CN102838198A - Preparation method of novel flocculant for sewage treatment - Google Patents
Preparation method of novel flocculant for sewage treatment Download PDFInfo
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- CN102838198A CN102838198A CN 201210337384 CN201210337384A CN102838198A CN 102838198 A CN102838198 A CN 102838198A CN 201210337384 CN201210337384 CN 201210337384 CN 201210337384 A CN201210337384 A CN 201210337384A CN 102838198 A CN102838198 A CN 102838198A
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Abstract
The invention discloses a preparation method of a novel flocculant for sewage treatment. The preparation method comprises the steps as follows: carrying out alkalization reaction on bagasse at first, and acylating and modifying the bagasse by ethylene diamine tetraacetic dianhydride, then reacting the acylated and modified bagasse with acrylic acid and pentaerythritol in the step 3 to obtain a net-shaped macromolecular structure taking acylated cellulose molecules in the bagasse as frameworks and radial multi-grafted polypropylenes as flexible tentacles. Such macromolecular structure can better capture suspension particles so as to obtain a good flocculation effect.
Description
Technical field
The present invention relates to a kind of preparation method of novel flocculant, relate to a kind of preparation method who is used for the novel flocculant of WWT especially.
Background technology
The discharging of city domestic sewage has caused the serious environmental pollution.Many-sided factors such as the character in city, existing water exhaust system, temperature, water resources and the level of economic development thereof all can influence the characteristic of municipal effluent.The principal feature of China's municipal effluent is at present: the municipal effluent of the low organic concentration of the organic concentration of (1) waste water causes difficulty to biological treatment; (2) biochemical method is also adopted in the rough handling of the biodegradability difference trade effluent of waste water often; So after treatment; Staying the organic matter that gets into city planting ductwork in the waste water is difficult to biodegradable often; The B/C value of waste water is lower, therefore contains the biodegradability variation of the municipal effluent of a large amount of trade effluents, is unfavorable for biochemical treatment; (3) complicated component of waste water is because the complicacy and the economic technology possibility of each industrial and mining enterprises' waste water composition; The project of control can not be comprehensive; So may introduce the material that some are unfavorable for the objectionable impurities of microorganism growth or cause activated sludge bulking in the waste water, thereby make troubles for the operation and the management of Sewage Plant; (4) water quality of waste water, water yield fluctuation are greatly.
The main method of current WWT has two big types: the one, and physico-chemical processes, i.e. Coagulation Method; The 2nd, biochemical process.Physico-chemical process is to removing colourity, heavy metal, phosphorus, effective, but undesirable to nitrogen and organic matter removal effect.Biochemical process has good removal effect to organic pollutant and nitrogen, phosphorus, but low to the COD clearance, decolorizing effect is poor, and can produce a large amount of mud, causes secondary environmental pollution.General biochemical process requires the biodegradability of waste water good; Each nutritive proportion is coordinated, concentration is suitable; And the concentration that wherein suppresses the biological growth material is not higher than the scope that mikrobe can bear; So for the present waste water in some cities, maybe be owing to contain aspects such as the fluctuation of a large amount of biostatss or water quality and quantity is excessive in the waste water, the operation of its biological treatment system is little sometimes normal.And biochemical process is had relatively high expectations to temperature, and when low temperature, microbic activity can step-down, have in addition possibly completely lose activity, thereby cause some biochemical treatment unit normally not move.Therefore, the physico-chemical process Treating Municipal Sewage has advantage than biochemical process.The flocculation agent of using in the physico-chemical process more and more comes into one's own.
The residue that the squeezing back produced when bagasse was meant cane sugar manufacture, according to present production level, one ton of sucrose of about every production will produce the bagasse about 3 tons.These bagasse rich cellulose, bagasse is mainly used in the growth matrix of papermaking and edible mushrooms at present.Also rarely have bagasse is applied to the report that flocculation agent is produced.
Summary of the invention
The invention provides a kind of is the preparation method of the novel flocculant that is used for WWT of main raw material with bagasse, and this method comprises the steps:
(1) the bagasse powder being placed excessive concentration is 20%～25% sodium hydroxide solution, and the reaction times is 20～24 hours, and it is air-dry subsequently bagasse to be taken out the back, makes its water cut be lower than 10%;
(2) the bagasse powder after the alkalinisation treatment is at first placed toluene; And utilize heater means to make toluene solution remain on 40～50 degrees centigrade; Adding concentration subsequently is the YD 30 dianhydride acetone soln of 0.1～0.15g/mL, in temperature is under 30～35 degrees centigrade the situation, to react 40～60 minutes; The amount of the YD 30 dianhydride acetone soln that adds is 50%～90% of a bagasse powder, and product is cleaned with acetone and be dry;
(3) with the aqueous solution of the product of handling gained in the step (2) and the acrylic acid aqueous solution of monomer, tetramethylolmethane; And make and be full of nitrogen in the reaction environment; Reaction times is 4～6 hours; Add the sodium dichromate 99 sulphuric acid soln subsequently, and temperature is remained between 40～45 degrees centigrade, reacted again 1～2 hour;
(4) dropping sodium solution in the mashed prod that in step (3), obtains is adjusted to its pH value between 7～8, uses extraction using alcohol twice then, then the throw out that obtains is used washing with acetone, and drying obtains flocculation agent of the present invention.
Wherein the excessive sodium hydroxide solution described in the step (1) is meant that the sodium hydroxide solution and the volume mass ratio of bagasse are not less than 5ml: 1g.
Wherein the concentration of the monomer acrylic acid aqueous solution described in the step (3) is 12%～15%; The concentration of the tetramethylolmethane aqueous solution is 5%～10%; The concentration of sodium dichromate 99 sulphuric acid soln is 10%～15%; The volume mass ratio of employed amount and bagasse is following: monomer acrylic acid aqueous solution 3～5mL: 1g, the tetramethylolmethane aqueous solution 2～3mL: 1g, sodium dichromate 99 sulphuric acid soln 0.5～1mL: 1g.
The present invention at first carries out quaternization with bagasse; Make it obtain acylation modification with the YD 30 dianhydride subsequently; Bagasse behind the acylation modification reacts with vinylformic acid, tetramethylolmethane one in step 3, and can to obtain cellulosic molecule with acidylate in the bagasse be skeleton, is the netted macromolecular structure of flexible tentacle with radial racemosus Vestolen PP 7052.This macromolecular structure can be caught suspended particle better, reaches good flocculating effect.
Embodiment
Embodiment 1
Prepare flocculation agent by following method:
(1) the bagasse powder being placed excessive concentration is 25% sodium hydroxide solution, and the reaction times is 20 hours, and it is air-dry subsequently bagasse to be taken out the back, makes its water cut be lower than 10%;
(2) the bagasse powder after the alkalinisation treatment is at first placed toluene; And utilize heater means to make toluene solution remain on 50 degrees centigrade; Adding concentration subsequently is the YD 30 dianhydride acetone soln of 0.1g/mL, in temperature is under 35 degrees centigrade the situation, to react 40 minutes; The amount of the YD 30 dianhydride acetone soln that adds is 70% of a bagasse powder, and product is cleaned with acetone and be dry;
(3) with the aqueous solution of the product of handling gained in the step (2) and the acrylic acid aqueous solution of monomer, tetramethylolmethane; And make to be full of nitrogen in the reaction environment, the reaction times is 4 hours, adds the sodium dichromate 99 sulphuric acid soln subsequently; And temperature remained between 40 degrees centigrade, reacted again 2 hours;
(4) dropping sodium solution in the mashed prod that in step (3), obtains is adjusted to 7.5 with its pH value, uses extraction using alcohol twice then, then the throw out that obtains is used washing with acetone, and drying obtains flocculation agent of the present invention.
Wherein the volume mass of sodium hydroxide solution described in the step (1) and bagasse is 10ml: 1g.
Wherein the concentration of employed monomer acrylic acid aqueous solution is 12% in the step (3); The concentration of the tetramethylolmethane aqueous solution is 7%; The concentration of sodium dichromate 99 sulphuric acid soln is 10%; The volume mass ratio of employed amount and bagasse is following: monomer acrylic acid aqueous solution 5mL: 1g, tetramethylolmethane aqueous solution 3mL: 1g, sodium dichromate 99 sulphuric acid soln 1mL: 1g.
Embodiment 2
Prepare flocculation agent by following method:
(1) the bagasse powder being placed excessive concentration is 20% sodium hydroxide solution, and the reaction times is 24 hours, and it is air-dry subsequently bagasse to be taken out the back, makes its water cut be lower than 10%;
(2) the bagasse powder after the alkalinisation treatment is at first placed toluene; And utilize heater means to make toluene solution remain on 40 degrees centigrade; Adding concentration subsequently is the YD 30 dianhydride acetone soln of 0.15g/mL, in temperature is under 30 degrees centigrade the situation, to react 60 minutes; The amount of the YD 30 dianhydride acetone soln that adds is 90% of a bagasse powder, and product is cleaned with acetone and be dry;
(3) with the aqueous solution of the product of handling gained in the step (2) and the acrylic acid aqueous solution of monomer, tetramethylolmethane; And make to be full of nitrogen in the reaction environment, the reaction times is 6 hours, adds the sodium dichromate 99 sulphuric acid soln subsequently; And temperature remained between 60 degrees centigrade, reacted again 1 hour;
(4) dropping sodium solution in the mashed prod that in step (3), obtains is adjusted to 8 with its pH value, uses extraction using alcohol twice then, then the throw out that obtains is used washing with acetone, and drying obtains flocculation agent of the present invention.
Wherein the volume mass of sodium hydroxide solution described in the step (1) and bagasse is 10ml: 1g.
Wherein the concentration of the monomer acrylic acid aqueous solution described in the step (3) is 15%; The concentration of the tetramethylolmethane aqueous solution is 10%; The concentration of sodium dichromate 99 sulphuric acid soln is 15%; The volume mass ratio of employed amount and bagasse is following: monomer acrylic acid aqueous solution 3mL: 1g, tetramethylolmethane aqueous solution 2mL: 1g, sodium dichromate 99 sulphuric acid soln 0.5mL: 1g.
The flocculating effect experiment
With the flocculation agent and the Poly aluminum Chloride (PAC) that are obtained among the embodiment 1,2, the flocculating effect of Tai-Ace S 150 compares.The experimental technique of flocculating effect is following: get pending water 1L and place beaker, add the flocculation agent of 100ppm, left standstill at normal temperatures 5 minutes after fully shaking up, each item index to supernatant detects subsequently.The index that detects comprises: turbidity, COD, suspended substance (SS).Wherein adopt the WGZ-2000 turbidometer of Shanghai thunder magnetic instrument plant to measure turbidity, adopt potassium dichromate process to measure COD, adopt the filter paper filtering weighting method to measure suspended substance (SS).
Each item index of pending water is: turbidity 36, COD 360mg/L, SS 210mg/L.Experimental result is as shown in the table.Can find out that from experimental result flocculation agent provided by the invention is being removed aspect the turbidity, COD removal aspect, removed the SS aspect and all be superior to Poly aluminum Chloride (PAC) and Tai-Ace S 150.Explain that the method for preparing flocculation agent provided by the present invention can prepare the flocculation agent of excellent property.
| The flocculation agent that uses | Turbidity | COD(mg/L) | SS(mg/L) |
| Embodiment 1 flocculation agent | 3.4 | 34.8 | 11.3 |
| Embodiment 2 flocculation agents | 4.1 | 36.1 | 12.7 |
| Poly aluminum Chloride (PAC) | 7.8 | 46.7 | 30.2 |
| Tai-Ace S 150 | 9.4 | 50.3 | 37.3 |
Those skilled in the art can make replacement or modification to content of the present invention according to content disclosed by the invention and the art technology of being grasped; But these replacements or modification should not be regarded as breaking away from the present invention's design, and these replacements or modification are all in the interest field that the present invention requires to protect.
Claims (3)
1. preparation method who is used for the novel flocculant of WWT, this method comprises the steps:
(1) the bagasse powder being placed excessive concentration is 20%～25% sodium hydroxide solution, and the reaction times is 20～24 hours, and it is air-dry subsequently bagasse to be taken out the back, makes its water cut be lower than 10%;
(2) the bagasse powder after the alkalinisation treatment is at first placed toluene; And utilize heater means to make toluene solution remain on 40～50 degrees centigrade; Adding concentration subsequently is the YD 30 dianhydride acetone soln of 0.1～0.15g/mL, in temperature is under 30～35 degrees centigrade the situation, to react 40～60 minutes; The amount of the YD 30 dianhydride acetone soln that adds is 50%～90% of a bagasse powder, and product is cleaned with acetone and be dry;
(3) with the aqueous solution of the product of handling gained in the step (2) and the acrylic acid aqueous solution of monomer, tetramethylolmethane; And make and be full of nitrogen in the reaction environment; Reaction times is 4～6 hours; Add the sodium dichromate 99 sulphuric acid soln subsequently, and temperature is remained between 40～45 degrees centigrade, reacted again 1～2 hour;
(4) dropping sodium solution in the mashed prod that in step (3), obtains is adjusted to its pH value between 7～8, uses extraction using alcohol twice then, then the throw out that obtains is used washing with acetone, and drying obtains flocculation agent of the present invention.
2. the preparation method of the novel flocculant that is used for WWT described in the claim 1 is characterized in that wherein the excessive sodium hydroxide solution described in the step (1) is meant that the sodium hydroxide solution and the volume mass ratio of bagasse are not less than 5ml: 1g.
3. the preparation method of the novel flocculant that is used for WWT described in the claim 1; It is characterized in that wherein the concentration of the monomer acrylic acid aqueous solution described in the step (3) is 12%～15%; The concentration of the tetramethylolmethane aqueous solution is 5%～10%; The concentration of sodium dichromate 99 sulphuric acid soln is 10%～15%; The volume mass ratio of employed amount and bagasse is following: monomer acrylic acid aqueous solution 3～5mL: 1g, the tetramethylolmethane aqueous solution 2～3mL: 1g, sodium dichromate 99 sulphuric acid soln 0.5～1mL: 1g.
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| CN 201210337384 CN102838198A (en) | 2012-09-13 | 2012-09-13 | Preparation method of novel flocculant for sewage treatment |
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| CN 201210337384 CN102838198A (en) | 2012-09-13 | 2012-09-13 | Preparation method of novel flocculant for sewage treatment |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621577A (en) * | 2016-02-29 | 2016-06-01 | 济南大学 | Composite biomass fiber coagulant prepared from bagasse |
| CN105668738A (en) * | 2016-02-29 | 2016-06-15 | 济南大学 | Biomass coupling coagulant synthesized by vinegar residue |
| CN109879578A (en) * | 2019-03-14 | 2019-06-14 | 广东省生物工程研究所（广州甘蔗糖业研究所） | A kind of dehydrating residual active sludge filter aid and its application |
| CN111320355A (en) * | 2019-11-21 | 2020-06-23 | 佛山科学技术学院 | Preparation method of efficient flocculant for sludge dewatering |
-
2012
- 2012-09-13 CN CN 201210337384 patent/CN102838198A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621577A (en) * | 2016-02-29 | 2016-06-01 | 济南大学 | Composite biomass fiber coagulant prepared from bagasse |
| CN105668738A (en) * | 2016-02-29 | 2016-06-15 | 济南大学 | Biomass coupling coagulant synthesized by vinegar residue |
| CN109879578A (en) * | 2019-03-14 | 2019-06-14 | 广东省生物工程研究所（广州甘蔗糖业研究所） | A kind of dehydrating residual active sludge filter aid and its application |
| CN109879578B (en) * | 2019-03-14 | 2022-01-28 | 广东省生物工程研究所（广州甘蔗糖业研究所） | Residual activated sludge dewatering filter aid and application thereof |
| CN111320355A (en) * | 2019-11-21 | 2020-06-23 | 佛山科学技术学院 | Preparation method of efficient flocculant for sludge dewatering |
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Application publication date: 20121226 |