CN113651588A - Efficient phosphorus-removing baking-free ceramsite and preparation method and application thereof - Google Patents
Efficient phosphorus-removing baking-free ceramsite and preparation method and application thereof Download PDFInfo
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
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Abstract
The invention discloses a preparation method of high-efficiency phosphorus-removing baking-free ceramsite, which comprises the following steps: pretreating residual sludge and Fenton sludge of a water supply plant, and then uniformly mixing the pretreated residual sludge and Fenton sludge with cement, fly ash and an excitant according to a certain mass ratio; then adding water solution of water glass into the uniformly mixed raw materials, uniformly stirring and granulating to obtain ceramsite raw materials; placing the ceramsite raw material at room temperature for a certain time, and then placing the ceramsite raw material into a sterilization pot for steam curing; naturally air-drying and aging the steamed ceramsite at room temperature; and aging the ceramsite after natural air drying and aging in an oven to obtain the high-efficiency phosphorus-removing non-fired ceramsite mainly comprising Fenton sludge and residual sludge of a water supply plant. The preparation method is simple, the raw materials are cheap and easy to obtain, the equipment investment and the operation cost are low, the prepared non-sintered ceramsite has excellent adsorption effect and strong phosphorus adsorption capacity, can be used as an adsorption material to be applied to a wastewater treatment process, has good mechanical property, and can realize the win-win goal of treating wastes with processes of wastes against one another.
Description
Technical Field
The invention relates to the technical field of water treatment, and particularly relates to high-efficiency phosphorus-removing unfired ceramsite and a preparation method and application thereof.
Background
The Fenton method is a well-known catalytic oxidation reaction, discovered in 1893 by the chemist Fenton HJ. Although the chemical and environmental sciences have long studied this method, its large-scale application in sewage treatment has been less than ten years old. According to the knowledge, the Fenton method advanced treatment process is adopted in several sewage treatment plants with the treatment scale of more than ten thousand tons per day in China at present. The production practice shows that: for the waste water in the general chemical industry park, the waste water can reach the standard stably after the Fenton method advanced treatment, but the problems that appear are that: the amount of sludge produced is too much and the engineering economy is not well tolerated. Taking an actual sewage plant as an example, FeSO is added into effluent after biochemical treatment4The salt content is about 1000mg/L, the theoretical sludge yield is about 5.8 tons/ten thousand tons of water, and the sludge is basically iron compound (hereinafter referred to as iron sludge) and is about five times of the sludge yield of the municipal sewage plant. Therefore, the method for the export and resource utilization of the iron sludge generated in the advanced treatment is researched, and has important significance for reducing the sewage treatment cost and solving the problem of secondary pollution.
At present, an effective treatment method for Fenton sludge is not available, and the Fenton sludge is generally subjected to incineration or landfill treatment after being dried. The Fenton sludge drying after-incineration treatment has high investment and operation cost and complex operation management, waste gas can be generated in the incineration process to pollute the atmosphere, and meanwhile, the Fenton sludge contains a large amount of inorganic matters, has low heat value and is not beneficial to incineration. The problem of Fenton sludge environmental pollution is not fundamentally solved in the landfill after the Fenton sludge is dried, the site which can be used for burying the Fenton sludge at present is gradually reduced, the landfill cost is gradually increased, and sludge leachate pollution and air pollution can be generated in the landfill process.
The residual sludge of the water supply plant is a byproduct generated in the water supply treatment process, mainly consists of a flocculating agent, colloid and organic matters carried in raw water, and is a safe and nontoxic waste proved by a large number of researches. The yield is huge, and according to statistics, the annual discharge amount (water content) of residual mud of water supply plants in China in recent years reaches 55 hundred million m3Wherein more than 80% of the residual sludge of the water supply plant is directly discharged into natural water bodies and urban sewage systems without resource recycling, or is subjected to land filling after dehydration. Along with the growth of population and the enhancement of water supply capacity in China, the yield of residual mud in a water supply plant is in an exponential growth situation, and meanwhile, the environmental protection requirement in China is continuously improved, the urban sewage discharge standard is increasingly strict, and the land resources are increasingly tense. In order to relieve the contradiction between water supply demand and environmental protection, the resource recycling of residual mud in a water supply plant is bound to become an important application demand.
At present, the disposal of sludge in water supply plants mainly focuses on the direct discharge of discharged sludge, the marine abandonment of dewatered sludge cakes, land abandonment, sanitary landfill, the regeneration of aluminum salt and iron salt, land utilization, building material utilization and the like, but has the problems of secondary pollution, high subsequent treatment cost and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the efficient phosphorus removal unfired ceramsite which takes Fenton sludge and residual sludge of a water supply plant as main bodies, and the preparation method and the application thereof. The preparation method disclosed by the invention is simple in process, cheap and easily available in raw materials, low in equipment investment and operation cost, high in porosity and large in specific surface area of the prepared non-sintered ceramsite, high in phosphorus adsorption capacity, good in mechanical property and capable of meeting requirements, can be used as a phosphorus removal adsorption material to be applied to a wastewater treatment process, and is easy to popularize and use.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-efficiency phosphorus-removing unfired ceramsite comprises the following steps:
(1) preparing materials: pretreating residual sludge and Fenton sludge of a water supply plant, and mixing the pretreated residual sludge and Fenton sludge with cement, fly ash and an activator uniformly, wherein the mass ratio of the Fenton sludge to the residual sludge of the water supply plant to the cement to the fly ash to the activator is 5-30%, 30-55%, 10-15%, 10-20% and 2-5%;
(2) and (3) granulation: adding water solution of water glass into the uniformly mixed raw materials, uniformly stirring, and granulating to obtain ceramsite raw material;
(3) steaming: placing the ceramsite raw material at room temperature for a certain time, and then placing the ceramsite raw material into a sterilization pot for steam curing;
(4) aging at room temperature: naturally air-drying and aging the steamed ceramsite at room temperature;
(5) aging in an oven: and aging the ceramsite after natural air drying and aging in an oven to obtain the high-efficiency phosphorus-removing non-fired ceramsite mainly comprising Fenton sludge and residual sludge of a water supply plant.
Preferably, in the step (1), the Fenton sludge is pretreated by drying, crushing, sieving with a 100-mesh sieve, and burning; the pretreatment method of the residual sludge of the water supply plant comprises the steps of drying, crushing and sieving with a 100-mesh sieve.
Preferably, in the step (2), the addition amount of the water glass is 35-40 mL of water and 6-8 g of water glass per 100g of the raw material.
Preferably, the cement is ordinary portland cement; the excitant is a mixture of quicklime and gypsum, and the mass ratio of the quicklime to the gypsum in the mixture is 1-1.5: 1-2.
Preferably, in the step (5), the aging condition in the oven is aging for 1-3 h at 30-60 ℃.
Preferably, in the step (3), the ceramsite raw material is placed at room temperature for 2-3 hours; the steam curing temperature is 70-90 ℃, and the steam curing time is 10-12 h.
Preferably, in the step (4), the natural air-drying and aging time is 1-2 days.
Preferably, the particle size of the prepared high-efficiency phosphorus-removing baking-free ceramsite is 3-6 mm, and the shape of the ceramsite is spherical.
As a general inventive concept, the invention also provides the high-efficiency phosphorus-removing baking-free ceramsite prepared by the preparation method.
As a general inventive concept, the invention also provides the application of the high-efficiency phosphorus-removing baking-free ceramsite in the treatment of phosphorus-containing wastewater.
The beneficial effects produced by the invention are as follows:
(1) the main raw materials of the invention are waste and Fenton sludge of a water supply plant, and other raw material excitants and fly ash are all industrial waste, so the required raw materials are all cheap and easy to obtain; and the prepared ceramsite has high porosity and large specific surface area.
(2) The preparation process is simple, high-temperature roasting furnace with high energy consumption is not needed, and the equipment investment cost and the operation cost are low.
(3) The ceramsite prepared from the residual sludge of the water supply plant and the Fenton sludge can be used as a phosphorus removal adsorption material to be applied to a water treatment process, is favorable for achieving the aim of treating wastes with processes of wastes against one another, and meets the development requirement of circular economy.
Drawings
FIG. 1 is a flow chart of the preparation of the high-efficiency phosphorus-removing unfired ceramsite.
FIG. 2 is a SEM comparison of UCFWTR prepared according to the present invention and UCWTR prepared using a feedwater sludge in a comparative example, in which (a) is an SEM image of UCWTR and (b) is an SEM image of UCFWTR.
FIG. 3 is a FT-IR spectrum of UCFWTR prepared in accordance with the present invention and UCWTR prepared using water plant sludge.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
A preparation method of high-efficiency phosphorus-removing unfired ceramsite comprises the following steps:
(1) pretreatment of raw materials: drying, crushing and grinding residual sludge of a water supply plant at 105 ℃ to 100 meshes, drying, crushing and grinding Fenton sludge at 105 ℃, then firing at 300 ℃, then respectively grinding cement, fly ash and an exciting agent to 100 meshes, and then mixing the treated residual sludge of the water supply plant, Fenton sludge, cement, fly ash and the exciting agent according to a certain mass ratio, wherein the mass ratio of the Fenton sludge is 5-30%, the mass ratio of the residual sludge of the water supply plant is 30-55%, the mass ratio of the cement is 10-15%, the mass ratio of the exciting agent is 2-6%, and the mass ratio of the fly ash is 10-20%;
(2) and (3) granulation: adding water glass aqueous solution into the uniformly mixed raw materials in the step (1), wherein the adding amount of the water glass is that 35-40 mL of water and 6-8 g of water glass are added into each 100g of raw materials, stirring, and then putting into a granulator for granulation to obtain spherical ceramsite raw material with the particle size of 3-6 mm;
(3) steaming: placing the ceramsite raw material at room temperature for 2-3 hours, and then putting the ceramsite raw material into a sterilization pot at the temperature of 80 ℃ for steam curing for 10-12 hours;
(4) aging at room temperature: naturally drying and aging the steamed ceramsite at room temperature for 1-2 days;
(5) aging in an oven: and ageing the ceramsite aged at room temperature in an oven at 30-60 ℃ for 1-3 h to obtain the high-efficiency phosphorus-removing non-fired ceramsite mainly comprising Fenton sludge and residual sludge of a water supply plant, wherein the particle size of the ceramsite is 3-6 mm.
It is worth noting that the cement in the step (1) is ordinary portland cement, and the residual cement and other raw materials in the water supply plant are ground by 100 meshes so as to be mixed uniformly; the excitant is quicklime and gypsum, and the mass ratio of the quicklime to the gypsum is 1: 1.
The prepared high-efficiency phosphorus-removing baking-free ceramsite has strong phosphorus adsorption capacity.
The preparation method is characterized in that the main raw materials of residual sludge and Fenton sludge of the water supply plant are doped with auxiliary raw materials such as a cementing material, an exciting agent and a binder to prepare the high-efficiency phosphorus removal baking-free ceramsite which mainly comprises the Fenton sludge and the residual sludge of the water supply plant, the raw materials are cheap and easy to obtain, the equipment input cost and the operation cost are low, the prepared baking-free ceramsite is spherical particles with the particle size of 3-6 mm, the shape is regular, and pores are developed, the baking-free ceramsite can be used as a phosphorus removal adsorption material to be applied to a wastewater treatment process, has high adsorption capacity, can provide a new solution for emission reduction of wastewater pollutants, and treatment of the Fenton sludge and the residual sludge of the water supply plant, is favorable for realizing a win-win target of 'treatment of waste with waste', and has wide market application prospect.
Comparative example
A preparation method of baking-free ceramsite from residual sludge in a water supply plant comprises the following steps:
(1) pretreatment of raw materials: respectively grinding residual mud of a water supply plant, ordinary portland cement, fly ash and an exciting agent, and mixing according to a certain mass ratio, wherein the mass ratio of the residual mud of the water supply plant is 60-80%, the mass ratio of the cement is 10-15%, the mass ratio of the exciting agent is 2-6%, and the mass ratio of the fly ash is 10-20%;
(2) and (3) granulation: adding 32-35 ml of water solution containing 2-5% of water glass into the uniformly mixed raw materials in the step (1), stirring, and then putting into a pelletizer for pelleting to obtain spherical ceramsite raw material with the particle size of 5-10 mm;
(3) steaming: placing the ceramsite raw material at room temperature for 2-3 hours, and then putting the ceramsite raw material into a sterilization pot at the temperature of 70-90 ℃ for steam curing for 10-14 hours;
(4) aging: and naturally air-drying and aging the steamed ceramsite at room temperature for 2-3 days to obtain the spherical WTR non-fired ceramsite with the particle size of 5-10 mm.
In the step (1) of comparative example 1, the residual sludge of the water supply plant and other raw materials are ground through 100 meshes so as to be uniformly mixed; and the raw materials (residual mud, cement, exciting agent and fly ash in the water supply plant) in the step (1) are the same as those in the above embodiment.
SEM tests of the non-fired ceramsite (UCFWTR) in the water supply plant modified by adding fenton sludge prepared in the present embodiment and the non-fired ceramsite (UCWTR) in the water supply plant prepared by using only the non-fired ceramsite in the water supply plant in the comparative example are shown in fig. 2, wherein (a) is an SEM image of UCWTR, and (b) is an SEM image of UCFWTR, which can be obtained from fig. 2: in contrast to UCWTR, UCFWTR coexists in a fiber network and a ribbon structure (see FIG. 2), indicating that calcium silicate hydrate forms I and II (C-S-H) are formed. The Fe content in the fiber structure part was relatively high compared to the main component in the strip structure (see table 1), indicating that the addition of fenton sludge with high Fe content may be one of the main factors causing the structural change of the non-sintered ceramsite. The FT-IR spectra of two kinds of ceramsite are shown in FIG. 3, and it can be seen from FIG. 3 that UCFWTR is located at 873.06cm-1Fe-OH-Fe and 3418.8cm-1All the stretching vibration peaks of-OH are higher than UCWTR, which indicates that UCFWTR is generated moreThe increased content of the FeOOH compounds is beneficial to improving the adsorption capacity of the non-sintered ceramsite to phosphorus.
Table 1 EDS principal component analysis under structural morphology
TABLE 2XRF Total analysis
ND means lower XRF was not detected.
Example 1:
a preparation method of efficient phosphorus removal baking-free ceramsite mainly comprising Fenton sludge and residual sludge of a water supply plant takes residual sludge of a certain water supply plant in Hunan Tan City and Fenton sludge of a certain sewage treatment plant in Xinyun City as main raw materials. The main components of the two sludges are shown in Table 3.
TABLE 3 residual sludge from water plant and its Fenton sludge content
| Composition (I) | Residual mud content (%) | Composition (I) | Fenton sludge content (%) |
| Si | 26.5 | Si | 1.321 |
| Ca | 0.751 | Ca | 1.841 |
| Al | 11.02 | Al | 0.193 |
| Fe | 4.802 | Fe | 87.379 |
| K | 2.33 | Ti | 1.687 |
| Mg | 0.688 | Mg | 1.28 |
| Na | 0.22 | Gd | 0.496 |
| S | 0.105 | S | 2.189 |
| Mn | 0.228 | Mn | 1.011 |
| P | 0.157 | P | 0.855 |
| Ba | 0.061 | Cl | 0.442 |
| Cr | 0.014 | Tb | 0.342 |
| Pb | 0.011 | Cd | 0.306 |
| Cu | 0.0128 | Co | 0.225 |
| Organic matter (g/kg) | 24.90 | Organic matter (g/kg) | - |
The preparation method comprises the following steps:
(1) drying, crushing and grinding residual sludge of a water supply plant at 105 ℃ to 100 meshes, drying, crushing and grinding fenton sludge at 105 ℃, then firing the fenton sludge at 300 ℃ after grinding to 100 meshes, and uniformly mixing the fenton sludge with an excitant, fly ash and ordinary portland cement in a certain mass ratio;
(2) adding 35-40 mL of water and 6-8 g of water glass (binder) into every 100g of raw materials, and putting the mixture into a granulator to prepare a non-sintered ceramsite raw material;
(3) placing the raw materials at room temperature for 2-3 h, and then placing the raw materials in a sterilization pot at 80 ℃ for steam curing for 10-12 h;
(4) naturally air-drying and aging the steamed ceramsite for 1-2 d;
(5) and ageing the ceramsite subjected to natural air drying and ageing for 1-3 hours by using an oven at the temperature of 30-60 ℃, wherein the prepared efficient phosphorus removal unfired ceramsite mainly comprising Fenton sludge and residual sludge of a water supply plant is regular in shape and has an average particle size of about 6 mm.
Example 2:
the high-efficiency phosphorus removal unfired ceramsite mainly comprises Fenton sludge and residual sludge of a water supply plant, and has the following adsorption capacity on phosphorus:
weighing 5 (2 g in total mass) water supply plant non-fired ceramsite of example 1, which comprises 5% of Fenton sludge, 55% of water supply plant residual sludge, 10-15% of cement, 2-6% of excitant and 10-20% of fly ash, into a 100mL centrifuge tube, and adding 90mL phosphate solution (prepared from potassium dihydrogen phosphate and the pH value of the solution is adjusted to be neutral) with the concentration of 10 mg/L. Shaking at constant temperature of 25 deg.C and 130rpm for 24h, centrifuging the sample at 8000r/min for 10min, and collecting supernatant to determine phosphorus concentration.
The result shows that the removal rate of the ceramsite to the phosphorus in the wastewater is 46.10 percent.
Example 3:
the high-efficiency phosphorus removal unfired ceramsite mainly comprises Fenton sludge and residual sludge of a water supply plant, and has the following adsorption capacity on phosphorus:
weighing 5 (2 g in total mass) water supply plant non-fired ceramsite which is prepared from 10% of Fenton sludge, 50% of water supply plant residual sludge, 10-15% of cement, 2-6% of excitant and 10-20% of fly ash in example 1, adding 90mL of phosphate solution (prepared from potassium dihydrogen phosphate and the pH value of the solution is adjusted to be neutral) with the concentration of 10mg/L into a 100mL centrifuge tube. Shaking at constant temperature of 25 deg.C and 130rpm for 24h, centrifuging the sample at 8000r/min for 10min, and collecting supernatant to determine phosphorus concentration.
The result shows that the removal rate of the ceramsite to the phosphorus in the wastewater is 57.68%.
Example 4:
the high-efficiency phosphorus removal unfired ceramsite mainly comprises Fenton sludge and residual sludge of a water supply plant, and has the following adsorption capacity on phosphorus:
weighing 5 (2 g in total mass) water supply plant non-fired ceramsite which is prepared from 20% of Fenton sludge, 40% of water supply plant residual sludge, 10-15% of cement, 2-6% of excitant and 10-20% of fly ash in the raw materials in example 1, adding 90mL of phosphate solution (prepared from potassium dihydrogen phosphate and the pH value of the phosphate solution is adjusted to be neutral) with the concentration of 10mg/L into a 100mL centrifuge tube. Shaking at constant temperature of 25 deg.C and 130rpm for 24h, centrifuging the sample at 8000r/min for 10min, and collecting supernatant to determine phosphorus concentration.
The result shows that the removal rate of the ceramsite to the phosphorus in the wastewater is 65.07 percent.
Example 5:
the high-efficiency phosphorus removal unfired ceramsite mainly comprises Fenton sludge and residual sludge of a water supply plant, and has the following adsorption capacity on phosphorus:
weighing 5 (2 g in total mass) water supply plant non-fired ceramsite which is prepared from 30% of Fenton sludge, 30% of water supply plant residual sludge, 10-15% of cement, 2-6% of excitant and 10-20% of fly ash in the raw materials in example 1, adding 90mL of phosphate solution (prepared from potassium dihydrogen phosphate and the pH value of the phosphate solution is adjusted to be neutral) with the concentration of 10mg/L into a 100mL centrifuge tube. Shaking at constant temperature of 25 deg.C and 130rpm for 24h, centrifuging the sample at 8000r/min for 10min, and collecting supernatant to determine phosphorus concentration.
The result shows that the removal rate of the ceramsite to the phosphorus in the wastewater is 47.87%.
The Fenton sludge mainly contains iron oxyhydroxide and a small amount of activated carbon, and detection shows that the UCFWTR prepared by adding the Fenton sludge has the particle size of about 3-6 mm, the cylinder pressure strength of 4.13-7.56 Mpa, the water absorption rate of about 40% and the wear rate of about 3%, and meets the performance requirements of ceramsite. When the Fenton sludge in the invention is changed into the activated carbon and other conditions are not changed to prepare the UCWTR, the mechanical strength is weak, most of the decomposition phenomenon occurs in the aqueous solution, and the complete ceramsite shape cannot be maintained; when the iron salt is replaced, the iron-supported UCWTR prepared by adding the iron salt has the advantages that the basic performance of the ceramsite is not changed greatly, but the iron loading rate is low, and the improvement effect on the phosphorus removal effect is small compared with the original UCWTR.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make many possible variations and modifications to the disclosed embodiments, or equivalent modifications, without departing from the spirit and scope of the invention, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (10)
1. The preparation method of the high-efficiency phosphorus-removing unfired ceramsite is characterized by comprising the following steps of:
(1) preparing materials: pretreating residual sludge and Fenton sludge of a water supply plant, and mixing the pretreated residual sludge and Fenton sludge with cement, fly ash and an activator uniformly, wherein the mass ratio of the Fenton sludge to the residual sludge of the water supply plant to the cement to the fly ash to the activator is 5-30%, 30-55%, 10-15%, 10-20% and 2-5%;
(2) and (3) granulation: adding water solution of water glass into the uniformly mixed raw materials, uniformly stirring, and granulating to obtain ceramsite raw material;
(3) steaming: placing the ceramsite raw material at room temperature for a certain time, and then placing the ceramsite raw material into a sterilization pot for steam curing;
(4) aging at room temperature: naturally air-drying and aging the steamed ceramsite at room temperature;
(5) aging in an oven: and aging the ceramsite after natural air drying and aging in an oven to obtain the high-efficiency phosphorus-removing non-fired ceramsite mainly comprising Fenton sludge and residual sludge of a water supply plant.
2. The preparation method of the efficient phosphorus removal unfired ceramsite according to claim 1, wherein in the step (1), the Fenton sludge is dried, crushed, sieved by a 100-mesh sieve, and then burned; the pretreatment method of the residual sludge of the water supply plant comprises the steps of drying, crushing and sieving with a 100-mesh sieve.
3. The preparation method of the efficient phosphorus removal unfired ceramsite according to claim 1, wherein in the step (2), 35-40 mL of water and 6-8 g of water glass are added to each 100g of raw materials.
4. The method for preparing high-efficiency phosphorus-removing unfired ceramsite according to claim 1, wherein the cement is ordinary portland cement; the excitant is a mixture of quicklime and gypsum, and the mass ratio of the quicklime to the gypsum in the mixture is 1-1.5: 1-2.
5. The preparation method of the efficient phosphorus removal unfired ceramsite according to any one of claims 1-4, wherein in the step (5), the aging condition in the oven is aging at 30-60 ℃ for 1-3 h.
6. The method for preparing high-efficiency phosphorus-removing unfired ceramsite according to any one of claims 1-4, wherein in the step (3), the ceramsite raw material is placed at room temperature for 2-3 hours; the steam curing temperature is 70-90 ℃, and the steam curing time is 10-12 h.
7. The preparation method of the efficient phosphorus removal unfired ceramsite according to any one of claims 1-4, wherein in the step (4), the natural air drying and aging time is 1-2 days.
8. The preparation method of the efficient phosphorus removal unfired ceramsite according to any one of claims 1-4, wherein the particle size of the prepared efficient phosphorus removal unfired ceramsite is 3-6 mm, and the prepared efficient phosphorus removal unfired ceramsite is spherical.
9. The efficient phosphorus removal unfired ceramsite is characterized by being prepared by the preparation method of any one of claims 1-8.
10. The high-efficiency phosphorus removal baking-free ceramsite of claim 9 is applied to treatment of phosphorus-containing wastewater.
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