacking method and landfill
Method, especially as this developing country, China.According to relevant report, a large amount of alkali lignin is contained in paper mill sludge, it is therefore, right
The utilization of alkali lignin is worth us to pay close attention in paper mill sludge.There are research, many for the modification of lignin and using early at present
Different types of functional group is grafted on lignin by person, prepares a series of lignin-base functional materials, and achieve certain
Achievement.However, mostly studying the lignin used is analysis level or technical grade, preparation cost is higher, constrains lignin
The application of product in the environment.Therefore, lignin is extracted from paper mill sludge, by the modified recycling of natural lignin, cost pole
It is big to reduce, there is great realistic meaning and promotional value.
Coagulation has many advantages, such as that cost input is low, environment influences small, is water and useless as a kind of conventional water treatment technology
One of top-priority technology in water process.Coagulant is the core of coagulation, directly determines the height of coagulation process efficiency, because
This, domestic and foreign scholars have carried out more research to coagulant.
Currently, common coagulant is divided into inorganic coagulant, organic coagulants and compound coagulant.Wherein composite flocculation
Agent refers to the copolymer that two or more single flocculants are formed it into a kind of macromolecular by certain chemical reaction, this
Copolymer can make up the deficiency of single flocculant in water treatment technology, play the effect of synergy complementation, have and numerous practice table
Bright, composite flocculation agent has a good flocculating property, and currently used composite flocculation agent divides inorganic-inorganic type flocculant and inorganic-
Organic type flocculant.Inorganic-inorganic flocculant is mainly the compound of aluminium salt, molysite and silicate.Inorganic-inorganic type flocculant is most
It will form eventually hydroxylated, have the form of more high polymerization degree, generate good flocculating effect.Currently used inorganic-inorganic is multiple
Closing flocculant has: polyferric silicate sulfate, polyaluminum ferric chloride, polymeric aluminum sulfate iron, polyaluminum sulfate aluminium chloride ferrum, polyphosphate iron sulfate.
Inorganic-organic composite flocculating agent, usually by inorganic flocculating agents and organic polymers such as aluminium system, iron series, iron aluminium system, polysilicates
Flocculant such as chitin, polyacrylamide, polydiene propyl poly dimethyl ammonium chloride etc. is combined.Organic flocculant is wide in variety
Sample, performance is polynary, and recombination mechanism is mainly its synergistic effect.On the one hand, inorganic flocculating agent can play the role of adsorbing charge neutrality
And make suspended particulate agglomerate and sink；On the other hand, the active group of organic flocculant can play bridging effect, grow wadding body
Become larger, net catches some colloids during sinking and tiny suspended particulate sinks together, to substantially increase flocculating effect.
Studies have shown that the flocculating effect of inorganic-organic composite flocculating agent is more preferably, but different formulations, different proportion has
There is very big difference in machine-inorganic composite flocculant flocculating effect, turbidity is still after some composite flocculation agent sewage treatments
It is very high；Turbidity of sewage removal rate is not high, and sewage treatment is not thorough；Along with the organic flocculant that current composite flocculation agent uses is big
It is mostly to use acrylamide, dimethyl diallyl ammonium chloride (DMDAAC) for monomer, the obtained generally existing molecular weight of product
Small, usually less than 1000kDa, wadding body is small, small with pollutant contact probability, at high cost, efficiency is not high enough etc. Shortcomings,
Effect is deteriorated after compounding with inorganic flocculating agent, and ideal treatment effect is not achieved.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides that a kind of high grafting rate paper mill sludge base of inorganic coagulant-is inorganic to be had
The preparation method of machine composite water disposal agent.
The present invention is achieved by the following scheme:
A kind of preparation method of the high grafting rate paper mill sludge base Inorganic whisker water treatment agent of inorganic coagulant-, including
Steps are as follows:
1) it takes the crude lignin as made from paper mill sludge to be added to the water, adjusts pH to 7.5-8.0, obtain rugose wood element liquid；
2) rugose wood element liquid is heated to 65-75 DEG C, is continually fed into high flow rate nitrogen, persistently stirs 25-35min, made thick
It is full of bubble in lignin liquid, obtains the lignin liquid full of bubble, the flow velocity that is passed through of high flow rate nitrogen is 100-500mL/
min；
3) potassium peroxydisulfate is added into the lignin liquid full of bubble and activates and react 15-25min, add ethylenediamine tetraacetic
Acetic acid disodium reacts 4-8min, and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is then added dropwise in batches, reacts 2-
6h, entire step carry out under nitrogen protection；
4) it after reaction, is cooled to room temperature, acetone evolution reaction product is added, filtering takes filter residue after Soxhlet extraction
It is dry, obtain high grafting rate paper mill sludge base organic polymer coargulator；
5) it takes sodium carbonate liquor to be added dropwise in liquor alumini chloridi, makes basicity 2.0, persistently stir 10-14h, make
Obtain polymeric aluminum chlorides solution；
6) high grafting rate paper mill sludge base organic polymer coargulator is dissolved in deionized water, it is 0.5- that concentration, which is made,
The high grafting rate paper mill sludge base organic polymer coargulator solution of 2.5g/L, by high grafting rate paper mill sludge base organic polymer
Flocculant solution is added dropwise in polymeric aluminum chlorides solution, persistently stirs 10-14h, is obtained the high grafting rate of inorganic coagulant-and is made
Paper sludge base Inorganic whisker water treatment agent.
Preferred according to the present invention, crude lignin is prepared as follows to obtain in step 1):
The paper mill sludge that water content is 5-15% is added in deionized water, the quality volume of paper mill sludge and deionized water
Than being 1: (15~30) g/mL；Stirring is lower to be added dropwise NaOH solution, and control pH stirs 30~50min 11.0~12.0, when pH perseverance
When fixed 11.5, centrifugation takes supernatant, and adjusting pH is 5.0~6.0, and centrifugation takes precipitating, is freeze-dried up to crude lignin.
It is further preferred that the concentration of NaOH solution is 0.1mol/L, centrifugal rotational speed 8000rpm, centrifugation time is
5min。
Preferred according to the present invention, in step 1), the mass volume ratio of crude lignin and deionized water is 2: (120~
160) g/mL uses concentration to adjust pH to 7.5-8.0 for the NaOH solution of 0.1mol/L, it is preferred that the pH of rugose wood element liquid is
7.8。
Preferred according to the present invention, in step 2), the flow velocity that is passed through of high flow rate nitrogen is 200-400mL/min, the most excellent
Choosing, in step 2), the flow velocity that is passed through of high flow rate nitrogen is 400mL/min.
Preferred according to the present invention, in step 2), mixing speed 50-120rpm is highly preferred, in step 2), stirs
Mixing speed is 120rpm.
It is preferred according to the present invention, in step 3), the mass ratio of the additional amount of potassium peroxydisulfate and rugose wood element for (0.02~
0.06): 2, it is preferred that the mass ratio of the additional amount of potassium peroxydisulfate and rugose wood element is 0.04:2.
It is preferred according to the present invention, in step 3), the additional amount of disodium ethylene diamine tetraacetate and the mass ratio of rugose wood element
For (0.04~0.08): 2, it is preferred that the additional amount of disodium ethylene diamine tetraacetate and the mass ratio of rugose wood element are 0.06:2.
It is preferred according to the present invention, in step 3), the mass concentration of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution
For 70~85wt%, rugose wood element and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution quality volume ratio are as follows: 2:(2~
20), unit: g/mL, it is preferred that rugose wood element and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution quality volume ratio are as follows:
2:15 unit: g/mL.
Preferred according to the present invention, in step 3), reaction temperature is 70 DEG C, and being stirred to react the time is 4h.
Preferred according to the present invention, in step 3), MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution divides 3-5 addition
In system, interval time 2-5min.
Preferred according to the present invention, in step 4), the drying is vacuum drying, and drying temperature is 50 DEG C.
Preferred according to the present invention, in step 5), the concentration of polymeric aluminum chlorides solution is 1-2g/L.
It is preferred according to the present invention, in step 6), high grafting rate paper mill sludge base organic polymer coargulator solution it is dense
Spending is 1g/L, and the mass ratio of polymeric aluminum chlorides solution and high grafting rate paper mill sludge base organic polymer coargulator solution is (20-
5): 1.
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, under the lignin pendular ring border full of bubble, improves reaction
Active degree can be such that more monomers are grafted on lignin, improve the grafting rate of lignin, make to react more abundant, pole
Big avoids side reaction, avoids the generation of homopolymer, further improves grafting rate, obtained organic flocculant molecular weight
Greatly, and there is branching backbone, molecular weight is 10000kDa~20000kDa；By the quality for adjusting aluminium chloride and sodium carbonate
Than preparing the polymeric aluminum chlorides solution of different basicities.By the liquor alumini chloridi of different basicities and high grafting rate paper mill sludge
Base flocculant solution is compounded, and the composite water disposal agent formation time is short and form is coarse is easy to salvage, composite water processing
Medicament not only has a large increase in charge density, and molecular weight is there has also been significantly increasing, therefore in sewage treatment
In improve absorption charge neutrality effect, and adsorption bridging can be provided and net catches sweeping effect of volume, be provided with good coagulation and imitate
Fruit.
Compared with prior art, excellent results of the invention are:
1, the present invention is compounded using polymeric aluminum chlorides solution with high grafting rate paper mill sludge base flocculant solution, is obtained
Composite water disposal agent form that the time is short and form is coarse, and wadding body is big, and the composite water treatment agent is not only in charge density
There is a large increase, and molecular weight is there has also been significantly increasing, therefore improves absorption charge neutrality in sewage treatment and make
With, and adsorption bridging can be provided and net catches the volume effect of sweeping, it is provided with good coagulation effect.
2, the present invention is compounded using polymeric aluminum chlorides solution with high grafting rate paper mill sludge base flocculant solution, the two
Play synergy, aluminium polychloride " is taken by charge neutrality " traction " high grafting rate paper mill sludge base flocculant progress
Bridge ", the surface for making high grafting rate paper mill sludge base flocculant be adsorbed on pollutant impurity particle are adsorbed on another pollutant again
Impurity particle surface assembles the pollutant impurity particle for being disappeared glutinous, and it is cotton-shaped to ultimately form the spongy bulk that can be easy to float
Object keeps turbidity of sewage removal rate high, and sewage treatment is thorough, under seldom additive amount, so that it may reach 98% or more coloration and go
Except rate.
3, composite water treatment agent simple production process of the invention, by-product is few, and device requirement is few, disposable to throw
Add, it is easy to operate.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but not limited to this.
Raw material used in embodiment is the paper mill sludge generated in dry alkali paper-making production process, and pH value is
6.62, content of ashes 34wt%, content of organic matter 66wt%, content of lignin 45wt%, content of cellulose are
10wt%, residue rate 62wt%.
Embodiment 1
A kind of preparation method of the high grafting rate paper mill sludge base Inorganic whisker water treatment agent of inorganic coagulant-, step
It is as follows:
1) the dry paper mill sludge of 10g is weighed, 150ml deionized water and 0.1M NaOH solution is added, stirring keeps pH steady
11.5 or so are scheduled on, is centrifuged 5min in 8000rpm；Taking supernatant to adjust pH is 5.5, is centrifuged 5min in 8000rpm, takes precipitating,
It is freeze-dried up to crude lignin；The crude lignin of 2.0g is weighed, is added in 150ml deionized water, 0.1mol/L is added dropwise
NaOH solution adjusts pH, stirs 30min, stablizes pH value of solution 7.8, then the solution is transferred in reactor；It will reaction
Device is put into 70 DEG C of water-baths, is continually fed into the high pure nitrogen of 400mL/min, is adjusted mixing speed and is 120rpm and stirs
30min；In the case where nitrogen protection, 40mg potassium peroxydisulfate is added into reactor, after priming reaction 20min, 60mg is added
Disodium ethylene diamine tetraacetate reacts 5min, the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 75wt% is added dropwise in three times
Solution 15mL, continues logical nitrogen 30min, the reaction was continued at 70 DEG C 4h；After reaction, it is cooled to room temperature, 200ml third is added
Product is precipitated in ketone, and Soxhlet extraction 72 hours, filter residue was organic high to get high grafting rate paper mill sludge base in 50 DEG C of vacuum drying
Molecular flocculant；High grafting rate paper mill sludge base organic polymer coargulator is dissolved in deionized water, being configured to concentration is 1g/
The solution for later use of L.
2) a certain amount of liquor alumini chloridi and sodium carbonate liquor are taken respectively, and liquor alumini chloridi is added dropwise to sodium carbonate liquor
In, 12h is persistently stirred, constant volume to 250ml prepares the polymeric aluminum chlorides solution that 1g/L basicity is 1.5.
3) a certain amount of 1g/L polymeric aluminum chlorides solution and 1g/L high grafting rate paper mill sludge base organic polymer coargulator are taken
High grafting rate paper mill sludge base organic polymer coargulator solution is added dropwise to polymerization chlorine by solution, mass ratio 10:1
Change in aluminum solutions, persistently stir 12h, be settled to 250ml, the high grafting rate papermaking of inorganic coagulant-for preparing concentration 1g/L is dirty
Composite water disposal agent is used to handle waste water, dosage 7.5-9.0mg/L by mud base Inorganic whisker water treatment agent.
Experimental example 1:
Changing the basicity that embodiment 1 closes liquor alumini chloridi, the basicity of polymeric aluminum chlorides solution is 1.0,1.5,2.0,
The polymeric aluminum chlorides solution of different basicities is mixed with high grafting rate paper mill sludge base organic polymer coargulator solution to be obtained respectively
To different composite water disposal agents, the charge density (μ eq/L) of these composite water disposal agents is surveyed, test result see the table below 1:
1 composite water disposal agent charge density of table (μ eq/L)
It can be seen from Table 1 that the polymeric aluminum chlorides solution and high grafting rate paper mill sludge base that basicity is 1.5 are organic high
The composite water disposal agent charge density that molecular flocculant solution is mixed to get is maximum, reaches 21200 μ eq/L.
The polymeric aluminum chlorides solution and high grafting rate paper mill sludge base organic polymer coargulator solution for being 1.5 by basicity
The composite water disposal agent being mixed to get handles disperse yellow dye wastewater and reactive blue dye wastewater, processing result respectively
It is shown in Table shown in 2, table 3.
The effect of 2 composite water disposal agent of table processing disperse yellow dye wastewater
| Dosage (mg/L) | Chroma removal rate removal rate (%) |
| 4.5 | -2.68097 |
| 6 | 69.07507 |
| 7.5 | 99.51475 |
| 9 | 99.56783 |
| 12 | 98.36423 |
| 15 | 98.07888 |
The effect of 3 composite water disposal agent of table processing reactive blue dye wastewater
| Dosage (mg/L) | Chroma removal rate removal rate (%) |
| 4.5 | 66.09626 |
| 6 | 89.06417 |
| 7.5 | 99.2246 |
| 9 | 99.27166 |
| 12 | 96.7123 |
| 15 | 94.86096 |
It can be seen that the increase of the dosage with composite water disposal agent by the effect of table 2, table 3, chroma removal rate is gone
Except rate increases, when dosage is 7.5mg/L, chroma removal rate is up to 98% or more, but with increasing, the color of dosage
There is downward trend instead in degree removal rate removal rate, thus, composite water disposal agent dosage of the invention is 7.5-9.0mg/L
Treatment effect is best.
Experimental example 2:
The basicity of polymeric aluminum chlorides solution is 1.5, changes 1 polymeric aluminum chlorides solution of embodiment and high grafting rate papermaking is dirty
The mass ratio of mud base organic polymer coargulator solution, respectively 20:1,10:1,5:1, different quality respectively obtain not than compound
Same composite water disposal agent, surveys the charge density (μ eq/L) of these composite water disposal agents, test result see the table below 4:
4 composite water disposal agent charge density of table (μ eq/L)
Different quality is obtained different composite water disposal agents and be respectively used to disperse yellow dye wastewater and work than compound
The coagulating treatment of property indigo plant dye wastewater, is as a result listed in table table 5, table 6 respectively.
The effect of 5 composite water disposal agent of table processing disperse yellow dye wastewater
| Dosage (mg/L) | 20:1 | 10:1 | 5:1 |
| 4.5 | -2.81501 | -2.68097 | -2.6455 |
| 6 | 74.57105 | 69.07507 | 87.53968 |
| 7.5 | 98.29759 | 99.51475 | 89.57672 |
| 9 | 97.30831 | 99.56783 | 86.8254 |
| 12 | 91.3807 | 98.36423 | 86.75132 |
| 15 | 90.31903 | 98.07888 | 86.14815 |
The effect of 6 composite water disposal agent of table processing reactive blue dye wastewater
| Dosage (mg/L) | 20:1 | 10:1 | 5:1 |
| 4.5 | 40.98361 | 66.09626 | 63.42246 |
| 6 | 83.79781 | 89.06417 | 88.95722 |
| 7.5 | 95.15152 | 99.2246 | 95.76471 |
| 9 | 94.87978 | 99.27166 | 93.4385 |
| 12 | 90.93989 | 96.7123 | 91.98449 |
| 15 | 89.70492 | 94.86096 | 89.99144 |
From the above processing result as it can be seen that when PAC basicity is 1.5, polymeric aluminum chlorides solution and high grafting rate papermaking are dirty
The mass ratio of mud base organic polymer coargulator solution is 10:1, and polymeric aluminum chlorides solution concentration is 1g/L, high grafting rate papermaking
Sludge base organic polymer coargulator solution concentration is 1g/L, and the composite water disposal agent charge density compounded is maximum,
Wadding body is big, and when dosage is 7.5-9.0mg/L, chroma removal rate reaches as high as 99%, in lower dosage, to dispersion
Yellow dye wastewater and reactive blue dye wastewater all have good removal effect.
Claims (10)
1. a kind of preparation method of the high grafting rate paper mill sludge base Inorganic whisker water treatment agent of inorganic coagulant-, including step
It is rapid as follows:
1) it takes the crude lignin as made from paper mill sludge to be added to the water, adjusts pH to 7.5-8.0, obtain rugose wood element liquid；
2) rugose wood element liquid is heated to 65-75 DEG C, is continually fed into high flow rate nitrogen, persistently stirs 25-35min, makes rugose wood
It is full of bubble in plain liquid, obtains the lignin liquid full of bubble, the flow velocity that is passed through of high flow rate nitrogen is 100-500mL/min；
3) potassium peroxydisulfate is added into the lignin liquid full of bubble and activates and react 15-25min, add ethylenediamine tetra-acetic acid
Disodium reacts 4-8min, and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is then added dropwise in batches, reacts 2-6h, whole
A step carries out under nitrogen protection；
4) it after reaction, being cooled to room temperature, acetone evolution reaction product is added, filtering takes filter residue dry after Soxhlet extraction,
Obtain high grafting rate paper mill sludge base organic polymer coargulator；
5) it takes sodium carbonate liquor to be added dropwise in liquor alumini chloridi, makes basicity 2.0, persistently stir 10-14h, be made poly-
Close liquor alumini chloridi；
6) high grafting rate paper mill sludge base organic polymer coargulator is dissolved in deionized water, it is 0.5-2.5g/L that concentration, which is made,
High grafting rate paper mill sludge base organic polymer coargulator solution, by high grafting rate paper mill sludge base organic polymer coargulator
Solution is added dropwise in polymeric aluminum chlorides solution, persistently stirs 10-14h, obtains the high grafting rate paper mill sludge of inorganic coagulant-
Base Inorganic whisker water treatment agent.
2. preparation method according to claim 1, which is characterized in that crude lignin is to make as follows in step 1)
It is standby to obtain:
The paper mill sludge that water content is 5-15% is added in deionized water, the mass volume ratio of paper mill sludge and deionized water is
1: (15~30) g/mL；Stirring is lower to be added dropwise NaOH solution, and control pH stirs 30~50min, when pH is constant 11.0~12.0
When 11.5, centrifugation takes supernatant, and adjusting pH is 5.0~6.0, and centrifugation takes precipitating, is freeze-dried up to crude lignin；NaOH
The concentration of solution is 0.1mol/L, centrifugal rotational speed 8000rpm, centrifugation time 5min.
3. preparation method according to claim 1, which is characterized in that the matter of crude lignin and deionized water in step 1)
Measuring volume ratio is 2: (120~160) g/mL, and concentration is used to adjust pH to 7.5-8.0 for the NaOH solution of 0.1mol/L,.
4. preparation method according to claim 1, which is characterized in that in step 2), the flow velocity that is passed through of high flow rate nitrogen is
200-400mL/min, it is preferred that the flow velocity that is passed through of high flow rate nitrogen is 400mL/min；Mixing speed is 50-120rpm.
5. preparation method according to claim 1, which is characterized in that in step 3), the additional amount of potassium peroxydisulfate and thick wood
The mass ratio of quality is (0.02~0.06): 2, it is preferred that the mass ratio of the additional amount of potassium peroxydisulfate and rugose wood element is 0.04:
2。
6. preparation method according to claim 1, which is characterized in that in step 3), the addition of disodium ethylene diamine tetraacetate
The mass ratio of amount and rugose wood element is (0.04~0.08): 2, it is preferred that the additional amount and rugose wood of disodium ethylene diamine tetraacetate
The mass ratio of element is 0.06:2.
7. preparation method according to claim 1, which is characterized in that in step 3), methylacryoyloxyethyl trimethyl
The mass concentration of ammonium chloride solution is 70~85wt%, rugose wood element and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution matter
Measure volume ratio are as follows: 2:(2~20), unit: g/mL, it is preferred that rugose wood element and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
Solution quality volume ratio are as follows: 2:15 unit: g/mL.
8. preparation method according to claim 1, which is characterized in that in step 3), reaction temperature is 70 DEG C, is stirred to react
Time is 4h；MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution divides in 3-5 addition system, interval time 2-5min.
9. preparation method according to claim 1, which is characterized in that in step 5), the concentration of polymeric aluminum chlorides solution is
1-2g/L。
10. preparation method according to claim 1, which is characterized in that in step 6), high grafting rate paper mill sludge base is organic
The concentration of flocculating polymer agent solution is 1g/L, and polymeric aluminum chlorides solution and high grafting rate paper mill sludge base organic polymer flocculate
The mass ratio of agent solution is (20-5): 1.
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| CN111547935A (en) * | 2020-04-15 | 2020-08-18 | 浙江省海洋水产研究所 | Method for purifying pond culture seawater by using micro-plastic |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105001381A (en) * | 2015-07-14 | 2015-10-28 | 山东大学 | Preparation method for papermaking sludge based amphoteric polymer flocculent |
| CN105384231A (en) * | 2015-12-22 | 2016-03-09 | 山东大学 | Polyaluminum ferric chloride-paper mill sludge based polymer composite flocculant and preparation method thereof |
| CN105565459A (en) * | 2015-12-22 | 2016-05-11 | 山东大学 | Compound flocculant with polymerization ferric chloride and amination polymers based on papermaking sludge and method for preparing compound flocculant |
| CN108299607A (en) * | 2018-01-12 | 2018-07-20 | 齐鲁工业大学 | A kind of preparation method and applications of lignin modified object |
| WO2018161164A1 (en) * | 2017-03-09 | 2018-09-13 | Fpinnovations | Process for producing cationic lignin copolymer under aqueous acid conditions |
| CN109292941A (en) * | 2018-11-30 | 2019-02-01 | 山东大学 | A kind of preparation method of high grafting rate paper mill sludge base organic polymer coargulator |
-
2019
- 2019-04-17 CN CN201910308950.3A patent/CN110002557A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105001381A (en) * | 2015-07-14 | 2015-10-28 | 山东大学 | Preparation method for papermaking sludge based amphoteric polymer flocculent |
| CN105384231A (en) * | 2015-12-22 | 2016-03-09 | 山东大学 | Polyaluminum ferric chloride-paper mill sludge based polymer composite flocculant and preparation method thereof |
| CN105565459A (en) * | 2015-12-22 | 2016-05-11 | 山东大学 | Compound flocculant with polymerization ferric chloride and amination polymers based on papermaking sludge and method for preparing compound flocculant |
| WO2018161164A1 (en) * | 2017-03-09 | 2018-09-13 | Fpinnovations | Process for producing cationic lignin copolymer under aqueous acid conditions |
| CN108299607A (en) * | 2018-01-12 | 2018-07-20 | 齐鲁工业大学 | A kind of preparation method and applications of lignin modified object |
| CN109292941A (en) * | 2018-11-30 | 2019-02-01 | 山东大学 | A kind of preparation method of high grafting rate paper mill sludge base organic polymer coargulator |
Non-Patent Citations (2)
| Title |
|---|
| AGHA HASAN等: "Flocculation of kaolin particles with cationic lignin polymers", 《SCIENTIFIC REPORTS》 * |
| KANGYING GUO等: "Evaluation of molecular weight, chain architectures and charge densities of various lignin-based flocculants for dye wastewater treatment", 《CHEMOSPHERE》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111547935A (en) * | 2020-04-15 | 2020-08-18 | 浙江省海洋水产研究所 | Method for purifying pond culture seawater by using micro-plastic |
| CN111547935B (en) * | 2020-04-15 | 2021-07-13 | 浙江省海洋水产研究所 | Method for purifying pond culture seawater by using micro-plastic |
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