CN110980932A - Oil shale semicoke/polyvinyl alcohol composite immobilized carrier and preparation method thereof - Google Patents
Oil shale semicoke/polyvinyl alcohol composite immobilized carrier and preparation method thereof Download PDFInfo
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- CN110980932A CN110980932A CN201911169133.0A CN201911169133A CN110980932A CN 110980932 A CN110980932 A CN 110980932A CN 201911169133 A CN201911169133 A CN 201911169133A CN 110980932 A CN110980932 A CN 110980932A
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/02—Aerobic processes
- C02F3/10—Packings; Fillings; Grids
- C02F3/105—Characterized by the chemical composition
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/28—Anaerobic digestion processes
- C02F3/2806—Anaerobic processes using solid supports for microorganisms
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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Abstract
The invention discloses an oil shale semicoke/polyvinyl alcohol composite immobilized carrier and a preparation method thereof, belonging to the technical field of sewage treatment. Dissolving polyvinyl alcohol in deionized water to prepare a uniform and transparent polyvinyl alcohol solution; then adding the oil shale semi-coke into the polyvinyl alcohol solution, and stirring at high temperature to form a uniform mixed solution; and then adding OP-10, sulfuric acid and formaldehyde into the mixed solution in sequence, stirring, curing and molding at high temperature, washing, cutting into blocks and drying to obtain the composite immobilized carrier. The composite immobilized carrier is porous sponge-shaped, and the density is 0.22-0.30 g/cm3The porosity is 60-92%, and the pore diameter is 1-4 mm. The method has the advantages of easily available raw materials, simple manufacturing process and low cost, and simultaneously solves the problem of environmental pollution caused by the oil shale byproduct, and has great application value and prospect in the field of sewage treatment.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, relates to a microorganism immobilized carrier for a sewage treatment process, and particularly relates to an oil shale semicoke/polyvinyl alcohol composite immobilized carrier and a preparation method thereof.
Background
The water environment pollution condition in China is increasingly serious, and the requirements for developing a new efficient wastewater treatment technology and a new material are more and more urgent.
A biochemical sewage treating process features that ⑴ high-efficiency microbes are immobilized to increase the treating efficiency and water resistance of reactor, increase the impact power of organic load and decrease sludge output, ⑵ microbes are immobilized to increase the stability to temp and pH value, ⑶ microbes with special function are fixed to degrade refractory organic substances, ⑷ is used to improve the theoretical staying time of microbes, so improving the contradiction between generation period and staying time of microbes, resulting in high treating performance, ⑸ is easy to separate from product, ⑹ is used to mix bacteria and algae and fix them together.
The contaminant removal ability of the immobilized microorganism is affected by the kind of the carrier and the preparation method thereof. Polyvinyl alcohol gel is used for microbial immobilization methods in many reports. Chinese patent CN1883787 reports a method for preparing spherical bentonite by polyvinyl alcohol embedding, which is used for adsorbing and removing pollutants in water; CN1920018 reports a polyvinyl alcohol immobilized cell spherical carrier, which is characterized in that a suspension of microbial cells is mixed with polyvinyl alcohol and sodium alginate, and then the mixture is subjected to sol-gel solidification. These supports affect their immobilization due to mass transfer problems. And CN101186720 reported a polyvinyl alcohol foaming material for sewage treatment, and application No. 200810150836 reported a macroporous reticular polyvinyl alcohol foam carrier, etc., so that the polyvinyl alcohol foam body has great development in the application field of biological immobilized carriers.
The oil shale semicoke is a byproduct generated after oil shale is subjected to low-temperature dry distillation technology to produce shale oil under the condition of air isolation, and the main component of the oil shale semicoke is SiO2、Al2O3And in addition, Fe in different quantities2O3CaO, MgO, and the like. The total amount of the world shale oil reserves is 3741 hundred million tons calculated in the early 2000, and the amount of Chinese proven resources is about 315 hundred million tons. After shale oil is industrially extracted, a large amount of oil shale semicoke is generated, for example, the yield of the semicoke of Gansu province, coal and electricity group Limited in the kiln street reaches 60-100 ten thousand tons every year, and about 300 ten thousand tons of the oil shale semicoke of China petrochemical group, famous petrochemical industry Limited, is generated every year. At present, the oil shale semicoke is mainly used as a poor-quality coal fuel to be sold to poor-quality coal power plants and cement plants, but the use amount is limited, and most of semicoke is piled on soil as waste to cause damage to soil environment and surrounding vegetation. In addition, the price of the semicoke is low and is about 15% of the exploitation cost of the oil shale, so that the industrial chain has serious cost hang-over. Therefore, the search for a new comprehensive utilization way of the oil shale semi-coke is particularly critical to the oil shale industry. CN1919912 reports an oil shale semicoke polyolefin master batch and a preparation method thereof. CN105879835 reports a method for preparing uranium adsorbing material by using oil shale semi-coke as a raw material. CN101254922 discloses a method for preparing modified white carbon by using oil shale oil-making residuesA black method. CN101037204 discloses a method for preparing white carbon black by using oil shale ash. The invention and the application can consume a part of the oil shale semicoke, but develop a new application of the oil shale semicoke, change waste into valuable and are a hot point of attention.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an oil shale semicoke/polyvinyl alcohol composite immobilized carrier and a preparation method thereof.
The invention is realized by the following technical scheme:
the invention provides an oil shale semicoke/polyvinyl alcohol composite immobilized carrier, which consists of the following components: 100 parts of polyvinyl alcohol, 400-1400 parts of deionized water, 30-50 parts of aldehyde, 30-40 parts of sulfuric acid, 102-5 parts of polyoxyethylene octyl phenol ether and 1-50 parts of oil shale semicoke.
Preferably, the composite immobilization carrier is composed of the following components: 100 parts of polyvinyl alcohol, 500 parts of deionized water, 35 parts of formaldehyde, 30 parts of sulfuric acid, 103 parts of polyoxyethylene octyl phenol ether and 5 parts of oil shale semicoke.
The invention also provides a preparation method of the oil shale semicoke/polyvinyl alcohol composite immobilized carrier, which comprises the following process steps:
1) dissolving polyvinyl alcohol in deionized water to prepare a uniform and transparent polyvinyl alcohol solution;
2) adding the oil shale semi-coke into the polyvinyl alcohol solution, and stirring at high temperature to form a uniform mixed solution;
3) sequentially adding polyoxyethylene octyl phenol ether-10, sulfuric acid and formaldehyde into the mixed solution obtained in the step 2), stirring, curing and molding at high temperature, washing, cutting into blocks and drying to obtain the composite immobilized carrier.
Further, the polyvinyl alcohol is selected from one or more of 1750, 1788 or 1799 in molecular weight.
Further, the particle size of the oil shale semi-coke is 2-70 μm.
Further, the oil shale semi-coke is subjected to pre-treatment before calcination or surface modification.
Further, the pretreatment of the oil shale semi-coke at the early stage of calcination is specifically to calcine the oil shale semi-coke for 2-4 hours at 200-1000 ℃ in an air atmosphere or a nitrogen atmosphere, and then cool the oil shale semi-coke to obtain the oil shale semi-coke.
Further, the pretreatment of the oil shale semicoke at the early stage of surface modification specifically comprises the step of adding the oil shale semicoke into a modification solvent, wherein the solid-liquid weight ratio is 1: stirring at 25-80 ℃ for 4-12 h at 500-1000 rpm/min, centrifuging at 3000rpm/min for 15min, pouring out supernatant, washing with deionized water for 3-5 times, drying at 50-120 ℃ for 3-6 h, and grinding to 2-70 mu m;
further, the modified solvent is alcohol, a silane coupling agent, a quaternary ammonium salt solution or an ammonium salt solution.
Further, the composite immobilized carrier is porous sponge-shaped, the density is 0.22-0.30 g/cm3, the porosity is 60-92%, and the pore diameter is 1-4 mm.
The raw materials in the invention can be obtained by a commercial mode, wherein the polyoxyethylene octyl phenol ether-10 is referred to as OP-10 for short. The oil shale semicoke is pretreated in the early stage, so that the dispersion characteristic of the semicoke in polyvinyl alcohol can be improved, the porosity of the carrier is improved, and the carrier is endowed with better microorganism adhesion characteristic.
Compared with the prior art, the invention has the following characteristics and beneficial effects:
1) the polyvinyl acetal foam has the advantages of good opening performance, high hydrophilicity, good biocompatibility and the like;
2) the oil shale semi-coke has a lamellar microstructure, strong adsorption performance and good filling performance on organic polymers, can effectively adjust the density of a carrier, and can be directly put into the existing aeration tank to form carrier microorganisms with excellent pollutant treatment performance, thereby realizing the upgrading and reconstruction of the aeration tank.
3) The invention takes the polyvinyl acetal foam as a matrix and the oil shale semicoke as an inorganic filler to prepare the oil shale semicoke composite polyvinyl acetal foam microorganism immobilized carrier, can fix dominant strains which are selectively screened out, provides living organic matters and nutrient components, and improves the survival rate of sewage biochemical treatment population and the sewage treatment efficiency.
4) Because the oil shale semicoke is added in the traditional polyvinyl acetal foam processing process, the carrier has a cross-linked net-shaped structure and a strong-polarity water absorption surface, and has the huge adsorption capacity, organic matter content and nutritional ingredients of a nano material, so that the affinity and mass transfer performance of the foam carrier to microorganisms are improved, immobilized microorganisms can form a microenvironment which continuously changes from aerobic to anaerobic inside the carrier, and the variety, the biofilm formation rate, the survival rate and the pollutant treatment effect of the immobilized microorganisms are effectively improved.
5) The detection shows that the invention not only can effectively improve the porosity of the carrier material and perfect the pore structure, but also can improve the dimensional stability of the polyvinyl acetal foam and the water absorption rate of the carrier material, thereby strengthening the microorganism immobilization effect and the biochemical treatment performance.
6) The invention has the advantages of easily obtained raw materials, simple manufacturing process and low cost, and simultaneously solves the problem of environmental pollution caused by oil shale byproducts, so the invention has great application value and prospect in the field of sewage treatment.
Detailed Description
The principles and features of this invention are described in conjunction with the following embodiments, which are given by way of illustration only and are not intended to limit the scope of the invention.
Example 1 preparation of oil shale semicoke/polyvinyl alcohol composite Carrier
Weighing 100g of polyvinyl alcohol (1788) and dissolving in 500g of distilled water to prepare a uniform transparent polyvinyl alcohol solution; weighing 5g of oil shale semi-coke, adding the oil shale semi-coke into the solution, stirring the solution for 5min at a stirring speed of 500r/min, then sequentially adding 3g of OP-10, 30g of sulfuric acid and 35g of formaldehyde, adjusting the rotation speed to 1500r/min, foaming the solution for 10min, and then curing the solution in an oven at 70 ℃ for 3 h. Cooling, taking out, washing for several times, and washingDrying and cutting into blocks to obtain the oil shale semicoke/polyvinyl alcohol composite carrier, wherein the density of the composite carrier is 243kg/m3The water absorption capacity was 3.83g/g, and the porosity was 84%.
In a total volume of 0.14m3Adding 50% of reaction volume of oil shale semicoke/polyvinyl alcohol composite carrier into the self-made cylindrical plastic aeration barrel continuous flow reactor, adding pre-acclimated activated sludge according to the concentration of 5g/L, introducing chemical wastewater to enable the chemical wastewater to soak the carrier in the tank, and carrying out a microorganism immobilization film formation process under a stuffy aeration condition (namely the working state of stopping water inflow aeration). 10% of the wastewater in the tank is changed every day from the next day, and after 20 days, the microorganism immobilization and film formation process is completed. An immobilized carrier microorganism treatment system is formed in the reaction period, and the quality of the effluent is stable, which marks the successful start of the reactor. According to the test of GB18918-2002 discharge Standard of pollutants for municipal wastewater treatment plants, the COD (namely the chemical oxygen demand) of the inlet water is averagely 800mg/l and NH3The chemical wastewater with average-N (ammonia nitrogen) of 110mg/l and pH of 6-9 is biochemically treated for 16 hours to obtain effluent index COD<60mg/l，NH3-N<8mg/l, and meets the first grade B standard requirement of the standard.
Example 2
Firstly, the alcohol washing pretreatment of the oil shale semicoke: 20g of crude oil shale semicoke and 200g of absolute ethyl alcohol are weighed and mixed in a flask. Heating and refluxing in a water bath at 45 ℃ and stirring for 2 hours at the rotating speed of 500 r/min. Centrifuging at 3000r/min for 15min, pouring out supernatant, placing the rest solid substance into glass dish, oven drying at 105 deg.C for 4 hr, grinding, and sieving with 200 mesh sieve.
The procedure for the preparation of the alcohol washed char/polyvinyl alcohol was the same as in example 1, the inorganic phase being the alcohol washed pre-treated char. The density of the obtained oil shale semicoke/polyvinyl alcohol composite carrier is 210kg/m3The water absorption capacity was 3.61g/g, and the porosity was 89%.
The biochemical treatment method and the test method of the sewage are the same as those of example 1.
The COD of the inlet water is tested to be 648mg/l and NH on average3The average N is 68mg/l and the pH value is 7-8, the sewage is biochemically treated for 5 hours, and the effluent index COD is<50mg/l，NH3-N<5mg/l，SS<10mg/l, meets the first-class A standard requirement in GB18918-2002 discharge Standard of pollutants for municipal wastewater treatment plants.
Example 3
Firstly, calcining pretreatment of oil shale semicoke: weighing 20g of crude oil shale semicoke, placing the crude oil shale semicoke in a crucible, evenly spreading, placing the crucible in an induction resistance furnace, calcining for 2 hours in an air atmosphere at 900 ℃, and then turning off a power supply to cool the crucible along with the furnace.
Taking out, grinding and sieving with a 200-mesh sieve.
The calcined semicoke/polyvinyl alcohol was prepared in the same manner as in example 1, the inorganic phase being the calcined pretreated semicoke. The density of the obtained oil shale semicoke/polyvinyl alcohol composite carrier is 189kg/m3The water absorption capacity was 3.41g/g, and the porosity was 91%.
The biochemical treatment method and the test method of the sewage are the same as those of example 1.
The COD of the inlet water is tested to be 480mg/l and NH on average3The average N is 62mg/l and the pH value is 7-8, the sewage is biochemically treated for 8 hours, and the effluent index COD is<50mg/l，NH3-N<5mg/l，SS<10mg/l, which meets the first class A standard in the standard.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (7)
1. The oil shale semicoke/polyvinyl alcohol composite immobilization carrier is characterized by comprising the following components: 100 parts of polyvinyl alcohol, 400-1400 parts of deionized water, 10-50 parts of aldehyde, 30-40 parts of sulfuric acid, 102-5 parts of polyoxyethylene octyl phenol ether and 1-50 parts of oil shale semicoke.
2. The oil shale semicoke/polyvinyl alcohol composite immobilization carrier as claimed in claim 1, wherein the composite immobilization carrier is composed of the following components: 100 parts of polyvinyl alcohol, 500 parts of deionized water, 35 parts of formaldehyde, 30 parts of sulfuric acid, 103 parts of polyoxyethylene octyl phenol ether and 5 parts of oil shale semicoke.
3. The preparation method of the oil shale semicoke/polyvinyl alcohol composite immobilization carrier according to claim 1 or 2, characterized by comprising the following process steps:
1) dissolving polyvinyl alcohol in deionized water to prepare a uniform and transparent polyvinyl alcohol solution;
2) adding the oil shale semi-coke into the polyvinyl alcohol solution, and stirring at a stirring speed of 500-1000 rpm/min at a temperature of 25-95 ℃ to obtain a uniform mixed solution;
3) sequentially adding polyoxyethylene octyl phenol ether-10, sulfuric acid with the concentration of 50-70 percent and formaldehyde with the concentration of 36-40 percent into the mixed solution obtained in the step 2), stirring at the speed of 500-3000 rpm/min, curing and forming at 70 ℃, washing, cutting into blocks and drying to obtain the composite immobilized carrier, wherein the composite immobilized carrier is porous sponge-shaped and has the density of 0.22-0.30 g/cm3The porosity is 60-92%, and the pore diameter is 1-4 mm.
4. The preparation method of the oil shale semicoke/polyvinyl alcohol composite immobilization carrier according to claim 3, wherein the polyvinyl alcohol is selected from one or more of 1750, 1788 and 1799 in molecular weight.
5. The preparation method of the oil shale semicoke/polyvinyl alcohol composite immobilized carrier according to claim 3, wherein the particle size of the oil shale semicoke is 2-70 μm, and the oil shale semicoke is subjected to pre-treatment before calcination or surface modification.
6. The preparation method of the oil shale semicoke/polyvinyl alcohol composite immobilized carrier according to claim 5, wherein the pretreatment before calcination of the oil shale semicoke is specifically to calcine the oil shale semicoke for 1-4h at 200-1000 ℃ in an air atmosphere or a nitrogen atmosphere, and then cool the oil shale semicoke.
7. The preparation method of the oil shale semicoke/polyvinyl alcohol composite immobilized carrier according to claim 5, wherein the pretreatment of the oil shale semicoke at the early stage of surface modification is to add the oil shale semicoke into a modification solvent, and the solid-liquid weight ratio is 1: stirring at 25-80 ℃ for 4-12 h at 500-1000 rpm/min, centrifuging at 3000rpm/min for 15min, pouring out supernatant, washing with deionized water for 3-5 times, drying at 50-120 ℃ for 3-6 h, and grinding to 2-70 mu m, wherein the modified solvent is alcohol, a silane coupling agent, a quaternary ammonium salt solution or an ammonium salt solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113058565A (en) * | 2021-03-19 | 2021-07-02 | 兰州交通大学 | Method for preparing adsorbent with good adsorption performance by using carbon fiber and chitosan as raw materials |
| CN113943438A (en) * | 2021-11-08 | 2022-01-18 | 中国科学院兰州化学物理研究所 | Preparation method of oil shale semicoke/sodium alginate composite cross-linked membrane |
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Cited By (3)
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