CN108821402A - A kind of preparation method of cation collagen flocculant - Google Patents
A kind of preparation method of cation collagen flocculant Download PDFInfo
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- CN108821402A CN108821402A CN201810525786.7A CN201810525786A CN108821402A CN 108821402 A CN108821402 A CN 108821402A CN 201810525786 A CN201810525786 A CN 201810525786A CN 108821402 A CN108821402 A CN 108821402A
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- flocculant
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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
- C02F1/5263—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
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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
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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
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of preparation methods of cationic collagen flocculant, using hides waste collagen albumen, acrylamide, acrylyl oxy-ethyl-trimethyl salmiac as raw material, and introduce chitosan/lignocellulosic/Nano composite material of montmorillonite, cause aqueous solution polymerization reaction by tert-butyl hydroperoxide, sodium pyrosulfite redox initiation system, synthesizes a kind of cationic collagen flocculant.Flocculant stable chemical performance prepared by the present invention, flocculation ability is good, at low cost, realizes the resource utilization of tanning waste, reduces tanning production pollutant emission, plays the role of " with pollution treatment of giving up ", and environmentally protective without secondary pollution, is easy to be degraded by microorganisms.
Description
Technical field
The present invention relates to a kind of flocculants, and in particular to a kind of flocculant of water process.
Background technique
Flocculation sedimentation plays very important effect in sewage disposal process, is suitable for papermaking, pharmacy, cosmetics, food
The wastewater treatments such as product, mineral processing, textile industry.Pollutant in waste water is usually electronegative, traditional neutral flocculant
Ideal treatment effect cannot be reached, cationic flocculant can solve this problem according to charging neutrality.However, some synthesis
Cationic polymer is expensive, and especially molecular mass is low, them is made to be difficult to transport, store and utilize as flocculant.Therefore,
High molecule mass cationic biopolymers flocculant can not only overcome traditional cationic polymer synthetic molecules quality low
The shortcomings that, and the biopolymer as environmentally friendly flocculant, it is universal nontoxic, biodegradable in nature and
It is from a wealth of sources, thus more and more concerns are caused in contemporary industry, ring is had more compared with inorganic and organic flocculant
Protect potentiality.
As leather industry big country, Animal Skin is resourceful in China, but the raw material in leather making process usually only less than 30%
Skin is changed into salable resultant Leather, remaining is used as waste to abandon mostly, generates 1,400,000 tons of leather solid wastes every year
Object.
In these wastes in addition to a small amount of non-collagen, 80% or more is made of collagen.Collagen
Contain amino, carboxyl, hydroxyl isoreactivity group on molecule, it, can be with acrylamide under initiator effect（AM）And acryloyl-oxy
Ethyl-trimethyl salmiac（DAC）Graft copolymerization generates strong cation collagen flocculant.Due to oil field waste suspended particulates
It is mostly negatively charged, the flocculation treatment of oil field waste will be used for based on collagen-modified cationic collagen flocculant, it can
Play the role of solving the problems, such as " secondary pollution " " with pollution treatment of giving up ", having broad application prospects.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of cationic collagen flocculant, waddings prepared by the present invention
Solidifying agent stable chemical performance, flocculation ability is good, at low cost, realizes the resource utilization of tanning waste, reduces tanning production
Pollutant emission is played the role of " with pollution treatment of giving up ", and environmentally protective without secondary pollution, is easy to be degraded by microorganisms.
A kind of preparation method of cation collagen flocculant, it is characterised in that this approach includes the following steps:
1）60 parts by weight hides waste collagen albumens are added in reaction kettle, 20 times of collagen quality of deionized water is added,
60 DEG C are warming up to, the concentrated sulfuric acid of collagen quality 1% is added, gradually instilling mass concentration after magnetic agitation reaction 60min is
Mixed solution pH value is adjusted to 7 by 20% sodium hydrate aqueous solution, spare；
2）By 60 ~ 100 parts by weight propylene amides, 20 ~ 60 parts of acrylyl oxy-ethyl-trimethyl salmiacs be dissolved in 180 parts by weight go from
It in sub- water, is transferred in reaction kettle after magnetic agitation 1h, then by above-mentioned steps 1）Obtained in solution be slowly added into reaction kettle
In, ultrasonic disperse 5min is warming up to 45 DEG C, vacuumizes, inflated with nitrogen displacement 30min, by 0.3 part of initiator（N tert-butyl hydroperoxide
Hydrogen:Sodium pyrosulfite=2 n:1）Wiring solution-forming is slowly alternately added in reaction kettle, and time for adding 0.5h is protected after being added dropwise
Temperature reaction 3h, adds 32 parts by weight chitosans/lignocellulosic/Nano composite material of montmorillonite and 30min is sufficiently stirred, react
After use acetone precipitation product, ethyl alcohol washs 3 ~ 5 times repeatedly, then dries to constant under temperature 60 C to get cation
Collagen flocculant.
Beneficial effect：The present invention provides a kind of preparation method of cationic collagen flocculant, with process hides waste collagen egg
White is raw material, realizes the resource utilization of tanning waste, reduces tanning production pollutant emission, plays and makees " with pollution treatment of giving up "
With；Using acrylamide, acrylyl oxy-ethyl-trimethyl salmiac as monomer, make collagen hydrolysate through graft copolymerization and sun
Ionization Modification improves its flocculation ability.In addition, cation collagen flocculant prepared by the present invention is environmentally protective, it is easy to
It is degraded by microorganisms.
Specific embodiment
Embodiment 1
1）60 parts by weight hides waste collagen albumens are added in reaction kettle, 20 times of collagen quality of deionized water is added,
60 DEG C are warming up to, the concentrated sulfuric acid of collagen quality 1% is added, gradually instilling mass concentration after magnetic agitation reaction 60min is
Mixed solution pH value is adjusted to 7 by 20% sodium hydrate aqueous solution, spare；
2）70 parts by weight propylene amides, 50 parts of acrylyl oxy-ethyl-trimethyl salmiacs are dissolved in 180 parts by weight of deionized water,
It is transferred in reaction kettle after magnetic agitation 1h, then by above-mentioned steps 1）Obtained in solution be slowly added into reaction kettle, ultrasound
Disperse 5min, is warming up to 45 DEG C, vacuumizes, inflated with nitrogen displacement 30min, by 0.3 part of initiator（N tert-butyl hydroperoxide:N is burnt
Sodium sulfite=2:1）Wiring solution-forming is slowly alternately added in reaction kettle, and rear insulation reaction is added dropwise in time for adding 0.5h
3h adds 32 parts by weight chitosans/lignocellulosic/Nano composite material of montmorillonite and 30min is sufficiently stirred, after reaction
With acetone precipitation product, ethyl alcohol is washed 3 ~ 5 times repeatedly, is then dried to constant under temperature 60 C to get cationic collagen egg
White flocculant.
Above-mentioned chitosan/lignocellulosic/Nano composite material of montmorillonite preparation method is as follows：
It weighs 6 parts by weight chitosans to be dissolved in the aqueous acetic acid that 150 parts by weight volume fractions are 1%, it is wooden that 4 parts by weight is added
Cellulose, it is 9 that the sodium hydroxide solution for being slowly added to mass fraction 20%, which adjusts solution ph, is added after magnetic agitation 30min
The aqueous acetic acid that volume fraction is 1% makes the pH value 7 of solution, forms it into unit for uniform suspension；By 8 parts by weight montmorillonites and
200 parts by weight distilled water are added in reaction kettle, are slowly added to above-mentioned suspension after stirring 0.5h with 500r/min, are warming up to 60
DEG C, water bath with thermostatic control is stirred to react 6h under nitrogen atmosphere, neutrality is washed to distillation after centrifuge separation, 140 under microwave dissolver
Ground 200 mesh after DEG C microwave treatment 2h, 105 DEG C of vacuum drying 5h, obtains chitosan/lignocellulosic/montmorillonite-based nano
Composite material.
Embodiment 2
Identical with embodiment 1, difference is：60 parts by weight propylene amides, 60 parts of acrylyl oxy-ethyl-trimethyl chlorine are added
Change ammonium.
Embodiment 3
Identical with embodiment 1, difference is：65 parts by weight propylene amides, 55 parts of acrylyl oxy-ethyl-trimethyl chlorine are added
Change ammonium.
Embodiment 4
Identical with embodiment 1, difference is：75 parts by weight propylene amides, 45 parts of acrylyl oxy-ethyl-trimethyl chlorine are added
Change ammonium.
Embodiment 5
Identical with embodiment 1, difference is：80 parts by weight propylene amides, 40 parts of acrylyl oxy-ethyl-trimethyl chlorine are added
Change ammonium.
Embodiment 6
Identical with embodiment 1, difference is：85 parts by weight propylene amides, 35 parts of acrylyl oxy-ethyl-trimethyl chlorine are added
Change ammonium.
Embodiment 7
Identical with embodiment 1, difference is：90 parts by weight propylene amides, 30 parts of acrylyl oxy-ethyl-trimethyl chlorine are added
Change ammonium.
Embodiment 8
Identical with embodiment 1, difference is：95 parts by weight propylene amides, 25 parts of acrylyl oxy-ethyl-trimethyl chlorine are added
Change ammonium.
Embodiment 9
Identical with embodiment 1, difference is：100 parts by weight propylene amides, 20 parts of acrylyl oxy-ethyl-trimethyl chlorine are added
Change ammonium.
Comparative example 1
Identical with embodiment 1, difference is：Chitosan/wooden is added without when preparing the cation collagen flocculant
Cellulose/Nano composite material of montmorillonite.
Comparative example 2
Identical with embodiment 1, difference is：Be added when preparing the cation collagen flocculant be not chitosan/
Lignocellulosic/Nano composite material of montmorillonite but common montmorillonite.
Comparative example 3
Identical with embodiment 1, difference is：It is not added when preparing chitosan/lignocellulosic/Nano composite material of montmorillonite
Enter aqueous acetic acid.
Comparative example 4
Identical with embodiment 1, difference is：Be added when preparing the cation collagen flocculant be not chitosan/
Lignocellulosic/Nano composite material of montmorillonite but lignocellulosic/Nano composite material of montmorillonite.
Comparative example 5
Identical with embodiment 1, difference is：Be added when preparing the cation collagen flocculant be not chitosan/
Lignocellulosic/Nano composite material of montmorillonite but Chitosan/Montmorillonite Hybrid Nanocomposite.
Comparative example 6
Identical with embodiment 1, difference is：The concentrated sulfuric acid is added without when preparing the cation collagen flocculant.
Comparative example 7
Identical with embodiment 1, difference is：Methylacryoyloxyethyl when preparing the cation collagen flocculant
Trimethyl ammonium chloride replaces acrylyl oxy-ethyl-trimethyl salmiac.
Comparative example 8
Identical with embodiment 1, difference is：With the tertiary fourth of initiator amount n when preparing the cation collagen flocculant
Base hydrogen peroxide:Sodium pyrosulfite=1 n:1.
Comparative example 9
Identical with embodiment 1, difference is：It is water-soluble that sodium hydroxide is added without when preparing the cation collagen flocculant
Liquid.
The cationic collagen flocculant prepared as follows to the embodiment of the present invention 1 ~ 9 and comparative example 1 ~ 9 carries out
Performance test：
Cationic collagen flocculant performance test
Flocculating experiment is carried out to Liaohe Oil Field drilling well oily waste water using freshly prepd cationic collagen flocculant.It takes
100ml turbidity is 510NTU drilling well oily waste water, adds the 0.5mg cation collagen flocculant, first low whipping speed is
2min, then low whipping speed are stirred under the conditions of 300r/min fastly to stir 5min slowly under the conditions of 80r/min, quiet heavy 30min after coagulation takes
Supernatant liquor measures turbidity and Zeta potential, and turbidity removal rate is used to test the flocculating property of product for measurement index, calculates turbid
Degree removal rate formula is as follows, and test result see the table below.
Cationic collagen flocculant the performance test results
As embodiment 1 ~ 9 it can be found that when in the proportion environment at embodiment 1, cation collagen flocculation obtained
Agent turbidity removal rate highest, reaches 98.7%, but cationic collagen flocculant turbidity removal rate prepared by embodiment 2 ~ 9
Be not it is especially desirable, turbidity removal rate 85% hereinafter, embodiment 1 match under the cationic collagen flocculant for preparing
Turbidity removal rate is out of sight, the possible reason is under the weight ratio, with acrylamide, acrylyl oxy-ethyl-trimethyl chlorination
Ammonium is that monomer prepares cationic collagen flocculant graft copolymerization rate height, and cation modifying effect is best, improves its absorption
Bridge formation ability, thus flocculating property greatly improves.In addition comparative example 1 ~ 5 illustrates that chitosan/lignocellulosic/montmorillonite-based nano is multiple
The addition of condensation material is affected to flocculant flocculating property, and comparative example 5 ~ 9 illustrates to prepare the cation collagen flocculant
The selection of raw material and condition has prominent influence to flocculant performance.
Claims (6)
1. a kind of preparation method of cation collagen flocculant, it is characterised in that this approach includes the following steps:
1）60 parts by weight hides waste collagen albumens are added in reaction kettle, 20 times of collagen quality of deionized water is added,
60 DEG C are warming up to, the concentrated sulfuric acid of collagen quality 1% is added, gradually instilling mass concentration after magnetic agitation reaction 60min is
Mixed solution pH value is adjusted to 7 by 20% sodium hydrate aqueous solution, spare；
2）By 60 ~ 100 parts by weight propylene amides, 20 ~ 60 parts of acrylyl oxy-ethyl-trimethyl salmiacs be dissolved in 180 parts by weight go from
It in sub- water, is transferred in reaction kettle after magnetic agitation 1h, then by above-mentioned steps 1）Obtained in solution be slowly added into reaction kettle
In, ultrasonic disperse 5min is warming up to 45 DEG C, vacuumizes, inflated with nitrogen displacement 30min, by 0.3 part of initiator wiring solution-forming, slowly
It is alternately added in reaction kettle, time for adding 0.5h, rear insulation reaction 3h is added dropwise, add 32 parts by weight chitosans/wood
30min is sufficiently stirred in matter cellulose/Nano composite material of montmorillonite, uses acetone precipitation product after reaction, and ethyl alcohol is washed repeatedly
It washs 3 ~ 5 times, then dries to constant under temperature 60 C to get cationic collagen flocculant.
2. a kind of preparation method of cationic collagen flocculant according to claim 1, it is characterised in that step 1）In
Magnetic agitation speed is 500r/min, step 2）Middle stirring rate is 300 ~ 400r/min.
3. a kind of preparation method of cationic collagen flocculant according to claim 1, it is characterised in that step 2）In
Ultrasonic disperse power is 350w.
4. a kind of preparation method of cationic collagen flocculant according to claim 1, it is characterised in that step 2）In
Reaction kettle is ceramic electric heating reaction kettle.
5. a kind of preparation method of cationic collagen flocculant according to claim 1, it is characterised in that step 2）In
Initiator amount ratio is n tert-butyl hydroperoxide:Sodium pyrosulfite=2 n:1.
6. a kind of preparation method of cationic collagen flocculant according to claim 1, it is characterised in that step 2）In
Chitosan/lignocellulosic/Nano composite material of montmorillonite the preparation method is as follows：
It weighs 6 parts by weight chitosans to be dissolved in the aqueous acetic acid that 150 parts by weight volume fractions are 1%, it is wooden that 4 parts by weight is added
Cellulose, it is 9 that the sodium hydroxide solution for being slowly added to mass fraction 20%, which adjusts solution ph, is added after magnetic agitation 30min
The aqueous acetic acid that volume fraction is 1% makes the pH value 7 of solution, forms it into unit for uniform suspension；By 8 parts by weight montmorillonites and
200 parts by weight distilled water are added in reaction kettle, are slowly added to above-mentioned suspension after stirring 0.5h with 500r/min, are warming up to 60
DEG C, water bath with thermostatic control is stirred to react 6h under nitrogen atmosphere, neutrality is washed to distillation after centrifuge separation, 140 under microwave dissolver
Ground 200 mesh after DEG C microwave treatment 2h, 105 DEG C of vacuum drying 5h, obtains chitosan/lignocellulosic/montmorillonite-based nano
Composite material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113512299A (en) * | 2021-05-19 | 2021-10-19 | 广西荣昇新材料有限公司 | Preparation method of lignin/chitosan/montmorillonite composite material |
| CN113912194A (en) * | 2021-11-23 | 2022-01-11 | 重庆工商大学 | Modified microbial flocculant and application thereof in slowing down membrane pollution |
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Cited By (2)
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