CN112142153A - Dephosphorizing and organic matter removing reagent and method for treating phosphorus-containing organic matter-containing wastewater - Google Patents
Dephosphorizing and organic matter removing reagent and method for treating phosphorus-containing organic matter-containing wastewater Download PDFInfo
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- CN112142153A CN112142153A CN201910559840.4A CN201910559840A CN112142153A CN 112142153 A CN112142153 A CN 112142153A CN 201910559840 A CN201910559840 A CN 201910559840A CN 112142153 A CN112142153 A CN 112142153A
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- C02F2101/105—Phosphorus compounds
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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
- C02F2101/30—Organic compounds
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Abstract
The invention provides a reagent for removing phosphorus and Total Organic Carbon (TOC), a preparation method thereof and a method for treating phosphorus-containing wastewater containing TOC by using the reagent. The reagent is prepared from a mixture of a coagulating sedimentation material and anaerobic granular sludge, and can be modified by guar gum. The coagulating sedimentation material and the anaerobic granular sludge are derived from the remainder of the wastewater treatment. The reagent has good treatment effect on wastewater containing phosphorus and trace organic matters, and can effectively reduce the content of phosphorus and organic matters in the wastewater.
Description
Technical Field
The invention belongs to the field of wastewater treatment, and particularly relates to a dephosphorizing and organic matter removing reagent and a method for treating phosphorus-containing organic matter-containing wastewater.
Background
In the industrial production process, in order to realize the recycling of wastewater, a reverse osmosis process is often adopted to treat the produced water, reverse osmosis permeate clear water is used as circulating water for recycling, and concentrated water contains a certain amount of organic matters and is difficult to directly discharge.
The conventional treatment method of reverse osmosis concentrated water adopts ozone, hydrogen peroxide and the like as oxidants, and the oxidation is carried out under the action of catalysts, ultrasound and the like to degrade organic matters so as to reach the emission standard. CN102040294A discloses a method for treating reverse osmosis concentrated water by using ozone and hydrogen peroxide as oxidants and matching with activated carbon adsorption, the adding amount of the oxidants is large, and the operation cost is relatively high. CN102153171A discloses a method for treating reverse osmosis concentrated water by ozone catalytic oxidation, which needs to treat tail gas because of secondary pollution caused by aeration in the process.
In the industrial production process, the content of organic matters and total phosphorus in reverse osmosis concentrated water exceeds the standard, the standard of sea drainage is difficult to achieve, the traditional advanced oxidation treatment mode is adopted, the operation cost is high, and oxidation produced water often contains peroxide and causes secondary pollution to water, so that a new treatment process needs to be developed to treat reverse osmosis concentrated water.
Disclosure of Invention
The invention aims to provide a reagent for effectively dephosphorizing and removing organic matters. The reagent has stable treatment effect on phosphorus and organic matters in wastewater, and the raw materials of the reagent are by-products in the wastewater treatment process, so that the cost is low, and the waste can be prepared from waste.
Another object of the present invention is to provide a method for preparing the reagent. The operation method is simple and can realize industrial application.
It is still another object of the present invention to provide a method for treating wastewater containing phosphorus and organic matters using the reagent. The treatment method is simple and easy to implement, has high treatment efficiency, can effectively remove low-content phosphorus and organic matters in the wastewater, and reaches the direct discharge standard.
In order to achieve the above objects and achieve the above technical effects, the invention adopts the following technical scheme:
the reagent is prepared from byproducts generated after wastewater treatment, wherein the byproducts contain coagulating sedimentation substances and anaerobic granular sludge; optionally, the modifier guar gum is added at the time of preparation of the reagent.
In the invention, the mass ratio of the coagulating sedimentation object to the anaerobic granular sludge in the by-product is 1: 1-1: 5. The coagulating sedimentation and the anaerobic granular sludge are both byproducts from different wastewater treatment processes. The coagulating sedimentation is a porous oxide material rich in magnesium, aluminum, nickel, iron, calcium, silicate, phosphate and the like. In the pretreatment of wastewater, coagulation is often used to remove suspended particles from the wastewater, and during this process, a large amount of coagulated precipitate is produced, which is generally treated as solid waste. The anaerobic granular sludge is mainly a byproduct generated by the anaerobic reactor when treating high-concentration organic wastewater, and has a porous surface and a better adsorption effect. The invention has no special requirements on the composition of the coagulating sedimentation object and the anaerobic granular sludge, and mainly utilizes the porous compact structure of the coagulating sedimentation object and the anaerobic granular sludge, so that the coagulating sedimentation object by-product after coagulating treatment from a wastewater treatment plant and the anaerobic granular sludge by-product after anaerobic treatment are both suitable for the invention.
In the invention, when the modifier guar gum is added, the content of the guar gum is 2.0-12.0 wt%, preferably 4.0-6.0 wt%, based on the total weight of the coagulating sedimentation product and the anaerobic granular sludge. Guar gum is a macromolecular natural hydrophilic colloid, belongs to natural galactomannan, and is a quality modifier and a natural thickener. After guar gum is added according to a certain proportion for modification, the surface of the fired carrier has a layer of compact film, the hardness is high, the porosity is high, the strong acid and alkali resistance is realized, and the specific surface area and the structural strength of the porous solid particles can be effectively improved.
Uniformly mixing a coagulating sedimentation and anaerobic granular sludge, and sequentially performing vacuum pretreatment, water soaking, drying, roasting and strip extrusion forming procedures to obtain a porous solid granular reagent; optionally, the porous solid particulate reagent is modified with guar gum.
In the invention, the vacuum pretreatment time is 10-30 min, and the water immersion time is 20-40 min.
In the invention, the drying temperature is 60-150 ℃, and the drying time is 3-5 h; the roasting temperature is 450-600 ℃, the roasting time is 3-5 h, the preferable roasting time is 3.5-4.5 h,
in the invention, the length of the obtained porous solid particles is 0.5-1.5 cm, and the specific surface area is 500-2000 m2/g。
In the invention, when guar gum is added for modification, the method comprises the following steps: and (3) impregnating the porous solid particle reagent with guar gum aqueous solution, and then drying and roasting the obtained solid to obtain the guar gum modified porous solid particles.
In the invention, when guar gum is added for modification, the dipping time is 50-250 min, preferably 100-150 min; the concentration of the guar gum water solution is 0.02-0.12 g/mL; the drying temperature is 60-150 ℃, and the drying time is 3-5 h; the roasting temperature is 450-600 ℃, the roasting time is 3-5 h, and the preferable roasting time is 3.5-4.5 h.
A method for treating wastewater containing phosphorus and/or organic matter by using the reagent, comprising the following steps:
(A) adding the reagent into the wastewater to mainly perform dephosphorization reaction; and/or
(B) The reagent is added into the wastewater to mainly carry out organic matter removal reaction.
In the invention, the reaction temperature of the step (A) is 30-50 ℃, preferably 35-45 ℃, and the reaction time is 0.5-3.5 h, preferably 1.5-2.5 h; the addition amount of the reagent is 0.1-0.5kg/t wastewater. After the step (A), most of total phosphorus and part of organic matters in the wastewater can be adsorbed in the pore channels by the reagent, and the reagent can be treated as solid waste after the adsorption is saturated.
In the invention, the reaction temperature of the step (B) is 20-30 ℃, preferably 22-27 ℃, and the reaction time is 5-10 hours, preferably 7-8 hours; the addition amount of the reagent is 0.5-1.0kg/t wastewater. The selection of the reaction time and the reaction temperature determines the adsorption efficiency of the reagent on the organic matters, generally speaking, the increase of the reaction time is beneficial to the improvement of the treatment efficiency, when the reaction time reaches a certain value, the removal rate of the total phosphorus tends to a fixed value, and when the temperature is increased, the adsorption efficiency of the reagent on the organic matters is reduced, and when the temperature is less than 27 ℃, the adsorption efficiency is not greatly changed.
In the invention, the total phosphorus concentration of wastewater influent treated by the method is less than or equal to 10mg/L, and the Total Organic Carbon (TOC) concentration of wastewater influent is less than or equal to 100 mg/L.
In the invention, the vacuum degrees are absolute pressures.
The invention has the beneficial effects that:
(1) the coagulating sedimentation and the anaerobic granular sludge used in the invention are derived from byproducts in different wastewater treatment processes, are simple and easy to obtain, have low cost and realize the recycling of wastes.
(2) The dephosphorizing and organic matter removing reagent used by the invention has good treatment effect, the treated reverse osmosis concentrated water can reach the direct discharge standard (TP is less than 0.5mg/L, TOC is less than 20mg/L, DB37 Shandong peninsula watershed water pollution discharge standard and GB31571 petrochemical industry pollutant discharge standard), the environmental pressure is small, the economic investment is less, the method is simple and easy to operate, and the method is safe and reliable.
Detailed Description
The technical solution and the effects of the present invention are further described by the following specific examples. The following examples are merely illustrative of the present invention and are not intended to limit the scope of the present invention. Simple modifications of the invention applying the inventive concept are within the scope of the invention as claimed.
A jacketed stirred reactor was purchased from Zibofriend Sheng chemical plant manufacturing Co., Ltd.
The main raw material and wastewater information is as follows:
the coagulating sedimentation is from a wastewater treatment system of Wanhua chemical company, calcium and magnesium ions in the circulating water are treated by a flocculation means, and the obtained sedimentation product is the coagulating sedimentation;
anaerobic granular sludge comes from wastewater treatment systems of Wanhua chemical company, and a large amount of anaerobic granular sludge is generated due to bacterial proliferation;
reverse osmosis concentrated wastewater containing phosphorus and organic matters, wastewater treatment system of Wanhua chemical company;
guar gum, hongtao bioengineering ltd, Hebei.
GC analysis conditions were as follows: an Agilent HP-5 model gas chromatographic column is adopted, the size of the chromatographic column is 30m, 530 μm and 1.5 μm, and the temperature rising method of the chromatographic column comprises the following steps: setting the initial temperature to 50 ℃, keeping the temperature for 2min, heating to 280 ℃ at the speed of 5 ℃/min, keeping the temperature for 6min, and analyzing the main components of the water quality; total phosphorus test: hash-digestion ascorbic acid method; the organic matter content testing method comprises the following steps: national standard COD digestion method.
Example 1
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:1 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 4h, after roasting, taking out and cooling to room temperature to obtain the mixture with the length of 1cm and the specific surface area of 1250m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.41mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13mg/L under the adsorption action of the reagent.
Example 2
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:5 in a glass bottle, carrying out vacuum pretreatment for 20min, wherein the vacuum degree is 96.0KPa, then soaking for 30min by using pure water with the same volume, drying for 5h in an oven at 100 ℃, then roasting for 5h in a muffle furnace at 500 ℃, after roasting and sintering, taking out and cooling to room temperature, and simultaneously taking guar gum water-soluble solution containing 0.02g/mL of guar gumMixing and soaking 20.0mL of the solution for 125min, drying in an oven at 120 ℃ for 5h, roasting in a muffle furnace at 500 ℃ for 5h, taking out after roasting, and cooling to room temperature to obtain a product with the length of 0.6cm and the specific surface area of 550m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.40mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13.5mg/L under the adsorption action of the reagent.
Example 3
Putting 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 into a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking the sample in pure water for 30min, the sample is dried in an oven at 60 ℃ for 3h, then roasting the sample in a muffle furnace at 500 ℃ for 3h, after roasting and sintering, taking out the sample and cooling the sample to the room temperature, simultaneously taking 20.0mL of guar gum solution containing 0.05g/mL of guar gum, mixing and soaking the solution for 125min, putting the sample in the oven at 120 ℃ for drying for 3h, then roasting the sample in the muffle furnace at 500 ℃ for 3h, after roasting, taking out the sample and cooling the sample to the room temperature to obtain the product with the length of 1.452A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.42mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13.1mg/L under the adsorption action of the reagent.
Example 4
20g of a sample obtained by mixing the coagulating sedimentation material and the anaerobic granular sludge according to the ratio of 1:3 is placed in glassVacuum pre-treating in a bottle for 20min at vacuum degree of 96.0KPa, soaking in pure water of the same volume for 30min, drying at 150 deg.C for 3h in an oven, baking at 500 deg.C for 4h in a muffle furnace, taking out and cooling to room temperature after baking and sintering, mixing and soaking 20.0mL guar gum solution containing 0.05g/mL guar gum for 125min, drying at 120 deg.C in an oven for 3h, baking at 500 deg.C in a muffle furnace for 4h, taking out and cooling to room temperature after baking is finished to obtain a product with length of 1.2cm and specific surface area of 1310m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.40mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13.2mg/L under the adsorption action of the reagent.
Example 5
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven for 3h at 100 ℃, then roasting in a muffle furnace for 4h at 450 ℃, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, drying in the oven for 3h at 120 ℃, then roasting in the muffle furnace for 4h at 500 ℃, taking out and cooling to room temperature after roasting, and obtaining the mixture with the length of 0.9cm and the specific surface area of 1230m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.40mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13.5mg/L under the adsorption action of the reagent.
Example 6
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 600 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 4h, after roasting, taking out and cooling to room temperature to obtain a mixture with the length of 0.9cm and the specific surface area of 1130m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.40mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13.5mg/L under the adsorption action of the reagent.
Example 7
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment for 20min, wherein the vacuum degree is 96.0KPa, then soaking for 30min by using pure water with the same volume, drying for 3h at 100 ℃ in an oven, then roasting for 4h at 500 ℃ in a muffle furnace, taking out after roasting, cooling to room temperature to obtain a product with the length of 1.1cm and the specific surface area of 1130m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.48mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 17.8mg/L under the adsorption action of the reagent.
Example 8
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.12g/mL of guar gum, mixing and soaking for 125min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 4h, after roasting, taking out and cooling to room temperature to obtain the mixture with the length of 1.03cm and the specific surface area of 1320m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.37mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 12.5mg/L under the adsorption action of the reagent.
Example 9
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 50min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 4h, after roasting, taking out and cooling to room temperature to obtain the mixture with the length of 0.95cm and the specific surface area of 1260m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.4mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13.2mg/L under the adsorption action of the reagent.
Example 10
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 250min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 4h, after roasting, taking out and cooling to room temperature to obtain a product with the length of 0.9cm and the specific surface area of 1230m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.37mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 12.5mg/L under the adsorption action of the reagent.
Example 11
20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to the ratio of 1:3 is placed in a glass bottle for vacuum pretreatment, the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then the sample is soaked in pure water with the same volume for 30min, the sample is placed in an oven for drying at 100 ℃ for 3h, then the sample is roasted in a muffle furnace at 500 ℃ for 4h, after the roasting and sintering, the sample is taken out and cooled to the room temperature,simultaneously taking 20.0mL of guar gum aqueous solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing in an oven for drying at 120 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 3h, taking out after roasting, cooling to room temperature to obtain the guar gum with the length of 0.95cm and the specific surface area of 1230m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.4mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13.2mg/L under the adsorption action of the reagent.
Example 12
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 5h, after roasting, taking out and cooling to room temperature to obtain the mixture with the length of 0.96cm and the specific surface area of 1260m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 2h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.39mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 12.5mg/L under the adsorption action of the reagent.
Example 13
Taking the coagulating sedimentation and anaerobic20g of a sample mixed according to a ratio of 1:3 is placed in a glass bottle for vacuum pretreatment, the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, the sample is soaked in pure water for 30min in the same volume, the sample is placed in an oven for drying at 100 ℃ for 3h, the sample is roasted in a muffle furnace at 500 ℃ for 4h, after the roasting and sintering, the sample is taken out and cooled to the room temperature, 20.0mL of guar gum solution containing 0.05g/mL of guar gum is taken, the mixed soaking is carried out for 125min, the sample is placed in the oven for drying at 120 ℃ for 3h, the sample is roasted in the muffle furnace at 500 ℃ for 5h, the sample is taken out after the roasting is finished and cooled to the room temperature, and the sample with the length2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at the temperature of 30 ℃ for 2 hours, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.4mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13.2mg/L under the adsorption action of the reagent.
Example 14
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 5h, after roasting, taking out and cooling to room temperature to obtain a product with the length of 0.99cm and the specific surface area of 1230m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at the temperature of 50 ℃ for 2 hours, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.37mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 12.3mg/L under the adsorption action of the reagent.
Example 15
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 5h, after roasting, taking out and cooling to room temperature to obtain the mixture with the length of 0.9cm and the specific surface area of 1290m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 1h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.4mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13.2mg/L under the adsorption action of the reagent.
Example 16
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 5h, after roasting, taking out and cooling to room temperature to obtain the mixture with the length of 1.3cm and the specific surface area of 1330m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 3h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.37mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 12.3mg/L under the adsorption action of the reagent.
Example 17
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 5h, after roasting, taking out and cooling to room temperature to obtain a mixture with the length of 0.97cm and the specific surface area of 1230m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 3h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.2kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.38mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 12.3mg/L under the adsorption action of the reagent.
Example 18
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment for 20min, wherein the vacuum degree is 96.0KPa, then soaking for 30min by using pure water with the same volume, drying for 3h at 100 ℃ in an oven, then roasting for 4h at 500 ℃ in a muffle furnace, taking out and cooling to room temperature after roasting, and simultaneously taking 0.05g/mL of guar gum20.0mL of guar gum aqueous solution, mixing and soaking for 125min, drying in an oven at 120 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 5h, taking out after roasting, cooling to room temperature to obtain the guar gum with the length of 0.9cm and the specific surface area of 1290m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 3h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.4mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 20 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13.2mg/L under the adsorption action of the reagent.
Example 19
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 5h, after roasting, taking out and cooling to room temperature to obtain the mixture with the length of 1.1cm and the specific surface area of 1230m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 3h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.37mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 30 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 12.3mg/L under the adsorption action of the reagent.
Example 20
Taking a sample obtained by mixing the coagulating sedimentation material and the anaerobic granular sludge according to the ratio of 1:3Placing 20g of the product in a glass bottle, performing vacuum pretreatment for 20min at a vacuum degree of 96.0KPa, soaking for 30min by using pure water with the same volume, drying for 3h at 100 ℃ in an oven, roasting for 4h at 500 ℃ in a muffle furnace, taking out the product after roasting and sintering, cooling to room temperature, taking 20.0mL of guar gum solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing the product in the oven, drying for 3h at 120 ℃, roasting for 5h at 500 ℃ in the muffle furnace, taking out the product after roasting, cooling to room temperature to obtain the product with the length of 0.9cm and the specific surface area of 1270m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 3h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.4mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 5 hours, wherein the addition amount of the dephosphorizing and organic matter removing reagent is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 13.2mg/L under the adsorption action of the reagent.
Example 21
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 5h, after roasting, taking out and cooling to room temperature to obtain a mixture with the length of 0.95cm and the specific surface area of 1230m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 3h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.37mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 10h, wherein the addition amount of the dephosphorizing and organic matter removing reagent is 0.9kg/t of wastewater, and the TOC can be treated from 60mg/L to 12.3mg/L under the adsorption action of the reagent.
Example 22
Placing 20g of a sample obtained by mixing the coagulating sedimentation and the anaerobic granular sludge according to a ratio of 1:3 in a glass bottle, carrying out vacuum pretreatment, wherein the vacuum pretreatment time is 20min, the vacuum degree is 96.0KPa, then soaking in pure water for 30min with the same volume, drying in an oven at 100 ℃ for 3h, then roasting in a muffle furnace at 500 ℃ for 4h, after roasting and sintering, taking out and cooling to room temperature, simultaneously taking 20.0mL of guar gum water solution containing 0.05g/mL of guar gum, mixing and soaking for 125min, placing in the oven at 120 ℃ for drying for 3h, then roasting in the muffle furnace at 500 ℃ for 5h, after roasting, taking out and cooling to room temperature to obtain a mixture with the length of 0.9cm and the specific surface area of 1360m2A dephosphorizing and organic matter removing reagent per gram.
Taking 5L of wastewater containing phosphorus and organic matters, introducing the wastewater into a No. 1 stirring reactor, reacting at 40 ℃ for 3h, wherein the adding amount of a reagent for removing phosphorus and organic matters is 0.4kg/t of wastewater, and the total phosphorus can be treated from 9mg/L to 0.38mg/L under the adsorption action of the reagent; and (3) introducing the produced water into a No. 2 stirring reactor, reacting at 25 ℃ for 7.5h, wherein the addition amount of the reagent for removing phosphorus and organic matters is 0.6kg/t of wastewater, and the TOC can be treated from 60mg/L to 12.3mg/L under the adsorption action of the reagent.
Comparative example 1
In the industry, organic matters in the wastewater are treated by adopting an ozone and hydrogen peroxide oxidation mode, and total phosphorus is treated by adopting a flocculation sedimentation mode.
An ozone and hydrogen peroxide oxidation experiment is carried out at the temperature of 25 ℃ and normal pressure, 5L of wastewater is obtained, the hydrogen peroxide addition content is 500mg/L, the ozone concentration is 50mg/L, the ozone-containing air flow is 1.5L/min, the operation is continuously carried out for 2h, 50mg/L of polyaluminium chloride (PAC) and 2mg/L of Polyacrylamide (PAM) are added into produced water to carry out a flocculation sedimentation experiment, and the sedimentation time is 10 min.
Compared with the example 22, under the condition of consistent running cost, the TOC of the wastewater is treated to 30mg/L, and the total phosphorus is treated to 0.45mg/L, so that the wastewater can not reach the sea discharge standard.
Claims (11)
1. The reagent for removing phosphorus and organic matters is characterized in that the reagent is prepared by utilizing a by-product after wastewater treatment, and the by-product contains coagulating sedimentation and anaerobic granular sludge;
optionally, the modifier guar gum is added at the time of preparation of the reagent.
2. The reagent of claim 1, wherein the mass ratio of the coagulating sedimentation product to the anaerobic granular sludge in the by-product is 1: 1-1: 5.
3. The agent according to claim 1 or 2, wherein when the modifier guar gum is added, the guar gum is present in an amount of 2.0 to 12.0 wt.%, preferably 4.0 to 6.0 wt.%, based on the total weight of the coagulated precipitate and the anaerobic granular sludge.
4. A method for preparing the reagent for removing phosphorus and organic substances according to any one of claims 1 to 3, which comprises the steps of uniformly mixing the coagulating sedimentation and the anaerobic granular sludge, and sequentially carrying out vacuum pretreatment, water soaking, drying, roasting and strip extrusion molding to obtain a porous solid granular reagent;
optionally, the porous solid particulate reagent is modified with guar gum.
5. The method for preparing the reagent according to claim 4, wherein the drying temperature is 60-150 ℃ and the drying time is 3-5 h; the roasting temperature is 450-600 ℃, the roasting time is 3-5 h, and the preferable roasting time is 3.5-4.5 h; the length of the obtained porous solid particles is 0.5-1.5 cm, and the specific surface area is 500-2000 m2/g。
6. The method for preparing reagent according to claim 4 or 5, characterized in that when guar gum is added for modification, the method comprises the following steps: and (3) impregnating the porous solid particle reagent with guar gum aqueous solution, and then drying and roasting the obtained solid to obtain the guar gum modified porous solid particles.
7. The method for preparing a reagent according to any one of claims 4 to 6, wherein when guar gum is added for modification, the dipping time is 50 to 250min, preferably 100 to 150 min; the concentration of the guar gum water solution is 0.02-0.12 g/mL; the drying temperature is 60-150 ℃, and the drying time is 3-5 h; the roasting temperature is 450-600 ℃, the roasting time is 3-5 h, and the preferable roasting time is 3.5-4.5 h.
8. A method for treating wastewater containing phosphorus and/or organic substances by using the reagent according to any one of claims 1 to 3 or the reagent prepared by the preparation method according to any one of claims 4 to 7, comprising the steps of:
(A) adding the reagent into the wastewater to mainly perform dephosphorization reaction; and/or
(B) The reagent is added into the wastewater to mainly carry out organic matter removal reaction.
9. The wastewater treatment method according to claim 8, wherein the reaction temperature in the step (A) is 30-50 ℃, preferably 35-45 ℃, and the reaction time is 0.5-3.5 h, preferably 1.5-2.5 h; the addition amount of the reagent is 0.1-0.5kg/t wastewater.
10. The wastewater treatment method according to claim 8, wherein the reaction temperature in the step (B) is 20-30 ℃, preferably 22-27 ℃, and the reaction time is 5-10 hours, preferably 7-8 hours; the addition amount of the reagent is 0.5-1.0kg/t wastewater.
11. A method for treating wastewater according to any of claims 8-10, wherein the wastewater influent treated by the method has a total phosphorus concentration of 10mg/L or less and a Total Organic Carbon (TOC) concentration of 100mg/L or less.
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| JP2004114003A (en) * | 2002-09-30 | 2004-04-15 | Meidensha Corp | Phosphorus adsorbent and method of forming the same, method of recovering phosphorus, method of treating phosphorus adsorbent, and method of treating water containing phosphorus content |
| CN102701200A (en) * | 2012-05-14 | 2012-10-03 | 北京工业大学 | Method for preparing active carbon from municipal sludge by two-step thermal decomposition |
| CN104587960A (en) * | 2015-01-29 | 2015-05-06 | 长安大学 | Preparation method of dephosphorization high-temperature modified aluminum sludge |
| CN108862824A (en) * | 2018-06-13 | 2018-11-23 | 南京大学 | A kind of denitrification sewage-treatment plant and its treatment process |
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| JP2004114003A (en) * | 2002-09-30 | 2004-04-15 | Meidensha Corp | Phosphorus adsorbent and method of forming the same, method of recovering phosphorus, method of treating phosphorus adsorbent, and method of treating water containing phosphorus content |
| CN102701200A (en) * | 2012-05-14 | 2012-10-03 | 北京工业大学 | Method for preparing active carbon from municipal sludge by two-step thermal decomposition |
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