CN114380373A - Composite coagulant, preparation method thereof and application thereof in treatment of secondary effluent of sewage plant - Google Patents
Composite coagulant, preparation method thereof and application thereof in treatment of secondary effluent of sewage plant Download PDFInfo
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- CN114380373A CN114380373A CN202011112804.2A CN202011112804A CN114380373A CN 114380373 A CN114380373 A CN 114380373A CN 202011112804 A CN202011112804 A CN 202011112804A CN 114380373 A CN114380373 A CN 114380373A
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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
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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Abstract
The invention discloses a composite coagulant and a preparation method thereof and application thereof in treating secondary effluent of a sewage plant, wherein a grafting product of chitosan and dimethyl diallyl ammonium chloride is compounded on an inorganic high-molecular coagulant, so that the effects of net catching, rolling and sweeping and adsorption bridging are enhanced, colloidal particles and suspended matter charges in water can be effectively neutralized, the electric potential of an electric double layer is reduced, the size of alum flocs formed after coagulation is large, the alum flocs are easy to settle, a better pollutant removing effect is achieved, the preparation is convenient, the actual operation is easy, and the problems that the flocs of the inorganic high-molecular coagulant are fine and are difficult to settle are solved.
Description
Technical Field
The invention belongs to the field of sewage treatment, and particularly relates to a preparation method of an inorganic-organic coagulant and a method for removing total phosphorus and turbidity in secondary effluent.
Background
The advanced treatment of urban sewage as domestic miscellaneous water, industrial water or landscape water is an effective measure for effectively saving fresh water resources and reducing sewage discharge. The main problem in the current advanced treatment is the removal of phosphorus in water, the phosphorus is one of the most abundant pollutants in domestic sewage and industrial wastewater of residents, and if the discharge amount is strictly controlled without the advanced treatment, the eutrophication of surface water can be caused. In 2017 water resource bulletin, 76.9% of 117 lakes across the country are eutrophicated, which not only damages the ecological environment, but also threatens the human health.
The coagulating sedimentation is used as a common method for removing pollutants, is wide in application and simple to use, and can effectively remove the pollutants in sewage treatment. The coagulant is prepared into aqueous solution and added into water for stirring, and the effect of a compressed double electric layer is generated, so that suspended particles in the water lose stability, and colloid agglomeration causes the particles to be enlarged to form alum flocs. When the flocs grow to a certain volume, they settle down by gravity, thus removing a large amount of pollutants from the water.
The coagulant is divided into inorganic coagulant and organic coagulant, the finally formed floc of the inorganic coagulant is fine and not easy to settle, and the use of ferric salt and aluminum salt coagulant can influence the chroma of water and lead to the residue of aluminum in the water, so the research of the novel coagulant is more and more focused. The organic coagulant has the advantages of high flocculation speed, small dosage, small amount of generated sludge and the like, is widely used, but has certain limitation on use due to the problems of high price and the like, can simultaneously exert the advantages of the inorganic coagulant and the organic coagulant by compounding the inorganic coagulant and the organic coagulant, and has the advantages of convenient use, small dosage, low cost and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art that a high-molecular coagulant is used alone to form fine flocs, the flocs are not easy to settle and the removal effect is low, and provides a composite coagulant, a preparation method thereof and application thereof in treating secondary effluent of a sewage plant, so that the high-efficiency removal of total phosphorus in the secondary effluent is realized.
The technical object of the present invention is achieved by the following method:
a composite coagulant and a preparation method thereof are carried out according to the following steps:
step 1, dripping a ceric ammonium nitrate aqueous solution and a dimethyl diallyl ammonium chloride aqueous solution into an acetic acid solution of chitosan in an inert protective gas atmosphere, and carrying out a grafting reaction under heating and stirring to graft dimethyl diallyl ammonium chloride onto the chitosan, wherein the chitosan and the dimethyl diallyl ammonium chloride are in equal mass ratio, and the mass ratio of the ceric ammonium nitrate to the chitosan is (1-5): 65
The chitosan has a number average molecular weight of 1000 to 50000, preferably 10000 to 30000.
In step 1, heating is carried out by adopting water bath, and the reaction temperature is 80-90 ℃.
In step 1, the inert shielding gas is nitrogen, helium or argon.
In the step 1, 1-2 wt% of acetic acid aqueous solution is adopted to dissolve chitosan.
In the step 1, the concentration of the ammonium cerium nitrate aqueous solution is 0.055 mol/L; the mass percent of the dimethyl diallyl ammonium chloride aqueous solution is 60 wt%.
In step 1, the mass ratio of ammonium ceric nitrate to chitosan is (1-3): 65.
in the step 1, the ammonium ceric nitrate aqueous solution and the dimethyl diallyl ammonium chloride aqueous solution are dropwise added into the acetic acid solution of the chitosan at a constant speed for 10-30 min, and the reaction is continued for 2-4 h after the dropwise addition is finished.
In step 1, the stirring speed is 100-300 rpm.
And 2, placing the grafted product obtained in the step 1 into an aqueous solution of polyaluminum ferric chloride, heating, stirring and mixing, and drying to obtain solid particles, namely the composite coagulant, wherein the mixing ratio (namely the mass ratio) of the polyaluminum ferric chloride to the grafted product is (10-20): 1.
in step 2, the mass percentage of the polyaluminum ferric chloride in the aqueous solution of the polyaluminum ferric chloride is 10 wt%.
In step 2, the mass ratio of the polyaluminum ferric chloride to the grafting product is (15-20): 1.
in step 2, the reaction temperature is 20 to 40 degrees Celsius, preferably 30 to 40 degrees Celsius.
In step 2, the reaction time is 1 to 5 hours, preferably 2 to 5 hours.
In step 2, the stirring speed is 100-300 rpm.
Moreover, the system after the reaction in step 1 is separated and purified as follows: cooling the solution obtained in the step 1, adding a 5% NaOH aqueous solution in percentage by mass, adjusting the pH value to 10-12, and precipitating the graft copolymer and the residual chitosan and dimethyl diallyl ammonium chloride homopolymer as a jelly; then stirring the colloidal precipitate, placing the system in a constant-temperature shaking table, oscillating at 200rpm for 20-36 h, removing residual dimethyl diallyl ammonium chloride homopolymer, filtering a crude product, and drying in vacuum; and soaking the dried product in dilute hydrochloric acid at 60 ℃, preserving heat, stirring for 20-36 h, removing residual chitosan, filtering, and drying in vacuum to constant weight to obtain a purified grafting product.
The compound coagulant of the invention is applied to the treatment of secondary effluent of sewage plants.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention compounds the high molecular organic matter on the basis of the high molecular coagulant polymeric aluminum ferric chloride. The surface of the compounded coagulant is loose and porous, and the organic coagulant is compounded, so that the effects of net catching, rolling and sweeping and adsorption bridging are enhanced, colloidal particles and suspended matter charges in water can be effectively neutralized, the electric potential of a double electric layer is reduced, alumen ustum particles formed after coagulation are large in granularity and easy to settle, and compared with the method of independently using polyaluminium ferric chloride, the composite coagulant has a better coagulation effect and a better pollutant removal effect.
(2) The compound coagulant has good effect of removing pollutants in secondary effluent, and the removal rates of turbidity and total phosphorus can respectively reach 92% and 56.3%.
Detailed Description
The present invention will be described in further detail with reference to examples. Dimethyldiallylammonium chloride was purchased from the manufacturer Tianjin Kalmatt, molecular weight was 161.67, purity was 60%; ammonium cerium nitrate was purchased from manufacturer Tianjin Kalmate, molecular weight was 548.22, purity was analytically pure; the polyaluminum ferric chloride is purchased from the manufacturers of Henan scientific, the aluminum chloride content is more than 29 percent, the ferric chloride content is 3 to 5 percent, and the basicity is 65 to 92 percent; the chitosan is purchased from Tianjin Mokmann of manufacturers, the purity is superior pure, and the number average molecular weight is 10000-30000.
Example 1: composite coagulant and preparation method thereof
(1) Grafting reaction: weighing dried chitosan in a triangular flask, and weighing 1 wt% acetic acid aqueous solution in percentage by mass to dissolve the chitosan. Then under the conditions of water bath at 90 ℃, nitrogen protection and stirring at 150 r/min, dropwise adding 0.055mol/L cerium ammonium acid aqueous solution and 60% dimethyl diallyl ammonium chloride aqueous solution in percentage by mass into the acetic acid solution of chitosan at a constant speed to perform grafting reaction, wherein the weight ratio of cerium ammonium nitrate: and (3) chitosan: the mass ratio of the dimethyl diallyl ammonium chloride is 3: 65: 65, the time for dripping is 20min, and the reaction lasts for 3h after the dripping is finished.
(2) Separation and purification: after cooling the solution of step (1), 5% by weight aqueous NaOH solution was added to adjust the pH to 11, whereupon the graft copolymer precipitated as a gum with the residual chitosan and dimethyldiallylammonium chloride homopolymer. The colloidal precipitate was then stirred out and the system was placed in a constant temperature shaker at 200rpm for 24h to remove residual dimethyldiallylammonium chloride homopolymer. The crude product was then filtered and dried in vacuo. Soaking the dried product in dilute hydrochloric acid at 60 deg.c, stirring for 20 hr to eliminate chitosan, filtering and vacuum drying to constant weight to obtain the purified grafting product.
(3) Carrying out composite reaction: and (3) placing the grafted product obtained in the step (2) into a polymeric aluminum ferric chloride aqueous solution (the mass percent of the polymeric aluminum ferric chloride is 10 wt%), heating, stirring and mixing, and drying to obtain solid particles, namely the composite coagulant, wherein the mass ratio of the polymeric aluminum ferric chloride to the grafted product is 20: 1, heating, stirring and mixing for 2 hours at the temperature of 30 ℃, wherein the stirring speed is 150 revolutions per minute, and drying to obtain solid particles, namely the composite coagulant.
The prepared composite coagulant treats the secondary effluent with turbidity of 6.34NTU and total phosphorus of 0.9mg/L respectively, and when the addition amount is 30mg/L, the removal rates of the two are respectively 92% and 56.3% after 20min of coagulating sedimentation.
Example 2: composite coagulant and preparation method thereof
(1) Grafting reaction: weighing dried chitosan in a triangular flask, and weighing 2 wt% acetic acid aqueous solution in percentage by mass to dissolve the chitosan. Then under the conditions of water bath at 80 ℃, nitrogen protection and stirring at 150 r/min, dropwise adding 0.055mol/L cerium ammonium acid aqueous solution and 60% dimethyl diallyl ammonium chloride aqueous solution in percentage by mass into the acetic acid solution of chitosan at a constant speed to perform grafting reaction, wherein the weight ratio of cerium ammonium nitrate: and (3) chitosan: the mass ratio of the dimethyl diallyl ammonium chloride is 5: 65: 65, the time for dripping is 20min, and the reaction lasts for 2h after the dripping is finished.
(2) Separation and purification: and (2) cooling the solution obtained in the step (1), adding a 5 mass percent NaOH aqueous solution to adjust the pH value to 10, and precipitating the graft copolymer and residual chitosan and dimethyl diallyl ammonium chloride homopolymer as a jelly. The colloidal precipitate was then stirred out and the system was placed in a constant temperature shaker at 200rpm for 20h to remove residual dimethyldiallylammonium chloride homopolymer. The crude product was then filtered and dried in vacuo. Soaking the dried product in dilute hydrochloric acid at 60 deg.c, stirring for 24 hr to eliminate chitosan, filtering and vacuum drying to constant weight to obtain the purified grafting product.
(3) Carrying out composite reaction: and (3) placing the grafted product obtained in the step (2) into a polymeric aluminum ferric chloride aqueous solution (the mass percent of the polymeric aluminum ferric chloride is 10 wt%), heating, stirring and mixing, and drying to obtain solid particles, namely the composite coagulant, wherein the mass ratio of the polymeric aluminum ferric chloride to the grafted product is 15: 1, heating, stirring and mixing for 5 hours at the temperature of 20 ℃, wherein the stirring speed is 150 revolutions per minute, and drying to obtain solid particles, namely the composite coagulant.
The prepared composite coagulant treats the secondary effluent with turbidity of 6.34NTU and total phosphorus of 0.9mg/L respectively, and when the addition amount is 30mg/L, the removal rates of the two are 90.1 percent and 49.2 percent respectively after 20min of coagulating sedimentation.
Example 3: composite coagulant and preparation method thereof
(1) Grafting reaction: weighing dried chitosan in a triangular flask, and weighing 1 wt% acetic acid aqueous solution in percentage by mass to dissolve the chitosan. Then under the conditions of water bath at 85 ℃, nitrogen protection and stirring at 150 r/min, dropwise adding 0.055mol/L aqueous solution of ammonium ceric acid and 60% aqueous solution of ammonium dimethyldiallylammonium chloride in percentage by mass into the acetic acid solution of chitosan at a constant speed to perform grafting reaction, wherein the weight ratio of the ammonium ceric nitrate: and (3) chitosan: the mass ratio of the dimethyl diallyl ammonium chloride is 1: 65: 65, the time for dripping is 20min, and the reaction lasts for 5h after the dripping is finished.
(2) Separation and purification: after cooling the solution of step (1), 5% by weight aqueous NaOH solution was added to adjust the pH to 12, at which time the graft copolymer precipitated as a gum with the residual chitosan and dimethyldiallylammonium chloride homopolymer. The colloidal precipitate was then stirred out and the system was placed in a constant temperature shaker at 200rpm for 36h to remove residual dimethyldiallylammonium chloride homopolymer. The crude product was then filtered and dried in vacuo. Soaking the dried product in dilute hydrochloric acid at 60 deg.c, maintaining the temperature and stirring for 36 hr to eliminate chitosan, filtering and vacuum drying to constant weight to obtain the purified grafting product.
(3) Carrying out composite reaction: and (3) placing the grafted product obtained in the step (2) into a polymeric aluminum ferric chloride aqueous solution (the mass percent of the polymeric aluminum ferric chloride is 10 wt%), heating, stirring and mixing, and drying to obtain solid particles, namely the composite coagulant, wherein the mass ratio of the polymeric aluminum ferric chloride to the grafted product is 10: 1, heating, stirring and mixing for 1h at the temperature of 40 ℃, wherein the stirring speed is 150 revolutions per minute, and drying to obtain solid particles, namely the composite coagulant.
The prepared composite coagulant treats the secondary effluent with turbidity of 6.34NTU and total phosphorus of 0.9mg/L respectively, and when the addition amount is 30mg/L, the removal rates of the two are 83.9 percent and 41.2 percent respectively after 20min of coagulating sedimentation.
The preparation of the composite coagulant can be realized by adjusting the process parameters according to the content of the invention, the performance of the composite coagulant is basically consistent with that of the invention through tests, the coagulation effect can be effectively enhanced after the composite organic coagulant is added into the secondary effluent, and after the composite coagulant is added and stirred, large alum floc can be formed in the sewage and rapidly settled, so that the turbidity and the total phosphorus in the secondary effluent can be effectively removed. The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. The composite coagulant is characterized by comprising the following steps:
step 1, dripping a ceric ammonium nitrate aqueous solution and a dimethyl diallyl ammonium chloride aqueous solution into an acetic acid solution of chitosan in an inert protective gas atmosphere, and carrying out a grafting reaction under heating and stirring to graft dimethyl diallyl ammonium chloride onto the chitosan, wherein the chitosan and the dimethyl diallyl ammonium chloride are in equal mass ratio, and the mass ratio of the ceric ammonium nitrate to the chitosan is (1-5): 65, the number average molecular weight of the chitosan is 1000-50000;
and 2, placing the grafted product obtained in the step 1 into an aqueous solution of polyaluminum ferric chloride, heating, stirring and mixing, and drying to obtain solid particles, namely the composite coagulant, wherein the mass ratio of the polyaluminum ferric chloride to the grafted product is (10-20): 1.
2. the composite coagulant according to claim 1, wherein in step 1, a water bath is used for heating, and the reaction temperature is 80-90 ℃; the inert protective gas is nitrogen, helium or argon; the stirring speed is 100-300 r/min.
3. The composite coagulant according to claim 1, wherein in step 1, 1-2 wt% acetic acid aqueous solution is used to dissolve chitosan; the concentration of the ammonium ceric nitrate aqueous solution is 0.055 mol/L; the mass percent of the dimethyl diallyl ammonium chloride aqueous solution is 60 wt%; the mass ratio of the ammonium ceric nitrate to the chitosan is (1-3): 65; the chitosan has a number average molecular weight of 10000-30000.
4. The composite coagulant of claim 1, wherein in step 1, the ammonium cerium nitrate aqueous solution and the dimethyldiallylammonium chloride aqueous solution are added dropwise into the acetic acid solution of chitosan at a constant speed for 10-30 min, and the reaction is continued for 2-4 hours after the dropwise addition.
5. A composite coagulant according to claim 1 wherein in step 2 the mass percent of polyaluminum ferric chloride in the aqueous solution of polyaluminum ferric chloride is 10 wt%. (ii) a The mass ratio of the polymeric aluminum ferric chloride to the grafting product is (15-20): 1; the reaction temperature is 20-40 ℃, preferably 30-40 ℃; the reaction time is from 1 to 5 hours, preferably from 2 to 5 hours; the stirring speed is 100-300 r/min.
6. The preparation method of the composite coagulant is characterized by comprising the following steps of:
step 1, dripping a ceric ammonium nitrate aqueous solution and a dimethyl diallyl ammonium chloride aqueous solution into an acetic acid solution of chitosan in an inert protective gas atmosphere, and carrying out a grafting reaction under heating and stirring to graft dimethyl diallyl ammonium chloride onto the chitosan, wherein the chitosan and the dimethyl diallyl ammonium chloride are in equal mass ratio, and the mass ratio of the ceric ammonium nitrate to the chitosan is (1-5): 65, the number average molecular weight of the chitosan is 1000-50000;
and 2, placing the grafted product obtained in the step 1 into an aqueous solution of polyaluminum ferric chloride, heating, stirring and mixing, and drying to obtain solid particles, namely the composite coagulant, wherein the mass ratio of the polyaluminum ferric chloride to the grafted product is (10-20): 1.
7. the method for preparing a composite coagulant according to claim 6, characterized in that in the step 1, a water bath is adopted for heating, and the reaction temperature is 80-90 ℃; the inert protective gas is nitrogen, helium or argon; the stirring speed is 100-300 r/min; dissolving chitosan by adopting an acetic acid water solution with the mass percent of 1-2 wt%; the concentration of the ammonium ceric nitrate aqueous solution is 0.055 mol/L; the mass percent of the dimethyl diallyl ammonium chloride aqueous solution is 60 wt%; the mass ratio of the ammonium ceric nitrate to the chitosan is (1-3): 65; the number average molecular weight of the chitosan is 10000-30000; dropping ammonium ceric nitrate solution and dimethyl diallyl ammonium chloride solution into acetic acid solution of chitosan at constant speed for 10-30 min, and reacting for 2-4 hr.
8. The method for preparing a composite coagulant according to claim 6, wherein in the step 2, the mass percent of the polyaluminum ferric chloride in the aqueous solution of the polyaluminum ferric chloride is 10 wt%. (ii) a The mass ratio of the polymeric aluminum ferric chloride to the grafting product is (15-20): 1; the reaction temperature is 20-40 ℃, preferably 30-40 ℃; the reaction time is from 1 to 5 hours, preferably from 2 to 5 hours; the stirring speed is 100-300 r/min.
9. The method for preparing a composite coagulant according to claim 6, wherein the system after the reaction in the step 1 is separated and purified as follows: cooling the solution obtained in the step 1, adding a 5% NaOH aqueous solution in percentage by mass, adjusting the pH value to 10-12, and precipitating the graft copolymer and the residual chitosan and dimethyl diallyl ammonium chloride homopolymer as a jelly; then stirring the colloidal precipitate, placing the system in a constant-temperature shaking table, oscillating at 200rpm for 20-36 h, removing residual dimethyl diallyl ammonium chloride homopolymer, filtering a crude product, and drying in vacuum; and soaking the dried product in dilute hydrochloric acid at 60 ℃, preserving heat, stirring for 20-36 h, removing residual chitosan, filtering, and drying in vacuum to constant weight to obtain a purified grafting product.
10. Use of a complex coagulant according to any one of claims 1 to 5 for the treatment of secondary effluent from a sewage plant.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1236748A1 (en) * | 2001-02-22 | 2002-09-04 | Ecole Polytechnique Federale De Lausanne | Polymer flocculents and preparation thereof |
| CN108585155A (en) * | 2018-03-30 | 2018-09-28 | 浙江大学 | Polyaluminum ferric chloride-（Chitose-acrylic amide-magnesium lignosulfonate graft copolymer）Composite flocculation agent and preparation method thereof |
| CN109293796A (en) * | 2018-09-11 | 2019-02-01 | 北京华城新创环境科技有限公司 | A kind of preparation method and applications of n-trimethyl chitosan chloride |
| CN109319908A (en) * | 2018-11-07 | 2019-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Modification of chitosan-sodium alginate composite flocculation agent preparation method and products thereof and application |
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2020
- 2020-10-16 CN CN202011112804.2A patent/CN114380373A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1236748A1 (en) * | 2001-02-22 | 2002-09-04 | Ecole Polytechnique Federale De Lausanne | Polymer flocculents and preparation thereof |
| CN108585155A (en) * | 2018-03-30 | 2018-09-28 | 浙江大学 | Polyaluminum ferric chloride-（Chitose-acrylic amide-magnesium lignosulfonate graft copolymer）Composite flocculation agent and preparation method thereof |
| CN109293796A (en) * | 2018-09-11 | 2019-02-01 | 北京华城新创环境科技有限公司 | A kind of preparation method and applications of n-trimethyl chitosan chloride |
| CN109319908A (en) * | 2018-11-07 | 2019-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Modification of chitosan-sodium alginate composite flocculation agent preparation method and products thereof and application |
Non-Patent Citations (1)
| Title |
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| 程建华，等: "壳聚糖接枝共聚高分子絮凝剂CAS 的合成", 工业水处理, vol. 28, no. 9, pages 30 - 33 * |
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