CN107879447A - A kind of preparation method for being used to handle oil-polluted water flocculant - Google Patents
A kind of preparation method for being used to handle oil-polluted water flocculant Download PDFInfo
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- CN107879447A CN107879447A CN201711415735.0A CN201711415735A CN107879447A CN 107879447 A CN107879447 A CN 107879447A CN 201711415735 A CN201711415735 A CN 201711415735A CN 107879447 A CN107879447 A CN 107879447A
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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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic System
- C07F1/08—Copper compounds
Abstract
The invention discloses a kind of preparation method for being used to handle oil-polluted water flocculant, mainly using chitosan as primary raw material, bodied ferric sulfate, polyaluminium sulfate, PDDA and rhenocure CA copper complex are added in preparation process simultaneously and is modified processing, stable chelant thing is formed by heavy metal ion such as the mercury in the amino in chitosan molecule, carboxyl and sewage, lithium, copper, lead, silver, removes and reclaim the metal ion in waste water.Flocculant prepared by the present invention has good suction-operated, and biocompatibility is better, and its suction-operated to greasy dirt is stronger.Absorption and flocculation reaction of waste water in the decolouring of waste water, industrial production etc. are also used as in sewage disposal, there is good application value.
Description
Technical field
The present invention relates to a kind of flocculant, and in particular to the flocculant that a kind of oily sewage disposal uses.
Background technology
With the development of industrial expansion, particularly petrochemical industry, the discharge capacity of oily waste water is growing day by day, and its is right
The pollution of environment also getting worse.The industry discharge of oily waste water wide material sources, wherein petroleum industry and solid fuel hot-working
Oily waste water is its main source.In works such as oil, chemical industry, steel, coking, gas generating station, machine-building and food processings
In industry enterprise, every use water directly contacted with oils, all containing oil.In oil recovery production process, oily waste water essentially from
Oil field extracted water and water injection well well-flushing water.With the continuous exploitation in oil field, oil recovery technique continues to develop, and tertiary oil recovery technology starts
Generally applied, particularly polymer displacement of reservoir oil.Many solid particles, free oil, oil emulsion and various remaining auxiliary agents, processing
More difficult, the harm directly discharged without processing is bigger, can cause very serious environmental pollution.
The widely used method of the purification of oil-polluted water is flocculent precipitation at present, that is, flocculant is added into water.
Inorganic flocculating agent is used alone, it is big chemical feeding quantity to be present, and generation precipitation is more in water, is also easy to produce a large amount of sludge and scum silica frost, and pair plus
The shortcomings of medicine equipment, the anti-corrosion of pipeline have higher requirements, it has been difficult the requirement for meeting water process.Cation organic flocculant is not
Only overcome these shortcomings of inorganic flocculating agent, and shown in terms of enhanced flocculation removes difficult for biological degradation organic pollution
Big advantage and application prospect.Chitosan is dispersed with its strand as a kind of aboundresources, porous natural high polymer
Substantial amounts of free hydroxyl group and amino, amino is easily protonated in some dilute acid solns, so that band in chitosan molecule chain
There is substantial amounts of positive charge.One kind is synthesized using chitosan as main raw material(s) to be used to handle oil-polluted water flocculant, is improved such
The charge neutrality ability of flocculant, can further improve flocculant flocculating property, is effectively improved water quality.
The content of the invention
It is an object of the invention to provide a kind of preparation method for being used to handle oil-polluted water flocculant, and deacetylation is got over
Height, mechanical strength is bigger, and biocompatibility is better, and its suction-operated to greasy dirt is stronger.It is also used as in sewage disposal
The absorption and flocculation reaction of waste water in the decolouring of waste water, industrial production.
1st, a kind of preparation method for being used to handle oil-polluted water flocculant, it is characterised in that this method comprises the following steps：
1）10~20 parts by weight chitosans are weighed in three-necked flask, add 60~80 parts by weight of isopropyl alcohol, 15.5~20.5 weights
Part NaOH solids and 100 parts by weight of deionized water are measured, under 60 DEG C of temperature conditionss, 2~5h of stirring swelling.By 10~20 weight
Part monoxone is dissolved in 30 parts by weight of isopropyl alcohol, is added drop-wise in above-mentioned solution, is dripped in 20 minutes while stirring, and process is added dropwise
Middle temperature control is at 60~70 DEG C, after being added dropwise, continues to react 8h.After cooling, with filtered on buchner funnel, 70 % of filter residue
Ethanol solution desalination and alkali, filter 23~5 time.Then washed, filtered with the ethanol that mass fraction is 95 %, operated 3 times, filter
Dehydration is dried in vacuo above-mentioned powder solid under the conditions of 70 DEG C, that is, obtains sodium form carboxymethyl chitosan.
2）Take the above-mentioned parts by weight of sodium form carboxymethyl chitosan 5 to be placed in the beaker for filling acetone, 5~10 parts by weight oil is added dropwise
The mixed liquor of isoxazolecarboxylic acid and 5~10 pbw acetones, concentration are 6mol/L NaOH solution, being capable of temperature control during dropwise addition
Dripped in -5~0 DEG C of ice-water bath, 30min.Then above-mentioned solution is transferred in three-necked flask, controlled in semi-automatic PLC
1 ~ 2h is heated in heat-conducting oil furnace at 130 ~ 135 DEG C.Then add 2 weight parts of polymer ferric sulfate, 1 weight parts of polymer aluminum sulfate and
0.2 parts by weight PDDA, the rhenocure CA copper complex of 0.5 parts by weight, reaction time are 5 h,
Adjust pH=7.0.Reaction is filtered after terminating, and obtains solid block product, is washed, and filter residue mass fraction is 70 % second
Alcoholic solution desalination and alkali.Dried after washing, under the conditions of 80 DEG C and obtain pulverulent solids, that is, obtain can be used for processing to contain greasy dirt
The flocculant of water.
Beneficial effect：Native biopolymer polymer shell glycan heavy metal ion has very strong removal ability, and shell gathers
Substantial amounts of free amine group is dispersed with sugar subchain, is protonated in dilute acid soln, so that a large amount of on chitosan molecule chain band
Positive charge, turn into a kind of cationic polyelectrolyte.Cationic flocculant can play charge neutrality cohesion simultaneously and absorption of building bridge
Double action, i.e., the cationic reactive groups on macromolecular chain attract each other with negatively charged oil emulsion, reduce and neutralize
The surface charge of oil emulsion, while have compressed the diffusion layer of oil emulsion and make oil emulsion cohesion de- steady, and by means of macromolecule
The bonding bridging action of chain and produce adsorption and sedimentation.The rhenocure CA copper complex of addition, it is miscellaneous because containing N, S etc. in its structure
Atom and with well it is antibacterial.Chitosan can be made up in neutrality by flocculant prepared by primary raw material of chitosan in the present invention
The shortcomings that with flocculation oil emulsion is difficult in meta-alkalescence oily waste water water body, expand its applicable value scope in the treatment of waste water, and
And the absorption oil ability of chitosan can be strengthened, it is a kind of good flocculating effect, biodegradable, green new oily waste water
Inorganic agent.
Embodiment
Embodiment 1
16 parts by weight chitosans are weighed in three-necked flask, add 67 parts by weight of isopropyl alcohol, 19.5 parts by weight NaOH solids and 100
Parts by weight of deionized water, under 60 DEG C of temperature conditionss, 2~5h of stirring swelling.It is different that 10 parts by weight monoxones are dissolved in 30 parts by weight
In propyl alcohol, be added drop-wise in above-mentioned solution, dripped in 20 minutes while stirring, during dropwise addition temperature control at 60~70 DEG C,
After being added dropwise, continue to react 8h.After cooling, with filtered on buchner funnel, the 70 % ethanol solutions desalinations and alkali of filter residue, filtering
3~5 times.Then washed, filtered with the ethanol that mass fraction is 95 %, operated 3 times, filter dehydration vacuum under the conditions of 70 DEG C
Above-mentioned powder solid is dried, that is, obtains sodium form carboxymethyl chitosan.
2）Take the above-mentioned parts by weight of sodium form carboxymethyl chitosan 5 to be placed in the beaker for filling acetone, 6 parts by weight oleic acid acyls are added dropwise
The mixed liquor of chlorine and 6 pbw acetones, concentration be 6mol/L NaOH solution, during dropwise addition can temperature control -5~0
DEG C ice-water bath, drip in 30min.Then above-mentioned solution is transferred in three-necked flask, heat-conducting oil furnace is controlled in semi-automatic PLC
In 1 ~ 2h is heated at 130 ~ 135 DEG C.Then add 2 weight parts of polymer ferric sulfate, 1 weight parts of polymer aluminum sulfate and 0.2 parts by weight
PDDA, the rhenocure CA copper complex of 0.5 parts by weight, reaction time are 5 h, regulation pH=
7.0.Reaction is filtered after terminating, and obtains solid block product, is washed, and filter residue is removed with the ethanol solution that mass fraction is 70 %
Salt and alkali.Dried after washing, under the conditions of 80 DEG C and obtain pulverulent solids, that is, obtain the flocculation that can be used for processing oil-polluted water
Agent.
Above-mentioned rhenocure CA copper complex preparation method is as follows：
Accurately weigh 2 parts by weight rhenocure CAs to be dissolved in 15 parts by weight absolute ethyl alcohols, CuCl containing 1mmol is added dropwise2·2H2O's
The parts by weight of ethanol solution 10, in 150 ~ 155 DEG C of heating stirrings, back flow reaction 4h stops, and cooled and filtered, adds into filtrate
Enter 5 parts by weight DMFs, 0.521 parts by weight 4- pyridine carboxaldehydes, 5 weight parts Methylene chlorides, transfer the solution into
In 15mL test tubes, the absolute ethyl alcohol of 5 parts by weight is then gently added into test tube.Weigh the ZnSO of 0.006 parts by weight4·
7H2O, it is dissolved in the deionized water of 3 parts by weight, this solution is carefully added in above-mentioned test tube above solution, after adding
Solution holding is clarified and sealed in test tube, and after standing 14 days, the intermediate layer of second alcohol and water occurs muddy in test tube, at room temperature certainly
So volatilization, obtains bar-like single crystal, as rhenocure CA copper complex after 5 days.
Embodiment 2
Identical with embodiment 1, difference is：Weigh 10 parts by weight chitosans and 60 parts by weight are added in beaker, in beaker
Isopropanol, 15.5 parts by weight NaOH solids.
Embodiment 3
Identical with embodiment 1, difference is：Weigh 11 parts by weight chitosans and 62 parts by weight are added in beaker, in beaker
Isopropanol, 16.5 parts by weight NaOH solids.
Embodiment 4
Identical with embodiment 1, difference is：Weigh 12 parts by weight chitosans and 64 parts by weight are added in beaker, in beaker
Isopropanol, 17.5 parts by weight NaOH solids.
Embodiment 5
Identical with embodiment 1, difference is：Weigh 13 parts by weight chitosans and 65 parts by weight are added in beaker, in beaker
Isopropanol, 16.5 parts by weight NaOH solids.
Embodiment 6
Identical with embodiment 1, difference is：Weigh 14 parts by weight chitosans and 66 parts by weight are added in beaker, in beaker
Isopropanol, 17.5 parts by weight NaOH solids.
Embodiment 7
Identical with embodiment 1, difference is：Weigh 15 parts by weight chitosans and 66 parts by weight are added in beaker, in beaker
Isopropanol, 18.5 parts by weight NaOH solids.
Embodiment 8
Identical with embodiment 1, difference is：Weigh 17 parts by weight chitosans and 68 parts by weight are added in beaker, in beaker
Isopropanol, 19.5 parts by weight NaOH solids.
Embodiment 9
Identical with embodiment 1, difference is：Weigh 20 parts by weight chitosans and 68 parts by weight are added in beaker, in beaker
Isopropanol, 20.5 parts by weight NaOH solids.
Comparative example 1
Identical with embodiment 1, difference is：Rhenocure CA copper complex is not added when preparing the flocculant.
Comparative example 2
Identical with embodiment 1, difference is：Rhenocure CA copper is replaced to coordinate with rhenocure CA when preparing the flocculant
Thing.
Comparative example 3
Identical with embodiment 1, difference is：Prepare rhenocure CA copper complex and be added without 4- pyridine carboxaldehydes.
Comparative example 4
Identical with embodiment 1, difference is：Prepare rhenocure CA copper complex and be added without N,N-dimethylformamide.
Comparative example 5
Identical with embodiment 1, difference is：It is added without bodied ferric sulfate when preparing the flocculant, polyaluminium sulfate and poly-
Dimethyl diallyl ammonium chloride.
Comparative example 6
Identical with embodiment example 1, difference is：Add bodied ferric sulfate when preparing the flocculant, polyaluminium sulfate, still
It is added without PDDA.
Comparative example 7
Identical with embodiment example 1, difference is：It is added without bodied ferric sulfate when preparing the flocculant, polyaluminium sulfate, but
It is to add PDDA.
Comparative example 8
Identical with embodiment example 1, difference is：Be added without when preparing the flocculant PDDA and
Bodied ferric sulfate, add polyaluminium sulfate.
Comparative example 9
Identical with embodiment example 1, difference is：Change when preparing the flocculant and add in semi-automatic PLC controls heat-conducting oil furnace
Hot temperature is 100 ~ 105 DEG C.
Flocculant by being prepared as follows to the embodiment of the present invention 1 ~ 9 and comparative example 1 ~ 9 carries out performance test：
（1）Oil-polluted water is prepared:Weigh the gasoline of 1 g 93 to be added in 2 L glass beaker, add 2 L deionized water,
Under 90 DEG C of heated conditions, more than the h of high speed magnetic stirring 4, obtain originating oil content of wastewater C0Contain greasy dirt for 500 mg/L
Water.
（2）Flocculating property is tested:Embodiment 1 ~ 9 and each 0.5g of flocculant prepared in comparative example 1 ~ 9 are weighed, is sequentially added
Into different conical flasks, 100 m L oil-polluted water water samples are added into each conical flask, be put into constant temperature oscillation case 25 DEG C,
Continuously 6 h of concussion, taking-up are filtered under the conditions of 180r/min, the oil content C after measure processing in water1, calculated by below equation
Oil removal rate R is drawn, test result see the table below.
R=（C0- C1）/C0×100%
For handling oil-polluted water flocculant performance test
With the increasing of chitosan, isopropanol and NaOH solids loading contents in embodiment 1~9 it can be seen from upper table data analysis
Add, oil removal rate R is first raised and reduced afterwards, when chitosan, isopropanol and NaOH solid dosages distinguish 16,67,19.5 parts by weight when remove
Oil cut rate reaches highest, and reason is probably the chitosan molecule chain when the dosage increase of chitosan, isopropanol and NaOH amount of solid etc.
Upper positive charge is also more, can effectively remove negatively charged oil emulsion.When chitosan excess, formed flocculation body weight can be made
It is new to become stable colloid, absorption of the flocculant to residual oil is limited, causes oil removal rate to decline.It can be seen by comparative example 1 ~ 4
Go out, the addition of rhenocure CA copper complex is very big to flocculant oil removing performance impact when preparing flocculant, and reason is probably two
Because having containing hetero atoms such as N, S outside bacteriostasis in phenylthiourea copper complex structure, rhenocure CA copper complex exists
There is certain catalytic action when preparing flocculant.By comparative example 5~9 it can be seen that bodied ferric sulfate, polyaluminium sulfate and poly- two
The addition of methyl diallyl ammonium chloride has considerable influence to flocculant performance, and reason is probably bodied ferric sulfate, polymerised sulphur
Cation in sour aluminium and PDDA can produce synergy with the flocculant, remove oil emulsion.
Claims (4)
1. a kind of preparation method for being used to handle oil-polluted water flocculant, it is characterised in that this method comprises the following steps：
1）10~20 parts by weight chitosans are weighed in three-necked flask, add 60~80 parts by weight of isopropyl alcohol, 15.5~20.5 weights
Part NaOH solids and 100 parts by weight of deionized water are measured, under 60 DEG C of temperature conditionss, 2~5h of stirring swelling；
10 parts by weight monoxones are dissolved in 30 parts by weight of isopropyl alcohol, are added drop-wise to while stirring in above-mentioned solution, are dripped in 20 minutes
Add, temperature control is at 60~70 DEG C or so during dropwise addition, after being added dropwise, continues to react 8h；
After cooling, with filtered on buchner funnel, the 70 % ethanol solutions desalinations and alkali of filter residue, filter 23~5 time；
Then washed, filtered with the ethanol that mass fraction is 95 %, operated 3 times, filtered dehydration and be dried in vacuo under the conditions of 70 DEG C
Above-mentioned powder solid, that is, obtain sodium form carboxymethyl chitosan；
2）Take the above-mentioned parts by weight of sodium form carboxymethyl chitosan 5 to be placed in the beaker for filling acetone, be added dropwise 6 parts by weight oleic acid acyl chlorides and
The mixed liquor of 6 pbw acetones, concentration be 6mol/L NaOH solution, during dropwise addition can temperature control in -5~0 DEG C of ice
Water-bath, drip in 30min；
Then above-mentioned solution is transferred in three-necked flask, in semi-automatic PLC controls heat-conducting oil furnace heating 1 at 130 ~ 135 DEG C ~
2h；
Then add 2 weight parts of polymer ferric sulfate, 1 weight parts of polymer aluminum sulfate and 0.2 parts by weight poly dimethyl allyl chlorine
Change ammonium, the rhenocure CA copper complex of 0.5 parts by weight, the reaction time is 5 h, adjusts pH=7.0；
Reaction is filtered after terminating, and obtains solid block product, is washed, and filter residue is removed with the ethanol solution that mass fraction is 70 %
Salt and alkali.
2. being dried after washing, under the conditions of 80 DEG C and obtaining pulverulent solids, that is, obtain the flocculation that can be used for processing oil-polluted water
Agent；
A kind of preparation method for being used to handle oil-polluted water flocculant according to claim 1, it is characterised in that step 1）In
The viscosity of chitosan is 0.7~1.0Pas.
A kind of 3. preparation method for being used to handle oil-polluted water flocculant according to claim 1, it is characterised in that step 1）
Middle stir speed (S.S.) is 300rmp.
4. a kind of preparation method for being used to handle oil-polluted water flocculant according to claim 1, the rhenocure CA copper
Complex preparation method is as follows：
Accurately weigh 2 parts by weight rhenocure CAs to be dissolved in 15 parts by weight absolute ethyl alcohols, CuCl containing 1mmol is added dropwise2·2H2O's
The parts by weight of ethanol solution 10, in 150 ~ 155 DEG C of heating stirrings, back flow reaction 4h stops, and cooled and filtered, adds into filtrate
Enter 5 parts by weight DMFs, 0.521 parts by weight 4- pyridine carboxaldehydes, 5 weight parts Methylene chlorides, transfer the solution into
In 15mL test tubes, the absolute ethyl alcohol of 5 parts by weight is then gently added into test tube；
Weigh the ZnSO of 0.006 parts by weight4·7H2O, it is dissolved in the deionized water of 3 parts by weight, this solution is carefully added to
In above-mentioned test tube above solution, add solution in rear test tube and keep clarifying and sealing, stand 14 days, second alcohol and water in test tube
There is muddiness in intermediate layer, volatilizees naturally at room temperature, bar-like single crystal, as rhenocure CA copper complex are obtained after 5 days.
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| CN201711415735.0A CN107879447B (en) | 2017-12-25 | 2017-12-25 | Preparation method of flocculant for treating oily sewage |
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| CN201711415735.0A CN107879447B (en) | 2017-12-25 | 2017-12-25 | Preparation method of flocculant for treating oily sewage |
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| CN107879447B CN107879447B (en) | 2020-09-08 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111807483A (en) * | 2020-08-06 | 2020-10-23 | 中科乐美环保科技有限公司 | Flocculation and sterilization dual-function water treatment agent and preparation method thereof |
| CN117683185A (en) * | 2024-02-04 | 2024-03-12 | 天津环科瞻云科技发展有限公司 | Flocculant for sewage treatment and preparation method thereof |
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| CN102977227A (en) * | 2012-12-11 | 2013-03-20 | 杭州绿岛科技有限责任公司 | Method for preparing chitosan-like efficient flocculant |
| CN106905445A (en) * | 2017-03-30 | 2017-06-30 | 广州振清环保技术有限公司 | A kind of Polyaminated shitosan decolorising agent of carboxymethyl and its preparation method and application |
| CN107162133A (en) * | 2017-05-26 | 2017-09-15 | 贵州美瑞特环保科技有限公司 | A kind of oil gas field sewage functionalization chitin composite flocculant and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102898535A (en) * | 2012-10-19 | 2013-01-30 | 中国石油化工股份有限公司 | Preparation method and application of H-polysaccharide carboxymethyl oleoyl derivatives for oily sewage treatment |
| CN102977227A (en) * | 2012-12-11 | 2013-03-20 | 杭州绿岛科技有限责任公司 | Method for preparing chitosan-like efficient flocculant |
| CN106905445A (en) * | 2017-03-30 | 2017-06-30 | 广州振清环保技术有限公司 | A kind of Polyaminated shitosan decolorising agent of carboxymethyl and its preparation method and application |
| CN107162133A (en) * | 2017-05-26 | 2017-09-15 | 贵州美瑞特环保科技有限公司 | A kind of oil gas field sewage functionalization chitin composite flocculant and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111807483A (en) * | 2020-08-06 | 2020-10-23 | 中科乐美环保科技有限公司 | Flocculation and sterilization dual-function water treatment agent and preparation method thereof |
| CN117683185A (en) * | 2024-02-04 | 2024-03-12 | 天津环科瞻云科技发展有限公司 | Flocculant for sewage treatment and preparation method thereof |
| CN117683185B (en) * | 2024-02-04 | 2024-04-05 | 天津环科瞻云科技发展有限公司 | Flocculant for sewage treatment and preparation method thereof |
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| CN107879447B (en) | 2020-09-08 |
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