CN110128592A - A kind of preparation method of the chitosan-based flocculant of hydrophobicity - Google Patents
A kind of preparation method of the chitosan-based flocculant of hydrophobicity Download PDFInfo
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- CN110128592A CN110128592A CN201910402369.8A CN201910402369A CN110128592A CN 110128592 A CN110128592 A CN 110128592A CN 201910402369 A CN201910402369 A CN 201910402369A CN 110128592 A CN110128592 A CN 110128592A
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/52—Polymerisation initiated by wave energy or particle radiation by electric discharge, e.g. voltolisation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- Hydrology & Water Resources (AREA)
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of preparation methods of the chitosan-based flocculant of hydrophobicity.In the method using chitosan, acrylamide (AM) and valencene as raw material;Chitosan, acrylamide, valencene are sequentially added in reactor, and water appropriate is added, under rapid mixing conditions, three mixes well and is completely dissolved;Reactor is placed under the low pressure microwave induced plasma of nitrogen addition and carries out plasma functionalization;Then reactor is placed in plasma reaction instrument, starts radio-frequency signal generator initiated polymerization.After electric discharge, stirring certain time obtains mixture under polymerization temperature after appropriate, by after purification of products up to the chitosan-based flocculant of hydrophobicity.It is stable reaction of the present invention, easily controllable, and it does not need that initiator is added, resulting chitosan-based flocculant dissolubility is good, products pure, due to the introducing of hydrophobic grouping, the flocculant also shows higher Hydrophobic association property, it is more advantageous to the sedimentation of wadding body in flocculation process, is a kind of efficient water treatment flocculant.
Description
Technical field
The invention belongs to flocculant technical fields, and in particular to a kind of preparation method of the chitosan-based flocculant of hydrophobicity.
Background technique
Coagulation Method is because its is simple and easy, the characteristics of economical and efficient, is widely used in water process.In coagulation experiment, rise
Main function is flocculant, and absorption charge neutrality, compression double electric layer, adsorption bridging, net are mainly played in water treatment procedure
The effects of catching obtains the pollutions such as the colloidal solid that is difficult to settle in water body and remove, heavy metal ion, natural organic matter preferably
Removal.Flocculant mainly includes inorganic flocculating agent, organic polymer coargulator, natural organic high-molecular flocculant and microorganism wadding
Solidifying agent.Wherein natural organic high-molecular flocculant is to pass through chemistry using natural polymers such as starch, cellulose, shell classes as raw material
Modified a kind of organic polymer coargulator obtained, specifically includes that starch flocculant, cellulose flocculant, sodium alginate wadding
Solidifying agent, chitosan flocculant.
Chitosan is a kind of natural macromolecular material, because it is widely distributed in nature, and have good adsorptivity,
Microbic resolvability and environment friendly have obtained relatively broad concern in field of environment engineering.But chitosan is water-soluble
Property is poor, limits its application in environmental pollution treatment.For the flocculating effect for improveing chitosan, certain side can be passed through
Method introduces other groups in chitosan molecule chain to improve its physicochemical property.Currently, the research to this aspect is less.
Chinese Patent Application No. CN201810352608.9, a kind of entitled " chitosan-based green flocculation of hydrophobicity
The preparation method of material ", disclose it is a kind of by chitosan by benzaldehyde synthetic intermediate to being protected to amino, in alkali
Under the conditions of property, using chloroacetic acid as modifying agent, carboxymethyl is introduced on the hydroxyl in chitosan, is connect by initiator of cerous sulfate
The chitosan-based green flocculation material of hydrophobicity is prepared to introduce quaternary ammonium salt group in branch dimethyl diallyl ammonium chloride
Method.It has many advantages, such as that flocculating effect is good, environmentally protective, but its preparation process is complicated, and in preparation process need to 65 ~
Be stirred reaction at 90 DEG C, high temperature may structure to chitosan flocculant and performance have an impact, the initiator of addition
Also flocculant can be caused centainly to pollute.
Chinese Patent Application No. CN201810892554.5, entitled " a kind of caused using plasma synthesizes shell
The method of glycan base flocculant " discloses one kind with chitosan, acrylamide monomer and methylacryoyloxyethyl trimethyl chlorine
Change ammonium monomer is raw material, causes the method for synthesizing chitosan-based flocculant using glow discharge electrolysis device.This method has anti-
Mild condition, less cost of power are answered, but resulting flocculant settling property is bad, it is especially desirable for leading to treatment effect not.
Summary of the invention
In view of the above shortcomings of the prior art, the present invention provides a kind of simple process, properties of product stable hydrophobic
The preparation method of the chitosan-based flocculant of property.
To achieve the goals above, The technical solution adopted by the invention is as follows:
Using chitosan, acrylamide (AM) and valencene as raw material;Successively by chitosan, acrylamide, valencene
It is added in reactor, and water appropriate is added, under rapid mixing conditions, three mixes well and is completely dissolved;By reactor
It is placed under the low pressure microwave induced plasma of nitrogen addition and carries out plasma functionalization;Then by reactor be placed in etc. from
Daughter is reacted in instrument, and radio-frequency signal generator initiated polymerization is started.After electric discharge, one timing of stirring under rear polymerization temperature appropriate
Between obtain mixture, by after purification of products up to the chitosan-based flocculant of hydrophobicity.
Specifically includes the following steps:
1) it weighs a certain amount of chitosan to be placed in pure water, first stirs to chitosan and be uniformly dispersed, then be slowly added dropwise in the reactor
Glacial acetic acid simultaneously stirs continuously and healthily;After chitosan is completely dissolved, the chitosan solution that concentration is 3.5 ~ 4% is obtained.
2) continue to stir in the ratio addition AM and valencene monomer of 3 ~ 6:1 into reactor completely molten to the two
Solution.AM: when valencene is lower than 3:1, the amount of valencene is excessive, and the water solubility of the polymer samples of preparation is very poor.Its
When ratio is higher than 6:1, autohemagglutination crosslinking easily occurs between AM monomer, valencene cannot preferably be grafted to chitosan molecule chain
On.
3) reactor is placed on the platform under microwave source, apart from quartz window 5cm.It is passed through ammonia, is induced in low pressure microwave
Plasma functionalization is carried out under plasma.When being functionalized the time lower than 40s, the functional group of introducing is seldom, and function is not achieved
Change effect.When being functionalized the time higher than 60s, it is easy to cause the rupture for introducing amino.
4) reactor is placed in the electrode center of plasma reaction instrument, starts radio-frequency signal generator under suitable electrical power
Initiated polymerization.When being lower than 100 s between upon discharging, seldom activity can be generated by cracking monomer by energy of plasma
Free radical, can not efficiently initiation grafting copolymerization.Thus cause grafting efficiency low.When between upon discharging more than 120 s, grafting
Efficiency declines instead.The reason is that the living radical for cracking monomer and generating constantly is consumed after discharge time further extends
Totally, chain tra nsfer and chain termination reaction are accelerated, meanwhile, energy of plasma is to the polymer of the polymer chain formed
Original property causes destruction, brings it about chain fracture, grafting efficiency is caused to reduce.
5) it after discharging, is stirred at rear 60 ~ 70 DEG C of polymerization temperature appropriate and obtains mixture after a certain period of time.In rear polymerization
Under temperature 60 C, monomer reactivity and free radical movement are low with diffusion rate, therefore reaction rate is low.AM molecule cannot be combined sufficiently
The active site of CTS.And when rear polymerization temperature is more than 70 DEG C, the activated centre of CTS becomes highly unstable, on chain
Amino and hydroxyl polymerizing power reduce, and polymerization reaction release heat can not disperse in time, so that chain tra nsfer occur
And chain termination, so that grafting efficiency reduces.
Wherein: chitosan, which should be ensured that be uniformly dispersed, in step 1) adds glacial acetic acid later, otherwise there is a small amount of chitosan
Powder cannot dissolve, and the mass ratio of chitosan and glacial acetic acid is 1.5 ~ 2:1.When the mass ratio of chitosan and glacial acetic acid is higher than 2:1
When, chitosan can not be completely dissolved.
The chitosan is a kind of natural macromolecular material, widely distributed in nature.Chitosan has double helix
Structure, molecular weight are differed from hundreds of thousands to millions of;It is widely distributed in nature, has good adsorptivity, hypotoxicity
And environment friendly.
The total mass fraction of chitosan, AM and valencene is 30 ~ 35% in step 2.At this point, the inherent viscosity of product
And flocculating property is optimal.Wherein the mass ratio of chitosan and the sum of AM, two kinds of monomer masses of valencene are 1:2 ~ 3.
The microwave power for the low pressure microwave induced plasma that ammonia is added in step 3) is kept down to 300W.It is being full of ammonia
Before gas, the pressure of gas chamber is less than 5pa, and after gas stablizes 3 minutes, pressure is stablized to 20Pa.
Plasma power is 40 ~ 60W in step 4).When lower than 40W, electronics and free radical quantity in plasma compared with
Few, energy is relatively low, and active group number is also less.When plasma power is higher than 60W, the ground state molecule of graft copolymerization, original
Son etc. can be dissociated gradually, and active group number gradually decreases.
Polymerization time is 24 ~ 30h after in step 5).Polymerization time is before 24 hours afterwards, remaining free radical not by
It completely consuming, grafting efficiency is also less high, and after rear polymerization time reaches 30h, the polymerization reaction between monomer has been completed,
Continue elevated temperature to have little effect grafting efficiency.
Compared to existing technology, the invention has the following advantages:
1, preparation method of the invention does not need addition initiator, and product is stablized, high production efficiency.
2, preparation method stable reaction of the present invention, easily controllable, side reaction is few, the chitosan-based flocculant of hydrophobicity obtained
Molecular weight is high, good water solubility.
3, chitosan-based flocculant produced by the present invention more has compared with having higher Hydrophobic association property for other flocculants
Conducive to the sedimentation of wadding body in flocculation process, it is used not only for the processing of heavy metal ion, oily waste water, the pH scope of application,
The water treatmenting performances such as complexing power, salt-resistance have significant reinforcement.Therefore, the chitosan-based flocculant of hydrophobicity is in practical applications
With good Social benefit and economic benefit.
Specific embodiment
Invention is further described in detail combined with specific embodiments below, in embodiment unless otherwise specified, uses
Raw material be ordinary commercial products.
Embodiment 1:
It is prepared in the following ways with hydrophobic chitosan-based flocculant:
1) it weighs a certain amount of chitosan to be placed in pure water, first stirs to chitosan and be uniformly dispersed, then be slowly added dropwise in the reactor
Glacial acetic acid simultaneously stirs continuously and healthily, and control chitosan and glacial acetic acid mass ratio are 2:1;After chitosan is completely dissolved, obtain dense
The chitosan solution that degree is 4%.
2) continue to stir in the ratio addition AM and valencene monomer of 3 ~ 6:1 into reactor completely molten to the two
Solution, control chitosan, AM and valencene three are 35% in the total mass fraction of pure water.
3) reactor is placed under the low pressure microwave induced plasma of nitrogen addition and carries out plasma functionalization.Official
It is 60s that the time, which can be changed,.
4) reactor is placed in the electrode center of plasma reaction instrument, starts radio-frequency signal generator under the electrical power of 50W
Initiated polymerization.Discharge time is 120s.
5) it after discharging, is stirred at 70 DEG C and obtains mixture for 24 hours.To get hydrophobicity after product is purified with dehydrated alcohol
Chitosan-based flocculant.
Embodiment 2:
It is prepared in the following ways with hydrophobic chitosan-based flocculant:
1) it weighs a certain amount of chitosan to be placed in pure water, first stirs to chitosan and be uniformly dispersed, then be slowly added dropwise in the reactor
Glacial acetic acid simultaneously stirs continuously and healthily, and control chitosan and glacial acetic acid mass ratio are 1.5:1;After chitosan is completely dissolved, obtain
The chitosan solution that concentration is 3.5%.
2) AM is added in the ratio of 6:1 into reactor and valencene monomer continues stirring to the two and is completely dissolved,
It is 30% that chitosan, AM and valencene three, which are controlled, in the total mass fraction of pure water.
3) reactor is placed under the low pressure microwave induced plasma of nitrogen addition and carries out plasma functionalization.Official
It is 40s that the time, which can be changed,.
4) reactor is placed in the electrode center of plasma reaction instrument, starts radio-frequency signal generator under the electrical power of 40W
Initiated polymerization.Discharge time is 100s.
5) after discharging, 30h is stirred at 60 DEG C and obtains mixture.To get hydrophobicity after product is purified with dehydrated alcohol
Chitosan-based flocculant.
Embodiment 3:
It is prepared in the following ways with hydrophobic chitosan-based flocculant:
1) it weighs a certain amount of chitosan to be placed in pure water, first stirs to chitosan and be uniformly dispersed, then be slowly added dropwise in the reactor
Glacial acetic acid simultaneously stirs continuously and healthily, and control chitosan and glacial acetic acid mass ratio are 2:1;After chitosan is completely dissolved, obtain dense
The chitosan solution that degree is 3.5%.
2) AM is added in the ratio of 6:1 into reactor and valencene monomer continues stirring to the two and is completely dissolved,
It is 30% that chitosan, AM and valencene three, which are controlled, in the total mass fraction of pure water.
3) reactor is placed under the low pressure microwave induced plasma of nitrogen addition and carries out plasma functionalization.Official
It is 40s that the time, which can be changed,.
4) reactor is placed in the electrode center of plasma reaction instrument, starts radio-frequency signal generator under the electrical power of 60W
Initiated polymerization.Discharge time is 100s.
5) it after discharging, is stirred at 70 DEG C and obtains mixture for 24 hours.To get hydrophobicity after product is purified with dehydrated alcohol
Chitosan-based flocculant.
Embodiment 4:
It is prepared in the following ways with hydrophobic chitosan-based flocculant:
1) it weighs a certain amount of chitosan to be placed in pure water, first stirs to chitosan and be uniformly dispersed, then be slowly added dropwise in the reactor
Glacial acetic acid simultaneously stirs continuously and healthily, and control chitosan and glacial acetic acid mass ratio are 1.5:1;After chitosan is completely dissolved, obtain
The chitosan solution that concentration is 4%.
2) AM is added in the ratio of 3:1 into reactor and valencene monomer continues stirring to the two and is completely dissolved,
It is 35% that chitosan, AM and valencene three, which are controlled, in the total mass fraction of pure water.
3) reactor is placed under the low pressure microwave induced plasma of nitrogen addition and carries out plasma functionalization.Official
It is 60s that the time, which can be changed,.
4) reactor is placed in the electrode center of plasma reaction instrument, starts radio-frequency signal generator under the electrical power of 60W
Initiated polymerization.Discharge time is 120s.
5) it after discharging, is stirred at 60 DEG C and obtains mixture for 24 hours.To get hydrophobicity after product is purified with dehydrated alcohol
Chitosan-based flocculant.
Embodiment 5:
It is prepared in the following ways with hydrophobic chitosan-based flocculant:
1) it weighs a certain amount of chitosan to be placed in pure water, first stirs to chitosan and be uniformly dispersed, then be slowly added dropwise in the reactor
Glacial acetic acid simultaneously stirs continuously and healthily, and control chitosan and glacial acetic acid mass ratio are 2:1;After chitosan is completely dissolved, obtain dense
The chitosan solution that degree is 3.5%.
2) AM is added in the ratio of 3:1 into reactor and valencene monomer continues stirring to the two and is completely dissolved,
It is 35% that chitosan, AM and valencene three, which are controlled, in the total mass fraction of pure water.
3) reactor is placed under the low pressure microwave induced plasma of nitrogen addition and carries out plasma functionalization.Official
It is 60s that the time, which can be changed,.
4) reactor is placed in the electrode center of plasma reaction instrument, starts radio-frequency signal generator under the electrical power of 50W
Initiated polymerization.Discharge time is 120s.
5) after discharging, 30h is stirred at 70 DEG C and obtains mixture.To get hydrophobicity after product is purified with dehydrated alcohol
Chitosan-based flocculant.
The relevant nature of the chitosan-based flocculant of hydrophobicity made from embodiment 1 ~ 5 is measured respectively, and see Table 1 for details for data.
The chitosan-based flocculant characteristic of 1 hydrophobicity of table
Product | Molecular weight (kDa) | To oily waste water removal rate (%) |
Embodiment 1 | 1903.9 | 96.3 |
Embodiment 2 | 1122.3 | 93.5 |
Embodiment 3 | 1644.6 | 95.2 |
Embodiment 4 | 795.4 | 91.4 |
Embodiment 5 | 1101.1 | 92.1 |
The resulting chitosan-based flocculating agent molecule amount of hydrophobicity of the present invention is larger it can be seen from upper table 1, for oily waste water
Treatment effect is also preferable, thus proves that the chitosan-based flocculant of the hydrophobicity is with good performance.
The above embodiment of the present invention only example to illustrate the invention, and be not to embodiment party of the invention
The restriction of formula.For those of ordinary skill in the art, many differences can also be made on the basis of the above description
The variation of form.Here all embodiments can not be exhaustive.All technical solution of the present inventions that belongs to are amplified out
Obvious changes or variations still in the scope of protection of the present invention.
Claims (7)
1. a kind of preparation method of the chitosan-based flocculant of hydrophobicity, which is characterized in that with chitosan, acrylamide (AM) and Zhu
Goldenrain tree sequiterpene is raw material;Chitosan, acrylamide, valencene are sequentially added in reactor, and water appropriate is added,
Under rapid mixing conditions, three mixes well and is completely dissolved;Reactor is placed on to the low pressure microwave induction etc. of nitrogen addition
Plasma functionalization is carried out under gas ions;Then reactor is placed in plasma reaction instrument, starting radio-frequency signal generator draws
Send out polymerization reaction.After electric discharge, stirring certain time obtains mixture under polymerization temperature after appropriate, by after purification of products to obtain the final product
The chitosan-based flocculant of hydrophobicity.
2. the preparation method of the chitosan-based flocculant of hydrophobicity according to claim 1, which is characterized in that including following step
It is rapid:
1) it weighs a certain amount of chitosan to be placed in pure water, first stirs to chitosan and be uniformly dispersed, then be slowly added dropwise in the reactor
Glacial acetic acid simultaneously stirs continuously and healthily;After chitosan is completely dissolved, the chitosan solution that concentration is 3.5 ~ 4% is obtained;
2) AM is added in the ratio of 3 ~ 6:1 into reactor and valencene monomer continues stirring to the two and is completely dissolved;
3) reactor is placed on the platform under microwave source, apart from quartz window 5cm.Be passed through ammonia, low pressure microwave induction etc. from
Plasma functionalization is carried out under daughter.The functionalized time is 40 ~ 60s.
4) reactor is placed in the electrode center of plasma reaction instrument, starts radio-frequency signal generator initiated polymerization, when reaction
Between be 100 ~ 120s.
5) after discharging, certain time is stirred under 60 ~ 70 DEG C of rear polymerization temperature and obtains mixture, will dredge to obtain the final product after purification of products
Aqueous chitosan-based flocculant.
3. the preparation method of the chitosan-based flocculant of hydrophobicity according to claim 2, which is characterized in that shell in step 1)
The mass ratio of glycan and glacial acetic acid is 1.5 ~ 2:1.
4. the preparation method of the chitosan-based flocculant of hydrophobicity according to claim 2, which is characterized in that shell in step 2
Glycan, the total mass fraction of AM and valencene three in pure water are 30 ~ 35 %, wherein chitosan and AM, grapefruit sesquialter
The mass ratio of the sum of two kinds of monomer masses of terpene is 1:2 ~ 3.
5. the preparation method of the chitosan-based flocculant of hydrophobicity according to claim 2, which is characterized in that micro- in step 3)
Wave power is kept down to 300W.Before full of ammonia, the pressure of gas chamber is less than 5pa, and after gas stablizes 3 minutes, pressure is steady
Determine to 20Pa.
6. the preparation method of the chitosan-based flocculant of hydrophobicity according to claim 2, which is characterized in that step 4) is medium
Ion power is 40 ~ 60W.
7. the preparation method of the chitosan-based flocculant of hydrophobicity according to claim 2, which is characterized in that in step 5)
Polymerization time is in 24 ~ 30h afterwards.
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Cited By (1)
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CN111662411A (en) * | 2020-07-27 | 2020-09-15 | 重庆工商大学 | Preparation method of hydrophobic acacia gum flocculant for antibiotic treatment |
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CN109021168A (en) * | 2018-08-07 | 2018-12-18 | 重庆大学 | A method of caused using plasma and synthesizes chitosan-based flocculant |
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CN102477122A (en) * | 2010-11-22 | 2012-05-30 | 袁连海 | Synthesis process for hydrophobic polymeric flocculant with controlled content of hydrophobic monomers |
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