CN105645543A - Polysilicate aluminum ferric flocculant and preparation method thereof - Google Patents
Polysilicate aluminum ferric flocculant and preparation method thereof Download PDFInfo
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- CN105645543A CN105645543A CN201610130079.9A CN201610130079A CN105645543A CN 105645543 A CN105645543 A CN 105645543A CN 201610130079 A CN201610130079 A CN 201610130079A CN 105645543 A CN105645543 A CN 105645543A
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention relates to polysilicate aluminum ferric flocculant and a preparation method thereof. The preparation method includes: well mixing a silicon aluminum source, alkali carbonate and calcium carbonate, performing heating reaction, and naturally cooling to obtain a first product; placing the first product into an acid solution for acidification and ultrasonic treatment to obtain a second product; adding ferric salt into the second product to obtain a solid-liquid mixture, adjusting the pH of the upper solution of the solid-liquid mixture to 3.5-5.5, and standing for 6-48 hours to obtain the polysilicate aluminum ferric flocculant. The preparation method has the advantages that the waste fly ash, silicon aluminum residues and red mud are turned into treasure and used as the raw materials to prepare the polysilicate aluminum ferric flocculant; the polysilicate aluminum ferric flocculant prepared by the method has a good flocculation effect on the nitrogenous and phosphorous substances in domestic sewage.
Description
Technical field
The present invention relates to a kind of flocculant, the preparation method being specifically related to a kind of poly silicate aluminium ferric flocculating agent and the poly silicate aluminium ferric flocculating agent prepared by the method.
Background technology
Water is to be distributed the most extensively and the most valuable natural resources on the earth. It maintains the vital movement of all living things, is also the indispensable key factor of human social. 3/4ths of earth surface are awash, and the mankind are but only with wherein fresh water less than 1%. In recent years; quick increase along with socioeconomic fast development and population; make people's lives, industrial and agricultural production and urban ecology that the demand of water resource is increasing; in addition the significantly discharge of sanitary sewage and industrial wastewater; cause that water resources crisis phenomenon occurs again and again; Water-environment Ecological System function worsens increasingly, and advance and development to human society constitute serious threat. China is the country of a severe drought, hydropenia, freshwater resources total amount is 2.8 tcms, account for the 6% of whole world freshwater resources, be only second to Brazil, Russian and Canadian, occupy the 4th, the world, but only occupy 2200 cubic metres per capita, be only the world per capita the 1/4 of fresh water occupancy volume, the U.S. 1/5, rank 121 in the world, be one of 13 countries that water resource is the poorest per capita in the whole world. After deducting the flood, the runoff that are difficult by and being dispersed in groundwater resources from far-off regions, the available freshwater resources amount of reality of China is then less, and its distributed pole is unbalanced. Meanwhile, along with the development of science and technology, a large amount of industrial wastewater, sanitary sewage, agriculture backwater water, the unprocessed direct discharge of wherein most are created. Monitoring according to environment department, cities and towns, the whole nation have at least that 100,000,000 tons of sewage is unprocessed just directly to be discharged every day. In the seven big water systems of the whole nation, the section water quality of more than half is contaminated, the water body in the whole nation 1/3 is unsuitable for Fish Survival, the water body of 1/4 is unsuitable for irrigating, the urban waters of 90% is seriously polluted, the water source, cities and towns of 50% does not meet drinking water standard, the water source of 40% oneself can not drink, the 60%-70% of the total water deficit in Shelter in South China Cities due to water pollute cause. Increasingly severe by water situation, water contamination accident frequently occurs, own through having had a strong impact on the productive life of our people, seriously hinders the progress of expanding economy and science and technology, therefore, administers water and pollutes, and solution is lived, industrial water problem is extremely urgent.
Chinese patent CN101327975 discloses a kind of method preparing microbial flocculant, and the method adopts Dell's Ford acidovorax facilis to prepare into microbial flocculant by the preparation of fluid medium, the fermentation culture of strain, the preparation of flocculant semifinished product with the preparation process of flocculant highly finished product as the strain source preparing microbial flocculant. This invention is domestic find that Dell Ford acidovorax facilis can produce that flocculating property is stable, the good microbial flocculant of flocculating effect first, the flocculant filtered out has the good characteristics such as flocculation activity height, consumption is few, fermentation time is short, extraction process is simple, can be substantially reduced production cost; The method that this bacterium produces flocculant is simple, easy; Actual waste water being processed and experiments show that, after the application of this flocculant, flocculating effect is more satisfactory.
The preparation method that Chinese patent CN101693561A discloses a kind of composite flocculant, preparation process is: prepare bioflocculation agent solution; By composite to bioflocculation agent solution and inorganic flocculating agent solution: PAC, PFS or both mixture are dissolved in deionized water and obtain inorganic flocculating agent, by biological flocculant and inorganic flocculating agent by volume 3: 10��15 ratio mixing; Namely composite flocculant is obtained. The method that composite flocculant is prepared in this invention offer, the composite flocculant produced by the method both can obtain high flocculating rate and few total dosage, the amount of remaining metal ions in water body can be reduced again, overcome inorganic flocculating agent to process the weak point in using at water.
Traditional inorganic and organic flocculant needs by some specific raw material in preparation, and cost of material accounts for larger proportion in preparation cost.
Summary of the invention
In order to solve the problems referred to above that prior art exists, the invention provides the preparation method of a kind of poly silicate aluminium ferric flocculating agent and the poly silicate aluminium ferric flocculating agent prepared by the method, adopt poly silicate aluminium ferric flocculating agent prepared by the method for the present invention to nitrogenous in sanitary sewage and have good flocculation containing Phosphorous species.
The technical solution adopted in the present invention is:
The preparation method that the present invention provides a kind of poly silicate aluminium ferric flocculating agent, the method includes: be 100:(5-30 according to mass ratio): (0.1-1), by after silicon and aluminum source, alkali carbonate and calcium carbonate mix homogeneously, after 800-950 degrees Centigrade reacts 1-5 hour, natural cooling obtains the first product; Wherein, described silicon and aluminum source is at least one in flyash, sial slag and red mud, and described alkali carbonate is sodium carbonate and potassium carbonate; Be 1:(2-10 according to solid-liquid mass ratio) described first product put in the acid solution that mass concentration is 20%-40% carry out acidifying, under 70-100 degree Celsius ultrasonic 0.5-3 hour the second product; Wherein, the acid in described acid solution is hydrochloric acid, nitric acid or sulphuric acid; It is (5-20) according to the mass ratio of iron salt and silicon and aluminum source: 100 to second products add iron salt and obtains solidliquid mixture, the pH value regulating solidliquid mixture solution at the middle and upper levels is 3.5-5.5, stand 6-48 hour at 20-40 degree Celsius, obtain poly silicate aluminium ferric flocculating agent.
Preferably, it is 100:(5-15 according to mass ratio): after silicon and aluminum source is mixed homogeneously by (0.1-0.5) with alkali carbonate and calcium carbonate, after 850-900 degrees Centigrade reacts 2-4 hour, natural cooling obtains the first product.
Preferably, described reacting by heating includes: obtain Primary product by reacting natural cooling after 1-2 hour at 800-950 degrees Centigrade after described silicon and aluminum source, alkali carbonate and calcium carbonate mix homogeneously;After Primary product is ground, stirred, after 800-950 degrees Centigrade reacts 1-2, natural cooling obtains the first product.
Preferably, the acid in described acid solution also includes acetic acid or ethanedioic acid.
Preferably, be 1:(2-5 according to solid-liquid mass ratio) described first product put in the acid solution that mass concentration is 25%-35% carry out acidifying, under 80-95 degree Celsius ultrasonic 1-2 hour the second product.
Preferably, described ultrasonic frequency is 20-60KHz.
Preferably, described iron salt is iron chloride, ferric nitrate or iron sulfate.
Preferably, it is (5-10) according to the mass ratio of iron salt and flyash: 100 to second products add iron salt and obtains solidliquid mixture, the pH value regulating solidliquid mixture solution at the middle and upper levels is 4-5, stands 8-24 hour at 25-35 degree Celsius, obtains described poly silicate aluminium ferric flocculating agent.
Preferably, it is adjusted by adding hydrochloric acid solution that mass concentration is 10-30% or sulfuric acid solution during the pH value of described adjustment solidliquid mixture solution at the middle and upper levels.
Prepared by method made above poly silicate aluminium ferric flocculating agent.
The invention have the benefit that
One, prepared by the present invention, poly silicate aluminium ferric flocculating agent to nitrogenous in sanitary sewage and had good flocculation containing Phosphorous species, and the sanitary sewage processed through the poly silicate aluminium ferric flocculating agent of the present invention is obtained in that significantly high nitrogen removal rate and total tp removal rate;
Its two, flyash, sial slag and red mud are successfully prepared poly silicate aluminium ferric flocculating agent as reaction raw materials by the preparation method of the present invention, are turned waste into wealth by refuse;
Its three, the present invention adopts flyash, sial slag and red mud as preparing raw material, greatly reduces production cost, and the preparation method of the present invention is simple, is suitable for industrialized production.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly, technical scheme will be described in detail below. Obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiments. Based on the embodiment in the present invention, other embodiments all that those of ordinary skill in the art are obtained under the premise not making creative work, broadly fall into the scope that the present invention protects.
The preparation method that the present invention provides a kind of poly silicate aluminium ferric flocculating agent, the method includes: be 100:(5-30 according to mass ratio): (0.1-1), by after silicon and aluminum source, alkali carbonate and calcium carbonate mix homogeneously, after 800-950 degrees Centigrade reacts 1-5 hour, natural cooling obtains the first product; Wherein, described silicon and aluminum source is at least one in flyash, sial slag and red mud, and described alkali carbonate is sodium carbonate and potassium carbonate; Be 1:(2-10 according to solid-liquid mass ratio) described first product put in the acid solution that mass concentration is 20%-40% carry out acidifying, under 70-100 degree Celsius ultrasonic 0.5-3 hour the second product; Wherein, the acid in described acid solution is hydrochloric acid, nitric acid or sulphuric acid; It is (5-20) according to the mass ratio of iron salt and silicon and aluminum source: 100 to second products add iron salt and obtains solidliquid mixture, the pH value regulating solidliquid mixture solution at the middle and upper levels is 3.5-5.5, stand 6-48 hour at 20-40 degree Celsius, obtain poly silicate aluminium ferric flocculating agent.
According to the present invention, can be 100:(5-15 according to mass ratio): after silicon and aluminum source is mixed homogeneously by (0.1-0.5) with alkali carbonate and calcium carbonate, after 850-900 degrees Centigrade reacts 2-4 hour, natural cooling obtains the first product.
According to the present invention, described reacting by heating includes: can obtain Primary product by reacting natural cooling after 1-2 hour at 800-950 degrees Centigrade after described silicon and aluminum source, alkali carbonate and calcium carbonate mix homogeneously; After Primary product is ground, stirred, after 800-950 degrees Centigrade reacts 1-2, natural cooling obtains the first product.
According to the present invention, the acid in described acid solution can also include acetic acid or ethanedioic acid.
According to the present invention it is possible to be 1:(2-5 according to solid-liquid mass ratio) described first product put in the acid solution that mass concentration is 25%-35% carry out acidifying, under 80-95 degree Celsius ultrasonic 1-2 hour the second product.
According to the present invention, described ultrasonic frequency can be 20-60KHz.
According to the present invention, described iron salt can be iron chloride, ferric nitrate or iron sulfate.
According to the present invention, can be (5-10) according to the mass ratio of iron salt and flyash: 100 to second products add iron salt and obtains solidliquid mixture, the pH value regulating solidliquid mixture solution at the middle and upper levels can be 4-5, stand 8-24 hour at 25-35 degree Celsius, obtain described poly silicate aluminium ferric flocculating agent.
According to the present invention, can be adjusted by adding hydrochloric acid solution that mass concentration is 10-30% or sulfuric acid solution during the pH value of described adjustment solidliquid mixture solution at the middle and upper levels.
The present invention also provides for the poly silicate aluminium ferric flocculating agent prepared by preparation in accordance with the present invention.
Further illustrate the present invention following by embodiment, but the present invention is not therefore subject to any restriction.
If no special instructions, instrument of the present invention and reagent are and are purchased, and the commodity of different brands do not affect specifically used.
The mensuration of total nitrogen adopts alkaline chitinase to clear up ultraviolet spectrophotometry; Total phosphorus yield adopts Reduction with Stannous Chloride molybdenum blue method; The mensuration of ammonia nitrogen adopts Nessler's reagent photometer.
Embodiment 1
Being 100:5:0.1 by after flyash, sodium carbonate and calcium carbonate mix homogeneously according to mass ratio, after 800 degrees Centigrade react 1 hour, natural cooling obtains the first product; Be that described first product is put in the hydrochloric acid solution that mass concentration is 20% and carried out acidifying by 1:2 according to solid-liquid mass ratio, under 70 degrees Celsius, with frequency ultrasound 0.5-3 hour of 20KHz the second product; It is that 5:100 obtains solidliquid mixture to addition iron chloride in the second product according to the mass ratio of iron salt and flyash, the pH value regulating solidliquid mixture solution at the middle and upper levels by adding the hydrochloric acid solution that mass concentration is 10% is 3.5, stand 6 hours at 20 degrees Celsius, obtain poly silicate aluminium ferric flocculating agent JAT-1.
Embodiment 2
It is that 100:30:1 is by after sial slag, potassium carbonate and calcium carbonate mix homogeneously according to mass ratio, after 950 degrees Centigrade react 2 hours, natural cooling obtains Primary product, and after Primary product is ground, stirred, after 950 degrees Centigrade react 3 hours, natural cooling obtains the first product; Be that described first product is put in the salpeter solution that mass concentration is 40% and carried out acidifying by 1:10 according to solid-liquid mass ratio, under 100 degrees Celsius with ultrasonic 3 hours of 60KHz the second product; It is that 20:100 obtains solidliquid mixture to addition ferric nitrate in the second product according to the mass ratio of iron salt and flyash, the pH value regulating solidliquid mixture solution at the middle and upper levels by adding the sulfuric acid solution that mass concentration is 30% is 5.5, stand 48 hours at 40 degrees Celsius, obtain poly silicate aluminium ferric flocculating agent JAT-2.
Embodiment 3
Being 100:20:0.5 by after red mud, potassium carbonate and calcium carbonate mix homogeneously according to mass ratio, after 900 degrees Centigrade react 3 hours, natural cooling obtains the first product;Be that described first product is put in the sulfuric acid solution that mass concentration is 30% and carried out acidifying by 1:6 according to solid-liquid mass ratio, under 85 degrees Celsius of lower 40KHz ultrasonic 2 hours the second product; It is that 12:100 obtains solidliquid mixture to addition iron sulfate in the second product according to the mass ratio of iron salt and flyash, the pH value regulating solidliquid mixture solution at the middle and upper levels by adding the hydrochloric acid solution that mass concentration is 20% is 4.5, stand 30 hours at 30 degrees Celsius, obtain poly silicate aluminium ferric flocculating agent JAT-3.
Application Example 1
Take 200mL sanitary wastewater, measure total nitrogen content is 33.01mg/L, total phosphorus content is 1.08mg/L; The homemade poly silicate aluminium ferric flocculating agent JAT-1 of 5ml is added in 200mL sanitary wastewater, when low whipping speed is 100r/min, stir 10min, after staticly settling 30min, take total nitrogen content and the total phosphorus content of the waste water that supernatant mensuration processed, calculate nitrogen removal rate and total tp removal rate.
Application Example 2 is identical with Application Example 1 with the method for testing of Application Example 3, and the poly silicate aluminium ferric flocculating agent simply used asks JAT-2 and JAT-3 respectively.
The nitrogen removal rate of Application Example 1-3 and total tp removal rate are in Table 1.
Table 1
| Nitrogen removal rate | Total tp removal rate | |
| Application Example 1 | 82% | 95% |
| Application Example 2 | 86% | 92% |
| Application Example 3 | 79% | 97% |
From embodiment 1-3 and Application Example 1-3, poly silicate aluminium ferric flocculating agent prepared by the inventive method is to the nitrogenous class material of sanitary sewage and has good flocculation containing Phosphorous species, and the sanitary sewage that the poly silicate aluminium ferric flocculating agent through the present invention processed is obtained in that significantly high nitrogen removal rate and total tp removal rate.
Claims (10)
1. the preparation method of a poly silicate aluminium ferric flocculating agent, it is characterised in that the method includes:
It is 100:(5-30 according to mass ratio): (0.1-1), by after silicon and aluminum source, alkali carbonate and calcium carbonate mix homogeneously, after 800-950 degrees Centigrade reacts 1-5 hour, natural cooling obtains the first product; Wherein, described silicon and aluminum source is at least one in flyash, sial slag and red mud, and described alkali carbonate is sodium carbonate and potassium carbonate;
Be 1:(2-10 according to solid-liquid mass ratio) described first product put in the acid solution that mass concentration is 20%-40% carry out acidifying, under 70-100 degree Celsius ultrasonic 0.5-3 hour the second product; Wherein, the acid in described acid solution is hydrochloric acid, nitric acid or sulphuric acid;
It is (5-20) according to the mass ratio of iron salt and silicon and aluminum source: 100 to second products add iron salt and obtains solidliquid mixture, the pH value regulating solidliquid mixture solution at the middle and upper levels is 3.5-5.5, stand 6-48 hour at 20-40 degree Celsius, obtain poly silicate aluminium ferric flocculating agent.
2. preparation method according to claim 1, it is characterized in that, it is 100:(5-15 according to mass ratio): after silicon and aluminum source is mixed homogeneously by (0.1-0.5) with alkali carbonate and calcium carbonate, after 850-900 degrees Centigrade reacts 2-4 hour, natural cooling obtains the first product.
3. preparation method according to claim 1, it is characterised in that described reacting by heating includes: obtain Primary product by reacting natural cooling after 1-2 hour at 800-950 degrees Centigrade after described silicon and aluminum source, alkali carbonate and calcium carbonate mix homogeneously; After Primary product is ground, stirred, after 800-950 degrees Centigrade reacts 1-2, natural cooling obtains the first product.
4. preparation method according to claim 1, it is characterised in that the acid in described acid solution also includes acetic acid or ethanedioic acid.
5. the preparation method according to claim 1 and claim 2, it is characterized in that, be 1:(2-5 according to solid-liquid mass ratio) described first product put in the acid solution that mass concentration is 25%-35% carry out acidifying, under 80-95 degree Celsius ultrasonic 1-2 hour the second product.
6. preparation method according to claim 1, it is characterised in that described ultrasonic frequency is 20-60KHz.
7. preparation method according to claim 1, it is characterised in that described iron salt is iron chloride, ferric nitrate or iron sulfate.
8. preparation method according to claim 1, it is characterized in that, it is (5-10) according to the mass ratio of iron salt and flyash: 100 to second products add iron salt and obtains solidliquid mixture, the pH value regulating solidliquid mixture solution at the middle and upper levels is 4-5, stand 8-24 hour at 25-35 degree Celsius, obtain described poly silicate aluminium ferric flocculating agent.
9. preparation method according to claim 1, it is characterised in that be adjusted by adding hydrochloric acid solution that mass concentration is 10-30% or sulfuric acid solution during the pH value of described adjustment solidliquid mixture solution at the middle and upper levels.
10. the poly silicate aluminium ferric flocculating agent prepared by preparation method described in any one in claim 1-9.
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| CN106315603A (en) * | 2016-08-04 | 2017-01-11 | 广东紫方环保技术有限公司 | Preparation method of polymeric aluminum ferric silicate |
| CN107934978A (en) * | 2017-10-23 | 2018-04-20 | 昆明理工大学 | A kind of coal ash for manufacturing for inorganic polymer flocculant method |
| CN109809540A (en) * | 2017-11-20 | 2019-05-28 | 临沂大学 | A kind of poly silicate aluminium ferric flocculating agent and preparation method |
| CN109809419A (en) * | 2017-11-20 | 2019-05-28 | 临沂大学 | A method of preparing poly silicate aluminium ferric flocculating agent |
| CN111943336A (en) * | 2020-07-16 | 2020-11-17 | 国家能源集团宁夏煤业有限责任公司 | Method for preparing polysilicate aluminum ferric flocculant, polysilicate aluminum ferric flocculant and application thereof |
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| CN106315603A (en) * | 2016-08-04 | 2017-01-11 | 广东紫方环保技术有限公司 | Preparation method of polymeric aluminum ferric silicate |
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| CN109809419A (en) * | 2017-11-20 | 2019-05-28 | 临沂大学 | A method of preparing poly silicate aluminium ferric flocculating agent |
| CN109809540B (en) * | 2017-11-20 | 2021-11-05 | 临沂大学 | Polysilicate aluminum ferric flocculant and preparation method thereof |
| CN109809419B (en) * | 2017-11-20 | 2022-06-14 | 临沂大学 | Method for preparing polysilicate aluminum ferric flocculant |
| CN111943336A (en) * | 2020-07-16 | 2020-11-17 | 国家能源集团宁夏煤业有限责任公司 | Method for preparing polysilicate aluminum ferric flocculant, polysilicate aluminum ferric flocculant and application thereof |
| CN111943336B (en) * | 2020-07-16 | 2022-08-16 | 国家能源集团宁夏煤业有限责任公司 | Method for preparing polysilicate aluminum ferric flocculant, polysilicate aluminum ferric flocculant and application thereof |
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Application publication date: 20160608 |