CN106006890A - Preparation method of chitosan coagulant - Google Patents
Preparation method of chitosan coagulant Download PDFInfo
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- CN106006890A CN106006890A CN201610510218.0A CN201610510218A CN106006890A CN 106006890 A CN106006890 A CN 106006890A CN 201610510218 A CN201610510218 A CN 201610510218A CN 106006890 A CN106006890 A CN 106006890A
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a preparation method of a chitosan coagulant. The preparation method is characterized in that the chitosan coagulant is prepared by wrapping an aluminum-iron series flocculant with a chitosan flocculant. The method comprises the following steps: firstly, preparing the aluminum-iron series flocculant; secondly, preparing the chitosan flocculant; thirdly, wrapping the aluminum-iron series flocculant with the chitosan flocculant to obtain the chitosan coagulant. The preparation method disclosed by the invention has the characteristics of high yield, relatively-low cost, good coagulation effect and the like.
Description
Technical field
The invention belongs to environment-friendly materials technical field, be specifically related to the preparation method of a kind of chitosan coagulant.
Background technology
Along with China produces the quick raising of industrialization and living standard, annual production waste water and sanitary sewage
Discharge capacity also quickly increases on the ground in progression, and efficiently and safely these black waters being carried out process is ring
Border protection and resource develop in harmony a great problem that faces, are also that numerous chemical enterprise needs break away from tired badly
One of border.
Coagulation is to apply one of most common key link in waste water treatment process, and it affects to a great extent
The operating condition of follow-up flow process, final outflow water quality and cost, thus become important in environmental project
Technological research development field.Efficient coagulation technology system should by excellent coagulant, reactor and from
Control dispensing three aspects are combined closely and are formed, and wherein coagulant plays the role of a nucleus.Coagulating treatment technology it is crucial that
Select suitable coagulant.
Using coagulant to carry out chemical coagulation and precipitation is one of effective means of processing wastewater and sewage, also
It is focus and the difficult point of current sewage treatment area research.The sorting technique of coagulant is a lot, by composition not
With, typically can be classified as inorganic coagulant, organic coagulants, natural coagulant (such as biological coagulant),
If charged character after the height according to coagulant molecular weight, the feature of functional group and functional group's dissociation,
Macromolecule, low molecule, cationic, anionic and nonionic coagulant etc. can be further divided into.
Research finds that chitosan has chelating adsorption to many materials, the amino in its molecule and and amino
Adjacent hydroxyl and many metal ions are (such as Hg2+、Ni2+、Cu2+、Pb2+、CA2+、Ag+Deng) can be formed surely
Fixed chelate, is used for administering heavy metal wastewater thereby, purification tap water and separating metal ions in hydrometallurgy
Deng.But at present chitosan processes for water environment and only has a small amount of existence in China, mainly due to yielding poorly,
High in cost of production problem.
Summary of the invention
For solving above technical problem, it is an object of the invention to provide the preparation side of a kind of chitosan coagulant
Method.It is high that the present invention has productivity, the features such as cost is relatively low, and coagulation effect is good.
For achieving the above object, the present invention provides the preparation method of a kind of chitosan coagulant, it is characterized in that adopting
Prepare with chitosan flocculant parcel ferro-aluminum based flocculating agent；The method comprises the steps:
(1) ferro-aluminum based flocculating agent is prepared；
(2) chitosan flocculant is prepared；
(3) chitosan flocculant is wrapped up ferro-aluminum based flocculating agent and obtain chitosan coagulant；
Wherein, prepare ferro-aluminum based flocculating agent, comprise the steps:
(11) sodium silicate is configured to polymeric silicicacid sodium solution；
(12) in polymeric silicicacid sodium solution, add dilute sulfuric acid, make solution ph be down to 8-10；
(13) continue to add dicyandiamide, quaternary ammonium salt and the mixed solution of iron salt in solution, control temperature at 60 DEG C
-80 DEG C of reaction a period of times；
(14) continue to add aluminum salt solution in solution, control temperature and react a period of time at 60 DEG C-80 DEG C；
(15) by solution left standstill ripening after stopped reaction, ferro-aluminum based flocculating agent is obtained.
Preferably, in described step (11), for configuring the sodium silicate of polymeric silicicacid sodium solution and the mass ratio of water
For (0.5-0.8): 100.
Preferably, in described step (12), the concentration of dilute sulfuric acid is 0.15-0.18mol/L, the addition of dilute sulfuric acid
Polymeric silicicacid sodium can be made to obtain a certain degree of activation, beneficially the carrying out of subsequent reactions, described dilute sulfuric acid
After addition, continue stirring reaction 10-30min.
Preferably, in described step (13), in the mixed solution of dicyandiamide, quaternary ammonium salt and iron salt, dicyandiamide is dense
Degree is 30-35g/L, and the concentration of quaternary ammonium salt is 3-5g/L, and in iron salt, the concentration of ferric ion is 35-40g/L,
The addition of the mixed solution of wherein said dicyandiamide, quaternary ammonium salt and iron salt is molten with polymeric silicicacid sodium in step (11)
The volume ratio of liquid is (0.3-0.5): 1, after adding the mixed solution of described dicyandiamide, quaternary ammonium salt and iron salt, instead
It is 1-1.5h between Ying Shi.
Preferably, in described step (14), in aluminum salt solution, aluminum ions concentration is 120-135g/L, adds described
After aluminum salt solution, the response time is 2-4h.
Preferably, in described step (15) after stopped reaction, ripening time of repose is 12-36h.
Preferably, one or more during described iron salt preferably includes iron chloride, iron sulfate, ferric nitrate；
Described aluminium salt preferably includes aluminum chloride, aluminum sulfate, aluminum nitrate.
Preferably, the preparation of the chitosan flocculant in above-mentioned steps (2) specifically includes following steps: collect shrimp,
Carapax Eriocheir sinensis raw material, after 2-4% acid solution Prawn, Carapax Eriocheir sinensis decalcification, deproteinization in 2-4% alkali liquor, in washing, do
Dry rear chitin extraction, deacetylated in the 45-55% alkali liquor of 140-160 DEG C, it is centrifuged, washes, does
Dry, obtain chitosan, take chitosan 100 parts with by hydroxyethyl cellulose 50 parts, calcium carbonate 20 parts, β-
The adjuvant that cyclodextrin derivative 30 parts is constituted is mix homogeneously stirring in the bottle of magnetic, stands 15-30min
After, after being heated slowly to 55-65 DEG C, after cooling 40-50min, obtain chitosan flocculant slurry.
Preferably, above-mentioned steps (3) specifically includes following steps: by baked for described ferro-aluminum based flocculating agent,
Fine grinding and mixing just make pellet ferro-aluminum based flocculating agent, at pellet ferro-aluminum based flocculating agent outer wrapping flocculate with chitosan
Agent slurry, obtains described chitosan coagulant.
Beneficial effect
(1) combine organic and inorganic flocculating agent advantage, have and make simple, with low cost, absorption wadding
Solidifying ability is strong, it is possible to form bigger flocculation floccule, and the rate of settling is high, and resistance to acids and bases is strong.
(2) nontoxic pollution-free, in water can natural decomposition, greatly reduce secondary biochemical pollution；Absorption dirt
Foreign pigment in water, to the metal ion in water such as: Hg2+、Ni2+、Cu2+、pb2+、CA2+、Ag+Deng tool
Having significantly absorption and complexing, the metal ion in the most recyclable sewage, saves resource simultaneously.
Detailed description of the invention
Embodiment one
Prepare ferro-aluminum based flocculating agent
Sodium silicate is configured to polymeric silicicacid sodium solution；For configuring sodium silicate and the water of polymeric silicicacid sodium solution
Mass ratio be 0.5: 100.
In polymeric silicicacid sodium solution, add dilute sulfuric acid, make solution ph be down to 8-10；Preferably, described dilute
The concentration of sulphuric acid is 0.15mol/L, and the addition of dilute sulfuric acid can make polymeric silicicacid sodium obtain a certain degree of activation,
Be conducive to the carrying out of subsequent reactions, after described dilute sulfuric acid adds, continue stirring reaction 10min.
Continue to add dicyandiamide, quaternary ammonium salt and the mixed solution of iron salt in solution, control temperature at 60 DEG C DEG C
Reaction a period of time；In the mixed solution of dicyandiamide, quaternary ammonium salt and iron salt, dicyandiamide concentration is 30g/L, season
The concentration of ammonium salt is 3g/L, and in iron salt, the concentration of ferric ion is 35g/L, wherein said dicyandiamide, quaternary ammonium
The addition of the mixed solution of salt and iron salt is 0.3: 1 with the volume ratio of polymeric silicicacid sodium solution, adds described
After the mixed solution of dicyandiamide, quaternary ammonium salt and iron salt, the response time is 1h.Described iron salt preferably includes chlorine
Change one or more in ferrum, iron sulfate, ferric nitrate；Described aluminium salt preferably include aluminum chloride, aluminum sulfate,
Aluminum nitrate.
Continue to add aluminum salt solution in solution, control temperature and react a period of time at 60 DEG C；In aluminum salt solution
Aluminum ions concentration is 120g/L, and after adding described aluminum salt solution, the response time is 2h.
By solution left standstill ripening after stopped reaction, ripening time of repose is 12h, obtains ferro-aluminum based flocculating agent.
Prepare chitosan flocculant
Chitosan flocculant preparation specifically includes following steps: collect shrimp, Carapax Eriocheir sinensis raw material, 2% acid solution Prawn,
After Carapax Eriocheir sinensis decalcification, deproteinization in 2% alkali liquor, washing, dried chitin extraction, 140 DEG C 45%
In alkali liquor deacetylated, it be centrifuged, wash, be dried, obtain chitosan, take chitosan 100 parts with by hydroxyl
The adjuvant that ethyl cellulose 50 parts, calcium carbonate 20 parts, beta-cyclodextrin derivative 30 parts are constituted is at the bottle of magnetic
Mix homogeneously stirring in son, after standing 15min, after being heated slowly to 55 DEG C, obtains shell after cooling 40min
Chitosan flocculant slurry.
Chitosan flocculant is wrapped up ferro-aluminum based flocculating agent and obtains chitosan coagulant
Baked for described ferro-aluminum based flocculating agent, fine grinding and mixing are just made pellet ferro-aluminum based flocculating agent, at ball
Shape ferro-aluminum based flocculating agent outer wrapping chitosan flocculant slurry, with pellet ferro-aluminum based flocculating agent completely by chitosan
Flocculant slurry parcel is preferred, and obtains described chitosan coagulant.
Embodiment two
Prepare ferro-aluminum based flocculating agent
Sodium silicate is configured to polymeric silicicacid sodium solution；For configuring sodium silicate and the water of polymeric silicicacid sodium solution
Mass ratio be 0.8: 100.
In polymeric silicicacid sodium solution, add dilute sulfuric acid, make solution ph be down to 8-10；Preferably, described dilute
The concentration of sulphuric acid is 0.18mol/L, and the addition of dilute sulfuric acid can make polymeric silicicacid sodium obtain a certain degree of activation,
Be conducive to the carrying out of subsequent reactions, after described dilute sulfuric acid adds, continue stirring reaction 30min.
Continue to add dicyandiamide, quaternary ammonium salt and the mixed solution of iron salt in solution, control temperature anti-at 80 DEG C
Answer a period of time；In the mixed solution of dicyandiamide, quaternary ammonium salt and iron salt, dicyandiamide concentration is 35g/L, season
The concentration of ammonium salt is 5g/L, and in iron salt, the concentration of ferric ion is 40g/L, wherein said dicyandiamide, quaternary ammonium
The addition of the mixed solution of salt and iron salt is 0.5: 1 with the volume ratio of polymeric silicicacid sodium solution, adds described
After the mixed solution of dicyandiamide, quaternary ammonium salt and iron salt, the response time is 1.5h.Described iron salt preferably includes
One or more in iron chloride, iron sulfate, ferric nitrate；Described aluminium salt preferably includes aluminum chloride, sulphuric acid
Aluminum, aluminum nitrate.
Continue to add aluminum salt solution in solution, control temperature and react a period of time at 80 DEG C；In aluminum salt solution
Aluminum ions concentration is 135g/L, and after adding described aluminum salt solution, the response time is 4h.
By solution left standstill ripening after stopped reaction, ripening time of repose is 36h, obtains ferro-aluminum based flocculating agent.
Prepare chitosan flocculant
Chitosan flocculant preparation in above-mentioned steps (2) specifically includes following steps: collect shrimp, Carapax Eriocheir sinensis former
Material, after 4% acid solution Prawn, Carapax Eriocheir sinensis decalcification, deproteinization in 4% alkali liquor, in washing, extracts after drying
Chitin, deacetylated in the 45-55% alkali liquor of 160 DEG C, it is centrifuged, washes, is dried, obtain shell and gather
Sugar, takes chitosan 100 parts and by hydroxyethyl cellulose 50 parts, calcium carbonate 20 parts, beta-cyclodextrin derivative
The 30 parts of adjuvant constituted mix homogeneously stirrings in the bottle of magnetic, after standing 15-30min, are heated slowly to
After 65 DEG C, after cooling 50min, obtain chitosan flocculant slurry.
Chitosan flocculant is wrapped up ferro-aluminum based flocculating agent and obtains chitosan coagulant
Baked for described ferro-aluminum based flocculating agent, fine grinding and mixing are just made pellet ferro-aluminum based flocculating agent, at ball
Shape ferro-aluminum based flocculating agent outer wrapping chitosan flocculant slurry, with pellet ferro-aluminum based flocculating agent completely by chitosan
Flocculant slurry parcel is preferred, and obtains described chitosan coagulant.
Embodiment three
Prepare ferro-aluminum based flocculating agent
Sodium silicate is configured to polymeric silicicacid sodium solution；For configuring sodium silicate and the water of polymeric silicicacid sodium solution
Mass ratio be 0.6: 100.
In polymeric silicicacid sodium solution, add dilute sulfuric acid, make solution ph be down to 8-10；Preferably, described dilute
The concentration of sulphuric acid is 0.16mol/L, and the addition of dilute sulfuric acid can make polymeric silicicacid sodium obtain a certain degree of activation,
Be conducive to the carrying out of subsequent reactions, after described dilute sulfuric acid adds, continue stirring reaction 20min.
Continue to add dicyandiamide, quaternary ammonium salt and the mixed solution of iron salt in solution, control temperature anti-at 70 DEG C
Answer a period of time；In the mixed solution of dicyandiamide, quaternary ammonium salt and iron salt, dicyandiamide concentration is 32g/L, season
The concentration of ammonium salt is 4g/L, and in iron salt, the concentration of ferric ion is 38g/L, wherein said dicyandiamide, quaternary ammonium
The addition of the mixed solution of salt and iron salt is 0.4: 1 with the volume ratio of polymeric silicicacid sodium solution, adds described
After the mixed solution of dicyandiamide, quaternary ammonium salt and iron salt, the response time is 1.2h.Described iron salt preferably includes
One or more in iron chloride, iron sulfate, ferric nitrate；Described aluminium salt preferably includes aluminum chloride, sulphuric acid
Aluminum, aluminum nitrate.
Continue to add aluminum salt solution in solution, control temperature and react a period of time at 70 DEG C；In aluminum salt solution
Aluminum ions concentration is 130g/L, and after adding described aluminum salt solution, the response time is 3h.
By solution left standstill ripening after stopped reaction, ripening time of repose is 24h, obtains ferro-aluminum based flocculating agent.
Prepare chitosan flocculant
Chitosan flocculant preparation specifically includes following steps: collect shrimp, Carapax Eriocheir sinensis raw material, 3% acid solution Prawn,
After Carapax Eriocheir sinensis decalcification, deproteinization in 3% alkali liquor, at washing, dried chitin extraction, at 140-160 DEG C
50% alkali liquor in deacetylated, it be centrifuged, wash, be dried, obtain chitosan, take chitosan 100 parts
With by hydroxyethyl cellulose 50 parts, calcium carbonate 20 parts, 30 parts of adjuvants constituted of beta-cyclodextrin derivative at magnetic
Property bottle in mix homogeneously stirring, stand after 15-30min, after being heated slowly to 60 DEG C, cool down 45min
After obtain chitosan flocculant slurry.
Chitosan flocculant is wrapped up ferro-aluminum based flocculating agent and obtains chitosan coagulant
Baked for described ferro-aluminum based flocculating agent, fine grinding and mixing are just made pellet ferro-aluminum based flocculating agent, at ball
Shape ferro-aluminum based flocculating agent outer wrapping chitosan flocculant slurry, with pellet ferro-aluminum based flocculating agent completely by chitosan
Flocculant slurry parcel is preferred, and obtains described chitosan coagulant.
Comparative example
Buy coagulant from the market.
The coagulant of specific embodiment one, two, three and market is carried out contrast test, and result is as follows:
| COD of sewage mg/L | Sewage SS mg/L | Water outlet COD clearance | Water outlet SS clearance | |
| Embodiment one | 322 | 256 | 81% | 80% |
| Embodiment two | 322 | 256 | 82% | 79% |
| Embodiment three | 322 | 256 | 80% | 82% |
| Comparative example | 322 | 256 | 61% | 63% |
By the contrast of above-mentioned data, the specific embodiment one, two, three of the present invention and the coagulation of market sale
Agent product contrasts, the COD clearance of the present invention therein, SS clearance apparently higher than existing product,
Process to sewage is remarkably enhanced.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this
Any amendment, equivalent and the improvement etc. made within bright spirit and principle, all should be included in the present invention
Protection domain within.
Claims (9)
1. a preparation method for chitosan coagulant, is characterized in that using chitosan flocculant to wrap up ferro-aluminum system wadding
Solidifying agent prepares；The method comprises the steps:
(1) ferro-aluminum based flocculating agent is prepared；
(2) chitosan flocculant is prepared；
(3) chitosan flocculant is wrapped up ferro-aluminum based flocculating agent and obtain chitosan coagulant；
Wherein, prepare ferro-aluminum based flocculating agent, comprise the steps:
(11) sodium silicate is configured to polymeric silicicacid sodium solution；
(12) in polymeric silicicacid sodium solution, add dilute sulfuric acid, make solution ph be down to 8-10；
(13) continue to add dicyandiamide, quaternary ammonium salt and the mixed solution of iron salt in solution, control temperature at 60 DEG C
-80 DEG C of reaction a period of times；
(14) continue to add aluminum salt solution in solution, control temperature and react a period of time at 60 DEG C-80 DEG C；
(15) by solution left standstill ripening after stopped reaction, ferro-aluminum based flocculating agent is obtained.
2. the method for claim 1, it is characterised in that in described step (11), be used for configuring polymerization
The sodium silicate of sodium silicate solution and the mass ratio of water are (0.5-0.8): 100.
3. method as claimed in claim 2, it is characterised in that in described step (12), the concentration of dilute sulfuric acid
For 0.15-0.18mol/L, the addition of dilute sulfuric acid can make polymeric silicicacid sodium obtain a certain degree of activation, favorably
In the carrying out of subsequent reactions, after described dilute sulfuric acid adds, continue stirring reaction 10-30min.
4. method as claimed in claim 3, it is characterised in that in described step (13), dicyandiamide, quaternary ammonium
In the mixed solution of salt and iron salt, dicyandiamide concentration is 30-35g/L, and the concentration of quaternary ammonium salt is 3-5g/L, ferrum
In salt, the concentration of ferric ion is 35-40g/L, and the mixing of wherein said dicyandiamide, quaternary ammonium salt and iron salt is molten
The addition of liquid is (0.3-0.5) with the volume ratio of polymeric silicicacid sodium solution in step (11): 1, adds described pair of cyanogen
After the mixed solution of amine, quaternary ammonium salt and iron salt, the response time is 1-1.5h.
5. method as claimed in claim 4, it is characterised in that in described step (14) in aluminum salt solution aluminum from
The concentration of son is 120-135g/L, and after adding described aluminum salt solution, the response time is 2-4h.
6. method as claimed in claim 5, it is characterised in that in described step (15) after stopped reaction, ripe
Change time of repose is 12-36h.
7. method as claimed in claim 6, it is characterised in that described iron salt include iron chloride, iron sulfate,
One or more in ferric nitrate；Described aluminium salt includes aluminum chloride, aluminum sulfate, aluminum nitrate.
8. method as claimed in claim 7, it is characterised in that the flocculate with chitosan in above-mentioned steps (2)
Agent preparation specifically includes following steps: collect shrimp, Carapax Eriocheir sinensis raw material, after 2-4% acid solution Prawn, Carapax Eriocheir sinensis decalcification,
Deproteinization in 2-4% alkali liquor, at washing, dried chitin extraction, at the 45-55% alkali of 140-160 DEG C
In liquid deacetylated, it be centrifuged, wash, be dried, obtain chitosan, take chitosan 100 parts with by hydroxyl second
The adjuvant that base cellulose 50 parts, calcium carbonate 20 parts, beta-cyclodextrin derivative 30 parts are constituted is at the bottle of magnetic
Middle mix homogeneously stirs, after standing 15-30min, after being heated slowly to 55-65 DEG C, after cooling 40-50min
Obtain chitosan flocculant slurry.
9. method as claimed in claim 8, it is characterised in that specifically include as follows in above-mentioned steps (3)
Step: pellet ferro-aluminum based flocculating agent is just made in baked for described ferro-aluminum based flocculating agent, fine grinding and mixing,
Pellet ferro-aluminum based flocculating agent outer wrapping chitosan flocculant slurry, obtains described chitosan coagulant.
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| CN106904709A (en) * | 2017-03-27 | 2017-06-30 | 山东钢铁集团日照有限公司 | A kind of method for preparing hollow ball flocculant |
| CN108191019A (en) * | 2018-01-12 | 2018-06-22 | 常州华禹环保科技有限公司 | Iron chloride-chitosan compounding coagulation agent and preparation method thereof |
| CN108658198A (en) * | 2018-07-24 | 2018-10-16 | 昆山佳洪源环境科技有限公司 | A kind of environmental protection Waste water treatment medicament |
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| CN108658198A (en) * | 2018-07-24 | 2018-10-16 | 昆山佳洪源环境科技有限公司 | A kind of environmental protection Waste water treatment medicament |
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