CN109231390A - A kind of sewage treatment flocculating agent and preparation method with slow-release function - Google Patents
A kind of sewage treatment flocculating agent and preparation method with slow-release function Download PDFInfo
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- CN109231390A CN109231390A CN201811229464.4A CN201811229464A CN109231390A CN 109231390 A CN109231390 A CN 109231390A CN 201811229464 A CN201811229464 A CN 201811229464A CN 109231390 A CN109231390 A CN 109231390A
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- sewage treatment
- slow
- cyclodextrin
- flocculating agent
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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
-
- 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
-
- 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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- 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)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention belongs to the technical fields of sewage treatment, provide a kind of sewage treatment flocculating agent and preparation method with slow-release function.Flocculant is added while this method is by by the saturated aqueous solution heating stirring of cyclodextrin, is stood after lasting stirring, is then centrifuged for sediment separate out and washs repeatedly, the sewage treatment flocculating agent with slow-release function is made in last vacuum drying treatment.It is compared with the traditional method, the sewage treatment flocculating agent of preparation of the invention, flocculating property is good, and slow release flocculant activity ingredient is achieved the purpose that, has had the function of controlling medicament release, so that product active ingredient long action time, utilization rate is higher, preparation process is simple simultaneously, environmentally protective, has very high industrial application value.
Description
Technical field
The invention belongs to the technical field of sewage treatment, provide a kind of sewage treatment flocculating agent with slow-release function and
Preparation method.
Background technique
Water resource pollution is already a social concern the most serious, and water pollutant mainly includes suspended matter, organic
Object, heavy metal ion etc..Flocculence is a kind of simple, efficient, at low cost, wide adaptability processing side in sewage disposal process
Method makes the particle of difficult separation in water play pendulum, and form macromolecule polyalcohol by adding flocculant into water body
It precipitates and is removed, can be widely applied to turbidity and coloration, organic pollutant, heavy metal ion of water removal etc..
Flocculant is the key factor of flocculence sewage treatment, and by its chemical component, flocculant can be divided into inorganic salts wadding
Solidifying agent, organic polymer coargulator and microbial flocculant.Inorganic salts flocculant it is of less types, mainly aluminium salt, molysite,
The flocculants such as the low molecules such as hydrating polymer salt and inorganic polymer.Organic polymer coargulator mainly has the organic of synthesis
High polymer coagulant and Modified Natural Organic Polymeric Flocculants.
In recent years, using carrier loaded flocculant, efficient flocculating, sustained release and other effects can be reached in sewage treatment, thus
It is more and more for the research and application of the agent carrier that flocculates by favor.External hydrophilic, interior of its cyclodextrin due to cyclodextrin
The special construction of portion's oleophylic can wrap well and connect flocculant, achieve the purpose that be sustained flocculant, be conducive to control flocculation
The rate of release of the effective component of agent is taken seriously in the preparation and application of composite flocculation agent.
Flocculant sustained release performance side is improved in sewage treatment flocculating agent technology, especially addition cyclodextrin etc. both at home and abroad at present
Face has achieved certain effect.Wherein Liu Xi is far away et al. has invented a kind of slow release composite flocculant (Chinese invention patent application number
200810022487.8), in the flocculant particle containing the polyacrylamide that is coated by soluble coating, remaining for aluminium salt and
Molysite；Its composition by weight percentage are as follows: aluminium salt 40 ~ 60%, molysite 15 ~ 30%, polyacrylamide 0.1 ~ 10%, solubility packet
Cover object 1 ~ 5%；The invention combines the characteristics of inorganic and organic flocculant, improves adding of agent mode, multistep dissolution sustained release
Process increases the functioning efficiency of various flocculants, improves the efficiency of medicament.In addition, Yang Wensi has invented one kind with cyclodextrin
For the star copolymer sewage-treating agent and its RAFT the preparation method (Chinese invention patent application number 201710818672.7) of core, with
Cyclodextrin is core, and each glucose unit of cyclodextrin is connected with acrylamide copolymer strand, number-average molecular weight 300000 ~
800000, and polydispersity coefficient is less than 1.5；The preparation method comprises the following steps: using the dithioesters containing acid chloride group or three monothioesters first
The dithioesters or three monothioesters for preparing amino substitution are reacted with diamine, are then pasted again with more (6- p-toluenesulfonyl) rings
Essence reaction prepares star-like RAFT reagent；Then under the action of initiator, star-like RAFT reagent, cause monomer solution polymerization system
Standby star copolymer out.
As it can be seen that the generally existing flocculation rate of sewage treatment flocculating agent in the prior art is too fast, it is subsequent to continue to occur
The technological deficiency of effectiveness, and existing immature, the effect using cyclodextrin etc. as the technical method of carrier realization sustained release performance
It is undesirable.
Summary of the invention
In response to this, it is proposed that a kind of sewage treatment flocculating agent and preparation method with slow-release function, can show
The slow release effect for improving flocculant is write, so that the active constituent long action time of flocculant, utilization rate is higher, wastewater treatment efficiency
It is good.
To achieve the above object, specific technical solution of the present invention is as follows:
A kind of preparation method of the sewage treatment flocculating agent with slow-release function, by stirring the saturated aqueous solution heating of cyclodextrin
Flocculant is added while mixing, is stood after lasting stirring, is then centrifuged for sediment separate out and washs repeatedly, finally at vacuum drying
The sewage treatment flocculating agent with slow-release function is made in reason, and specific step is as follows for preparation:
(1) saturated aqueous solution of cyclodextrin is accurately prepared according to the solubility of cyclodextrin；
(2) cyclodextrin saturated aqueous solution made from step (1) is subjected to heating stirring, while flocculant is added, then persistently stirred
It mixes and stands after a certain period of time, using the special cavity structure of cyclodextrin, so that flocculant enters cavity inside and forms cyclodextrin packet
The product of flocculant is tied, mixed liquor is made；
(3) then mixed liquor made from step (2) is washed repeatedly using sediment is centrifugally separating to obtain with ethyl alcohol and acetone,
Surface of solids remnants flocculant is removed, is then dried in vacuo, the sewage treatment flocculating agent with slow-release function is made.
Preferably, step (1) cyclodextrin is at least one of alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin.
Preferably, step (2) cyclodextrin, flocculant mass ratio be 5 ~ 10:1.
Preferably, step (2) described flocculant is mixed by polyacrylamide, aluminium polychloride, poly-ferric chloride；
It is further preferred that in every 100 parts by weight flocculant, 4 ~ 8 parts by weight of polyacrylamide, 45 ~ 48 weight of aluminium polychloride
Part, 44 ~ 51 parts by weight of poly-ferric chloride.
Preferably, the temperature of step (2) described heating stirring is 60 ~ 80 DEG C, and speed of agitator is 500 ~ 600r/min.
Preferably, step (2) time persistently stirred is 10 ~ 24 h.
Preferably, the time of step (2) described standing is 6 ~ 10h.
Preferably, step (3) washing repeatedly is first to use ethanol washing 2 ~ 4 times, then with acetone washing 2 ~ 4 times.
Preferably, step (3) the vacuum drying temperature be 70 ~ 80 DEG C, vacuum degree be 50 ~ 100Pa, the time be 10 ~
12h。
Cyclodextrin is one that amylose generates under the cyclodextrin glycosyltransferase effect generated by bacillus
The general name of series of annular oligosaccharide usually contains 6 ~ 12 D- glucopyranose units.Cyclodextrin molecular, which has, to be tapered slightly
Hollow cylinder three-dimensional ring structure, in its empty structure, outer upper end (larger open end) is made of the secondary hydroxyl of C2 and C3,
Lower end (smaller opening end) is made of the primary hydroxyl of C6, has hydrophily, and due to the shielding action shape by c h bond in cavity
At hydrophobic region.Embeddable various organic compounds in its hydrophobic cavity form clathrate, and change by inclusion complex
Physics and chemical property；Can interlink on cyclodextrin molecular many functional groups or by cyclodextrin interlinkage on polymer, into
Row chemical modification is polymerize by monomer of cyclodextrin.The present invention creatively utilizes the external hydrophilic of cyclodextrin, inside
The special construction of oleophylic, using cyclodextrin as slow-released carrier, using the special cavity structure of cyclodextrin, so that flocculant enters sky
Intracavitary portion forms the product of cyclic dextrin clathrate flocculant, realizes excellent slow release effect.
The present invention also provides a kind of sewage treatment flocculating agents with slow-release function that above-mentioned preparation method is prepared.
The sustained release flocculant is the saturated aqueous solution for first preparing cyclodextrin, under condition of heating and stirring, flocculant is added, after lasting stirring
It stands, is centrifugated sediment, wash removal surface of solids remnants flocculant repeatedly with ethyl alcohol and acetone, gained solid content passes through
Vacuum drying treatment and be made.
The present invention provides a kind of sewage treatment flocculating agent and preparation method with slow-release function, with prior art phase
Than the feature and excellent effect protruded is:
1. sewage treatment flocculating agent prepared by the present invention, flocculating effect and sustained release performance are good, can be widely used in sewage treatment.
2. preparation method of the invention improves the flocculating property of flocculant, reach slow release flocculant activity ingredient
Purpose, and then play the role of control medicament release so that product active ingredient long action time, utilization rate are higher.
3. preparation process of the present invention is simple, Flocculating Effect of Flocculant obtained is good, environmentally protective, has very high industry
Application value.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
The saturated aqueous solution for first preparing alpha-cyclodextrin is then heated to temperature and is 68 DEG C and is stirred with the revolving speed of 560r/min, pressed
Mass ratio according to cyclodextrin, flocculant is that flocculant is added in 7:1, stands 8h after continuing 17h, mixed liquor is made, wherein flocculation
Agent is polyacrylamide, aluminium polychloride, poly-ferric chloride mix, and in every 100kg flocculant, polyacrylamide 5kg, is gathered
Close aluminium chloride 47kg, poly-ferric chloride 48kg；Then by mixed liquor using sediment is centrifugally separating to obtain, ethanol washing 3 is first used
It is secondary, then with acetone washing 3 times, surface of solids remnants flocculant is removed, it is finally dry in the case where temperature is 76 DEG C, vacuum degree is 70Pa
The sewage treatment flocculating agent with slow-release function is made in 11h.
Test method:
Using the municipal wastewater of sewage treatment plant as water sample, the volume ratio of sanitary sewage and industrial wastewater is about 8:2, and appearance is
Grayish green, color cloudy suspension, pH is 8 ~ 9；Floc test is carried out to municipal wastewater using Beaker Test method, takes 0.5L water sample in burning
In cup, sewage treatment flocculating agent produced by the present invention is added according to the dosage of 20mg/L, is added in 0.5L water sample, and quickly stir
Mix 1min(280r/min), then speed of agitator is down to 60r/min, stir 10min, respectively quiet heavy 5min, 15min, 30min,
60min takes supernatant at 2cm under liquid level with pipette, carries out analysis test.COD value is measured using potassium dichromate method,
GB13200-91 spectrophotometry measures sample turbidity, and liquid coloration measures fixation degree, removal rate=(A0- A1)/A0× 100%,
In formula, A0And A1Respectively water sample turbidity before and after the processing or coloration or COD value.
The data obtained is as shown in table 1.
Embodiment 2
The saturated aqueous solution for first preparing beta-cyclodextrin is then heated to temperature and is 65 DEG C and is stirred with the revolving speed of 580r/min, pressed
Mass ratio according to cyclodextrin, flocculant is that flocculant is added in 6:1, stands 9h after continuing 14h, mixed liquor is made, wherein flocculation
Agent is polyacrylamide, aluminium polychloride, poly-ferric chloride mix, and in every 100kg flocculant, polyacrylamide 5kg, is gathered
Close aluminium chloride 46g, poly-ferric chloride 49kg；Then by mixed liquor using sediment is centrifugally separating to obtain, ethanol washing 2 is first used
It is secondary, then with acetone washing 3 times, surface of solids remnants flocculant is removed, it is finally dry in the case where temperature is 72 DEG C, vacuum degree is 60Pa
The sewage treatment flocculating agent with slow-release function is made in 12h.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 3
The saturated aqueous solution for first preparing gamma-cyclodextrin is then heated to temperature and is 75 DEG C and is stirred with the revolving speed of 520r/min, pressed
Mass ratio according to cyclodextrin, flocculant is that flocculant is added in 9:1, stands 9h after continuing 22h, mixed liquor is made, wherein flocculation
Agent is polyacrylamide, aluminium polychloride, poly-ferric chloride mix, and in every 100kg flocculant, polyacrylamide 7kg, is gathered
Close aluminium chloride 47kg, poly-ferric chloride 46kg；Then by mixed liquor using sediment is centrifugally separating to obtain, ethanol washing 4 is first used
It is secondary, then with acetone washing 3 times, surface of solids remnants flocculant is removed, it is finally dry in the case where temperature is 78 DEG C, vacuum degree is 90Pa
The sewage treatment flocculating agent with slow-release function is made in 10.5h.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 4
The saturated aqueous solution for first preparing alpha-cyclodextrin is then heated to temperature and is 60 DEG C and is stirred with the revolving speed of 500r/min, pressed
Mass ratio according to cyclodextrin, flocculant is that flocculant is added in 5:1, stands 6h after continuing 10h, mixed liquor is made, wherein flocculation
Agent is polyacrylamide, aluminium polychloride, poly-ferric chloride mix, and in every 100kg flocculant, polyacrylamide 4kg, is gathered
Close aluminium chloride 45kg, poly-ferric chloride 51kg；Then by mixed liquor using sediment is centrifugally separating to obtain, ethanol washing 2 is first used
It is secondary, then with acetone washing 2 times, surface of solids remnants flocculant is removed, it is finally dry in the case where temperature is 70 DEG C, vacuum degree is 50Pa
The sewage treatment flocculating agent with slow-release function is made in 12h.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 5
The saturated aqueous solution for first preparing beta-cyclodextrin is then heated to temperature and is 80 DEG C and is stirred with the revolving speed of 600r/min, pressed
Mass ratio according to cyclodextrin, flocculant is that flocculant is added in 10:1, continues to stand 10h afterwards for 24 hours, mixed liquor is made, wherein wadding
Solidifying agent is polyacrylamide, aluminium polychloride, poly-ferric chloride mix, in every 100kg flocculant, polyacrylamide 8kg,
Aluminium polychloride 48kg, poly-ferric chloride 44kg；Then mixed liquor is first used into ethanol washing using sediment is centrifugally separating to obtain
4 times, then with acetone washing 4 times, surface of solids remnants flocculant is removed, finally done in the case where temperature is 80 DEG C, vacuum degree is 100Pa
The sewage treatment flocculating agent with slow-release function is made in dry 10h.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 6
The saturated aqueous solution for first preparing gamma-cyclodextrin is then heated to temperature and is 70 DEG C and is stirred with the revolving speed of 550r/min, pressed
Mass ratio according to cyclodextrin, flocculant is that flocculant is added in 8:1, stands 8h after continuing 18h, mixed liquor is made, wherein flocculation
Agent is polyacrylamide, aluminium polychloride, poly-ferric chloride mix, and in every 100kg flocculant, polyacrylamide 6kg, is gathered
Close aluminium chloride 46kg, poly-ferric chloride 48kg；Then by mixed liquor using sediment is centrifugally separating to obtain, ethanol washing 3 is first used
It is secondary, then with acetone washing 3 times, surface of solids remnants flocculant is removed, it is finally dry in the case where temperature is 75 DEG C, vacuum degree is 80Pa
The sewage treatment flocculating agent with slow-release function is made in 11h.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Comparative example 1
In sewage treatment flocculating agent preparation process, not using cyclodextrin as slow-released carrier, other preparation conditions and embodiment 6 one
It causes.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Table 1:
Claims (10)
1. a kind of preparation method of the sewage treatment flocculating agent with slow-release function, which is characterized in that pass through satisfying cyclodextrin
Flocculant is added while with aqueous solution heating stirring, is stood after lasting stirring, is then centrifuged for sediment separate out and washs repeatedly,
The sewage treatment flocculating agent with slow-release function is made in last vacuum drying treatment, and specific step is as follows for preparation:
(1) saturated aqueous solution of cyclodextrin is prepared；
(2) cyclodextrin saturated aqueous solution made from step (1) is subjected to heating stirring, while flocculant is added, then persistently stirred
It mixes and stands after a certain period of time, using the special cavity structure of cyclodextrin, so that flocculant enters cavity inside and forms cyclodextrin packet
The product of flocculant is tied, mixed liquor is made；
(3) then mixed liquor made from step (2) is washed repeatedly using sediment is centrifugally separating to obtain with ethyl alcohol and acetone,
Surface of solids remnants flocculant is removed, is then dried in vacuo, the sewage treatment flocculating agent with slow-release function is made.
2. a kind of preparation method of the sewage treatment flocculating agent with slow-release function according to claim 1, it is characterised in that:
Step (1) cyclodextrin is at least one of alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin.
3. a kind of preparation method of the sewage treatment flocculating agent with slow-release function according to claim 1, it is characterised in that:
Step (2) cyclodextrin, flocculant mass ratio be 5 ~ 10:1.
4. a kind of preparation method of the sewage treatment flocculating agent with slow-release function according to claim 1, it is characterised in that:
Step (2) described flocculant is mixed by polyacrylamide, aluminium polychloride, poly-ferric chloride；Every 100 parts by weight flocculation
In agent, 4 ~ 8 parts by weight of polyacrylamide, 45 ~ 48 parts by weight of aluminium polychloride, 44 ~ 51 parts by weight of poly-ferric chloride.
5. a kind of preparation method of the sewage treatment flocculating agent with slow-release function according to claim 1, it is characterised in that:
The temperature of step (2) described heating stirring is 60 ~ 80 DEG C, and speed of agitator is 500 ~ 600r/min.
6. a kind of preparation method of the sewage treatment flocculating agent with slow-release function according to claim 1, it is characterised in that:
Step (2) time persistently stirred is 10 ~ 24 h.
7. a kind of preparation method of the sewage treatment flocculating agent with slow-release function according to claim 1, it is characterised in that:
The time of step (2) described standing is 6 ~ 10h.
8. a kind of preparation method of the sewage treatment flocculating agent with slow-release function according to claim 1, it is characterised in that:
Step (3) washing repeatedly is first to use ethanol washing 2 ~ 4 times, then with acetone washing 2 ~ 4 times.
9. a kind of preparation method of the sewage treatment flocculating agent with slow-release function according to claim 1, it is characterised in that:
Step (3) the vacuum drying temperature is 70 ~ 80 DEG C, and vacuum degree is 50 ~ 100Pa, and the time is 10 ~ 12h.
10. the sewage treatment flocculating agent with slow-release function that any one of claim 1 ~ 9 preparation method is prepared.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811229464.4A CN109231390A (en) | 2018-10-22 | 2018-10-22 | A kind of sewage treatment flocculating agent and preparation method with slow-release function |
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| CN201811229464.4A CN109231390A (en) | 2018-10-22 | 2018-10-22 | A kind of sewage treatment flocculating agent and preparation method with slow-release function |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109809550A (en) * | 2019-02-28 | 2019-05-28 | 长沙埃比林环保科技有限公司 | A kind of preparation method of sewage treating material |
| CN111732173A (en) * | 2020-07-29 | 2020-10-02 | 陈泳帆 | Efficient composite flocculant for sewage treatment |
| CN112441675A (en) * | 2019-08-30 | 2021-03-05 | 中国石油化工股份有限公司 | Treatment method of oily sewage and application thereof |
-
2018
- 2018-10-22 CN CN201811229464.4A patent/CN109231390A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109809550A (en) * | 2019-02-28 | 2019-05-28 | 长沙埃比林环保科技有限公司 | A kind of preparation method of sewage treating material |
| CN112441675A (en) * | 2019-08-30 | 2021-03-05 | 中国石油化工股份有限公司 | Treatment method of oily sewage and application thereof |
| CN111732173A (en) * | 2020-07-29 | 2020-10-02 | 陈泳帆 | Efficient composite flocculant for sewage treatment |
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Application publication date: 20190118 |