CN114477326A - Demulsification coalescence material for oil sludge in coal chemical industry wastewater - Google Patents
Demulsification coalescence material for oil sludge in coal chemical industry wastewater Download PDFInfo
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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
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- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/04—Breaking emulsions
- B01D17/048—Breaking emulsions by changing the state of aggregation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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- C02F2001/007—Processes including a sedimentation step
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
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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
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Abstract
The invention discloses a demulsification coalescence material for oil sludge in coal chemical industry wastewater, which comprises a demulsification material LY-01 and a coalescence material LY-02; the demulsification material LY-01 is used for performing demulsification treatment on oil sludge substances in coal chemical wastewater to be treated so as to enable the oil sludge substances to be coalesced to form aggregates with smaller volume, and is prepared by adopting quaternary ammonium salt cationic monomers, oleophylic hydrophobic monomers and polyalcohol amine; the coalescence material LY-02 is used for coalescing the aggregates with smaller volumes to form aggregates with larger volumes, and is prepared by adopting gelatin, a magnetic powder material, citric acid and a demulsification material LY-01; according to the invention, through the synergistic effect of the demulsification material LY-01 and the coalescence material LY-02, oil sludge substances in the coal chemical industry wastewater are subjected to demulsification and coalescence, so that the oil sludge in the coal chemical industry wastewater is efficiently treated; the sludge-water separation effect is enhanced, the water content of the oil sludge is reduced, and the overall effluent quality is improved.
Description
Technical Field
The invention belongs to the technical field of pretreatment of coal chemical industry wastewater, and particularly relates to a demulsification coalescence material for oil sludge in coal chemical industry wastewater.
Background
More than 300 pollutants are contained in the coal chemical industry wastewater, including oil sludge, tar, phenol, ammonia nitrogen, nitrogen and sulfur-containing heterocyclic compounds and other pollutants; wherein, the oil sludge is the problem which is mainly solved in the pretreatment of the pollutants in the coal chemical industry wastewater; if the pretreatment process of the coal chemical wastewater has a poor oil sludge removal effect, the recovery difficulty of subsequent oil, phenol and ammonia is increased, the recovery efficiency is reduced, the serious waste of resources is caused, and the subsequent biochemical treatment is also difficult.
At present, the method for removing the oil sludge in the coal chemical industry wastewater mainly adopts gravity settling and flocculation methods to remove the oil sludge; with the development of the novel coal chemical industry, the continuous updating of production processes and products, pollutants in wastewater are more and more complicated; the use of the existing flocculating agent not only increases the dosage of the agent more and more, but also increases the operation cost more and more; and the use of the conventional medicament is difficult to meet the requirement of pretreatment of the coal chemical wastewater.
In conclusion, the invention aims to develop a demulsification coalescence material aiming at oil sludge in coal chemical industry wastewater so as to solve the problem of removing oil sludge pretreated by the coal chemical industry wastewater.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a demulsification coalescence material for oil sludge in coal chemical industry wastewater, which aims to solve the problems that the conventional agent consumption is large and the pretreatment requirement of the coal chemical industry wastewater is difficult to meet in the existing process of removing the oil sludge in the coal chemical industry wastewater by adopting a gravity settling or flocculation method.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a demulsification coalescence material for oil sludge in coal chemical industry wastewater, which comprises a demulsification material LY-01 and a coalescence material LY-02;
the demulsification material LY-01 is used for performing demulsification treatment on oil sludge substances in the coal chemical industry wastewater to be treated so as to enable the oil sludge substances to be aggregated to form aggregates with smaller volume; the demulsification material LY-01 is prepared from a quaternary ammonium salt cationic monomer, an oleophylic hydrophobic monomer and polyalcohol amine;
the coalescing material LY-02 for coalescing the smaller volume of aggregates to form a larger volume of coalesced bodies; wherein the coalescence material LY-02 is prepared from gelatin, a magnetic powder material, citric acid and a demulsification material LY-01.
Further, the preparation process of the demulsification material LY-01 comprises the following specific steps:
mixing a quaternary ammonium salt cationic monomer, an oleophylic hydrophobic monomer and polyalcohol amine to prepare a mixed solution;
adding an introducing agent into the mixed solution to carry out polymerization reaction to obtain a polymerization reaction product;
adding a cross-linking agent into the polymerization reaction product to carry out cross-linking polymerization reaction to obtain a cross-linked polymerization product;
and separating and purifying the crosslinked polymerization product to obtain the demulsification material LY-01.
Further, the quaternary ammonium salt cationic monomer is one of dimethyl diallyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride and methacrylamidoalkyl ammonium chloride; the oleophylic and hydrophobic monomer is one of lauryl methacrylate, isodecyl methacrylate and butyl methacrylate; the polyalcohol amine is polytriethanolamine.
Further, the process of mixing the quaternary ammonium salt cationic monomer, the oleophilic hydrophobic monomer and the polyalcohol amine to prepare the mixed solution comprises the following specific steps:
mixing quaternary ammonium salt cationic monomer, oleophylic hydrophobic monomer and polyalcohol amine to obtain a mixed system; wherein, in the mixed system, the mass percent of the quaternary ammonium salt cationic monomer is 30-50%, the mass percent of the oleophylic hydrophobic monomer is 20-30%, and the mass percent of the polyalcohol amine is 40-60%;
under the condition of water bath, deionized water is added into the mixed system, stirred and dissolved, and then the pH is adjusted to be neutral until the deionized water is completely dissolved, so that a mixed solution is obtained.
Further, a process of adding an introducing agent into the mixed solution to perform a polymerization reaction to obtain a polymerization reaction product is as follows:
adding an initiator into the mixed solution, and stirring at a constant speed to obtain a polymerization reaction system; adjusting the temperature of a polymerization reaction system to 50-70 ℃, introducing nitrogen into the polymerization reaction system, uniformly mixing, and carrying out closed reaction for 1-2h to obtain a polymerization reaction product;
wherein, the initiator adopts one of ammonium persulfate, potassium persulfate and hydrogen peroxide; the mass percentage of the initiator in the polymerization reaction system is 1-5%.
Further, a cross-linking agent is added into the polymerization reaction product to perform cross-linking polymerization reaction, and the process of obtaining the cross-linked polymerization product is as follows:
adding a cross-linking agent into the polymerization reaction product, and stirring at a constant speed to obtain a cross-linking polymerization reaction system; adjusting the temperature of a crosslinking polymerization reaction system to 70-90 ℃, introducing nitrogen into the crosslinking polymerization reaction system, uniformly mixing, carrying out closed reaction for 4-7h, and cooling to room temperature after complete reaction to obtain a crosslinking polymerization product; wherein, the cross-linking agent is one of ethylenediamine, n-butylamine and polyethylene polyamine.
Further, the process of separating and purifying the crosslinked polymer product to obtain the demulsification material LY-01 comprises the following steps:
washing, centrifugally separating and purifying the crosslinked polymer product to obtain a purified product; and (3) carrying out cold drying, crushing and screening on the purified product to obtain the demulsification material LY-01.
Further, the preparation process of the coalescence material LY-02 is as follows:
dissolving gelatin in water to obtain gelatin solution; adding a magnetic powder material and citric acid into the gelatin solution, and performing ultrasonic stirring to obtain a magnetic colloid;
adding the demulsifying material LY-01 into a magnetic colloid, and stirring to obtain a black solution;
and (3) carrying out magnetic adsorption separation on the black solution to obtain a separation product, washing the separation product, and carrying out cold dry grinding on the separation product into powder to obtain the agglomeration material LY-02.
Further, dissolving gelatin in water to obtain a gelatin solution; adding a magnetic powder material and citric acid into a gelatin solution, and performing ultrasonic stirring to obtain a magnetic colloid, wherein the mass fraction of the gelatin is 3% -7%, the mass fraction of the magnetic powder material is 5% -15%, and the mass fraction of the citric acid is 2% -5%; wherein the magnetic powder material is one of iron oxide magnetic powder, chromium dioxide magnetic powder and metal magnetic powder.
Further, the demulsifying material LY-01 is added into the magnetic colloid and stirred to obtain a black solution, and the process is as follows:
under the condition of constant-temperature water bath, adding the demulsifying material LY-01 into the magnetic colloid, and stirring to obtain a black solution; wherein the temperature of the constant-temperature water bath is 30-40 ℃; the mass ratio of the demulsifying material LY-01 to the magnetic colloid is 1 (10-30).
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a demulsification coalescence material for oil sludge in coal chemical industry wastewater, wherein the demulsification material LY-01 is prepared from a quaternary ammonium salt cationic monomer, an oleophylic hydrophobic monomer and polyalcohol amine; the demulsification material LY-01 is a high molecular compound which carries a large number of positive charge groups, has unique oleophylic and hydrophobic properties and has a rich chain structure on the surface; the oil-water interface emulsion can efficiently neutralize the surface negative charges of colloidal particles of oil sludge substances, destroy the stability of the oil sludge substances, and enable the oil sludge substances to be rapidly adsorbed on an oil-water interface through the interaction force among molecules, thereby destroying the O/W emulsion, replacing a surfactant and asphaltene molecules, reducing the interface tension and the interface film strength of oil water, promoting the rapid generation of the agglomeration effect among oil sludge substances, and enhancing the coalescence effect among small oil sludge particles; the coalescence material LY-02 is obtained by modifying the demulsification material LY-01 by using a magnetic material in a magnetic colloid, and the coalescence material is used as a macromolecular surfactant with excellent performance, has rich branched chain structures and specific functional groups, can coalesce oil sludge particles dispersed in water, and has a strong promotion effect on the rapid separation of an oil phase, a water phase and a sludge phase in the coal chemical industry wastewater; adding a demulsifying material LY-01 and a coalescing material LY-02 into wastewater to be treated, wherein the surfaces of the demulsifying material LY-01 and the coalescing material LY-02 are both provided with abundant positive charges and branched structures, so that colloidal substance particles with negative charges in the wastewater are destabilized, and aggregates with smaller volume are coalesced by utilizing the coalescing performance of the coalescing material LY-02 to form a coalescent body with larger volume; oil sludge substances in the coal chemical industry wastewater are subjected to demulsification and coalescence through the synergistic effect of the demulsification material LY-01 and the coalescence material LY-02, and finally, separation and removal of oil sludge are realized; the method is more beneficial to removing the oil sludge in the coal chemical industry wastewater, simultaneously reduces the sludge yield, enhances the sludge-water separation effect, reduces the water content of the oil sludge, improves the overall effluent quality, and realizes the efficient treatment of the oil sludge in the coal chemical industry wastewater.
Furthermore, in the preparation process of the demulsification material LY-01, the addition of the initiator and the cross-linking agent is less, the demulsification material is nontoxic and harmless, the initiation and cross-linking efficiency is high, the fracture of chemical bonds in monomers can be accelerated, the synthesis of new compounds can be promoted, and the demulsification material LY-01 is energy-saving, environment-friendly, practical and safe.
Furthermore, the demulsification material LY-01 is prepared from a quaternary ammonium salt cationic monomer, an oleophylic hydrophobic monomer and polyalcohol amine, the coalescence material LY-02 is prepared from gelatin, a magnetic powder material, citric acid and the demulsification material LY-01, the raw materials are all easily available commercial materials, the price is low, the whole production process is simple, the cost is low, the product is environment-friendly and nuisanceless, and can be recycled, and secondary pollution can not be generated; simple preparation process and low requirement on equipment.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects of the present invention more apparent, the following embodiments further describe the present invention in detail. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention relates to a demulsification and coalescence material for oil sludge in coal chemical industry wastewater, which comprises a demulsification material LY-01 and a coalescence material LY-02; the demulsification material LY-01 is used for performing demulsification treatment on oil sludge substances in the coal chemical industry wastewater to be treated so as to enable the oil sludge substances to be aggregated to form aggregates with smaller volume; the demulsification material LY-01 is prepared from a quaternary ammonium salt cationic monomer, an oleophylic hydrophobic monomer and polyalcohol amine; the coalescing material LY-02 for coalescing the smaller volume of aggregates to form a larger volume of coalesced bodies; wherein the coalescence material LY-02 is prepared from gelatin, a magnetic powder material, citric acid and a demulsification material LY-01.
In the invention, the preparation process of the demulsification material LY-01 comprises the following specific steps:
step 1, mixing a quaternary ammonium salt cationic monomer, an oleophylic hydrophobic monomer and polyalcohol amine, and preparing a mixed solution under the condition of adjusting price in a water bath; the preparation process comprises the following specific steps:
step 11, mixing a quaternary ammonium salt cationic monomer, an oleophylic hydrophobic monomer and polyalcohol amine to obtain a mixed system; in the mixed system, the mass percent of quaternary ammonium salt cationic monomer is 30-50%, the mass percent of oleophylic hydrophobic monomer is 20-30%, and the mass percent of polyalcohol amine is 40-60%; wherein, the quaternary ammonium salt cationic monomer is one of dimethyl diallyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride and methacrylamidoalkyl ammonium chloride; the oleophylic and hydrophobic monomer is one of lauryl methacrylate, isodecyl methacrylate and butyl methacrylate; the polyalcohol amine is polytriethanolamine.
And step 12, adding deionized water into the mixed system under the water bath condition, stirring and dissolving, and then adjusting the pH value to be neutral until the deionized water is completely dissolved to obtain a mixed solution.
Step 2, adding an introducing agent into the mixed solution to carry out polymerization reaction to obtain a polymerization reaction product; specifically, adding an initiator into the mixed solution, and stirring at a constant speed to obtain a polymerization reaction system; adjusting the temperature of the polymerization reaction system to 50-70 ℃, introducing nitrogen into the polymerization reaction system, uniformly mixing, and carrying out closed reaction for 1-2h to obtain a polymerization reaction product.
Wherein, the initiator adopts one of ammonium persulfate, potassium persulfate and hydrogen peroxide; the mass percentage of the initiator in the polymerization reaction system is 1-5%.
Step 3, adding a cross-linking agent into the polymerization reaction product, and stirring at a constant speed to obtain a cross-linking polymerization reaction system; adjusting the temperature of a crosslinking polymerization reaction system to 70-90 ℃, introducing nitrogen into the crosslinking polymerization reaction system, uniformly mixing, carrying out closed reaction for 4-7h, and cooling to room temperature after complete reaction to obtain a crosslinking polymerization product; wherein the crosslinking agent is one of ethylenediamine, n-butylamine and polyethylene polyamine.
Step 4, separating and purifying the crosslinked polymerization product to obtain the demulsification material LY-01; wherein, the separation and purification process is as follows:
washing, centrifugally separating and purifying the crosslinked polymer product to obtain a purified product; the purified product is subjected to cold drying, crushing and screening to obtain the demulsification material LY-01; wherein, the freeze drying process adopts the step of placing the purified product in a freeze dryer for freeze drying treatment.
In the invention, the preparation process of the coalescence material LY-02 is as follows:
s1, taking 3-7% of gelatin, 70-90% of deionized water, 5-15% of magnetic powder material and 2-5% of citric acid by mass; dissolving gelatin in deionized water to obtain a gelatin solution; adding a magnetic powder material and citric acid into the gelatin solution, and performing ultrasonic stirring to obtain a magnetic colloid; wherein the magnetic powder material is one of metal magnetic powder in iron oxide magnetic powder and chromium dioxide magnetic powder.
S2, adding the demulsifying material LY-01 into a magnetic colloid under the condition of a constant-temperature water bath at the temperature of 30-40 ℃, and stirring to obtain a black solution; wherein the mass ratio of the demulsifying material LY-01 to the magnetic colloid is 1 (10-30); the stirring speed is 400-700r/min, and the stirring time is 12-24 h.
S3, carrying out magnetic adsorption separation on the black solution to obtain a separation product, washing the separation product, and carrying out cold dry grinding on the separation product into powder to obtain the coalescence material LY-02; wherein, the speed of magnetic adsorption separation is 5000r/min, and the time is 10 min.
According to the demulsification coalescence material for the oil sludge in the coal chemical industry wastewater, quaternary ammonium salt cationic monomers, oleophylic hydrophobic monomers, polyalcohol amine, an initiator, a cross-linking agent, gelatin, magnetic powder and citric acid are used as raw materials in the preparation process, and the raw materials are all easily available commercial materials, so that the material is low in price, simple in production and preparation process, low in cost, environment-friendly and pollution-free, can be recycled, and cannot generate secondary pollution; the demulsifying material LY-01 and the coalescing material LY-02 obtained by preparation have the characteristic of low requirements on equipment, and have a good effect on removal of oil sludge when the oil sludge substances in the coal chemical industry wastewater are cooperatively treated; meanwhile, the demulsifying material LY-01 and the coalescing material LY-02 can carry part of toxic and harmful substances such as heavy metals and aromatic hydrocarbon substances existing in the coal chemical industry wastewater while destabilizing and coagulating insoluble solid particles, and are removed by separating oil sludge.
According to the invention, when the demulsification coalescence material is used for removing oil sludge substances in the coal chemical industry wastewater, the low efficiency and insufficient gravity settling of the existing pretreatment process of the coal chemical industry wastewater are improved; meanwhile, in order to meet the requirement of continuously improved effluent quality, a quaternary ammonium salt monomer, an oleophylic hydrophobic monomer and a polymeric polyol are copolymerized, and a demulsification material LY-01 with rich positive charges is prepared by virtue of the neutralization effect of quaternary ammonium salt cationic charges, the bridging effect of long-chain molecules and the like; on the basis of the demulsification material LY-01, combining the magnetic powder material with the gel, and copolymerizing the magnetic powder material with the demulsification material LY-01 by adopting a copolymerization method to prepare a magnetic coalescence material LY-02; the demulsifying material LY-01 and the coalescing material LY-02 in the invention have synergistic effect to thoroughly remove the oil sludge in the coal chemical industry wastewater, thereby obviously improving the purpose of oil sludge separation effect.
In the invention, the surfaces of the demulsifying material LY-01 and the coalescing material LY-02 are provided with abundant positive charges and branched structures; wherein, ions with positive charges destabilize colloid particles with negative charges in the coal chemical industry wastewater, aggregates with smaller volume are aggregated into aggregates with larger volume by utilizing the aggregation performance of the aggregation material LY-02, and oil sludge is aggregated under the synergistic action of the aggregates and the aggregates, and then is removed by magnetic separation; the method is more beneficial to removing the oil sludge in the coal chemical industry wastewater, simultaneously reduces the sludge yield, enhances the sludge-water separation effect, reduces the water content of the oil sludge, improves the overall effluent quality, and realizes the efficient treatment of the oil sludge in the coal chemical industry wastewater.
Example 1
The embodiment 1 provides a demulsification coalescing material for oil sludge in coal chemical industry wastewater, which specifically comprises the following steps:
step 1, weighing dimethyl diallyl ammonium chloride, methacrylic acid and polytriethanolamine, and adding into a three-neck flask under a water bath condition to obtain a mixed system; wherein, in the mixed system, the mass percent of the dimethyl diallyl ammonium chloride is 30%, the mass percent of the methacrylic acid is 20%, and the mass percent of the polytriethanolamine is 50%.
Step 2, adding deionized water into the mixed system, stirring for dissolving, then adding ammonia water for adjusting the pH value to be neutral until the ammonia water is completely dissolved to obtain a mixed solution; wherein the mass fraction of the ammonia water is 25%.
Step 3, adding potassium persulfate into the mixed solution, and stirring at a constant speed to obtain a polymerization reaction system; wherein, potassium persulfate is used as an initiator; in a polymerization reaction system, the mass fraction of potassium persulfate is 1 percent; and adjusting the temperature of the polymerization reaction system to 50 ℃, introducing nitrogen into the polymerization reaction system, uniformly mixing, and carrying out closed reaction for 1h to obtain a polymerization reaction product.
Step 4, adding ethylenediamine into the polymerization reaction product, and stirring at a constant speed to obtain a cross-linking polymerization reaction system; adjusting the temperature of the crosslinking polymerization reaction system to 70 ℃; introducing nitrogen into the crosslinking polymerization reaction system, uniformly mixing, carrying out closed reaction for 4 hours, and cooling to room temperature after the reaction is completed to obtain a crosslinking polymerization product; wherein, the ethylene diamine is used as an initiator, and the mass fraction of the ethylene diamine in a crosslinking polymerization reaction system is 2%.
Step 5, washing the crosslinked polymer product by adopting absolute ethyl alcohol and acetone, centrifugally separating, and purifying to obtain a purified product; and (3) carrying out freeze drying, crushing and screening on the purified product by using a freezing drying agent to obtain the demulsification material LY-01.
Step 6, dissolving gelatin in deionized water to obtain a gelatin solution; adding a ferromagnetic oxide powder material and citric acid into a gelatin solution to obtain a mixed system, and carrying out ultrasonic stirring on the mixed system to obtain a magnetic colloid; in the mixed system, the mass fraction of gelatin is 3%, the mass fraction of deionized water is 90%, the mass fraction of magnetic powder material is 5%, and the mass fraction of citric acid is 2%.
Step 7, adding the demulsifying material into the magnetic colloid in a constant-temperature water bath kettle at the temperature of 30 ℃, and stirring and reacting at the speed of 400-700r/min for 12 hours to obtain a black solution; wherein the mass ratio of the demulsifying material to the magnetic colloid is 1: 10.
And 8, carrying out magnetic adsorption separation on the black solution to obtain a separation product, washing the separation product for multiple times by using ethanol-acetone, and carrying out cold drying and grinding to obtain black powder to obtain the aggregation material LY-02.
Example 2
The embodiment 2 provides a demulsification coalescing material for oil sludge in coal chemical industry wastewater, which specifically comprises the following steps:
step 1, weighing dimethyl diallyl ammonium chloride, lauryl methacrylate and polytriethanolamine according to requirements, and adding into a three-neck flask under the condition of water bath to obtain a mixed system; wherein, in the mixed system, the mass percent of the dimethyl diallyl ammonium chloride is 40%, the mass percent of the lauryl methacrylate is 20%, and the mass percent of the polytriethanolamine is 40%.
Step 2, adding deionized water into the mixed system, stirring for dissolving, then adding ammonia water for adjusting the pH value to be neutral until the ammonia water is completely dissolved to obtain a mixed solution; wherein the mass fraction of the ammonia water is 25%.
Step 3, adding potassium persulfate into the mixed solution, and stirring at a constant speed to obtain a polymerization reaction system; wherein, potassium persulfate is used as an initiator; in a polymerization reaction system, the mass fraction of potassium persulfate is 5 percent; and (3) adjusting the temperature of the polymerization reaction system to 60 ℃, introducing nitrogen into the polymerization reaction system, uniformly mixing, and carrying out closed reaction for 2 hours to obtain a polymerization reaction product.
Step 4, adding ethylenediamine into the polymerization reaction product, and stirring at a constant speed to obtain a cross-linking polymerization reaction system; adjusting the temperature of the crosslinking polymerization reaction system to 90 ℃; introducing nitrogen into the crosslinking polymerization reaction system, uniformly mixing, carrying out closed reaction for 7 hours, and cooling to room temperature after the reaction is completed to obtain a crosslinking polymerization product; wherein, the ethylene diamine is used as an initiator, and the mass fraction of the ethylene diamine in a crosslinking polymerization reaction system is 3 percent.
Step 5, washing the crosslinked polymer product by adopting absolute ethyl alcohol and acetone, centrifugally separating, and purifying to obtain a purified product; and (3) carrying out freeze drying, crushing and screening on the purified product by using a freezing drying agent to obtain the demulsification material LY-01.
Step 6, dissolving gelatin in deionized water to obtain a gelatin solution; adding chromium dioxide magnetic powder material and citric acid into gelatin solution to obtain a mixed system, and carrying out ultrasonic stirring on the mixed system to obtain magnetic colloid; in the mixed system, the mass fraction of gelatin is 5%, the mass fraction of deionized water is 80%, the mass fraction of magnetic powder material is 10%, and the mass fraction of citric acid is 5%.
Step 7, adding the demulsifying material into the magnetic colloid in a constant-temperature water bath kettle at 40 ℃, and stirring and reacting at the speed of 400-700r/min for 24 hours to obtain a black solution; wherein the mass ratio of the demulsifying material to the magnetic colloid is 1: 20. Suggested mass ratio relationship between the two.
And 8, carrying out magnetic adsorption separation on the black solution to obtain a separation product, washing the separation product for multiple times by using ethanol-acetone, and carrying out cold drying and grinding to obtain black powder to obtain the aggregation material LY-02.
Example 3
The embodiment 3 provides a demulsification coalescing material for oil sludge in coal chemical industry wastewater, which specifically comprises the following steps:
step 1, weighing methacryloyloxyethyl trimethyl ammonium chloride, isodecyl methacrylate and polytriethanolamine according to requirements, and adding the weighed materials into a three-neck flask under the condition of water bath to obtain a mixed system; wherein, in the mixed system, the mass percent of the methacryloyloxyethyl trimethyl ammonium chloride is 40%, the mass percent of the methacrylic acid isodecyl ester is 20%, and the mass percent of the polytriethanolamine is 40%.
Step 2, adding deionized water into the mixed system, stirring for dissolving, then adding ammonia water for adjusting the pH value to be neutral until the ammonia water is completely dissolved to obtain a mixed solution; wherein the mass fraction of the ammonia water is 25%.
Step 3, adding ammonium persulfate into the mixed solution, and stirring at a constant speed to obtain a polymerization reaction system; wherein, ammonium persulfate is taken as an initiator; in a polymerization reaction system, the mass fraction of ammonium persulfate is 2%; and adjusting the temperature of the polymerization reaction system to 60 ℃, introducing nitrogen into the polymerization reaction system, uniformly mixing, and carrying out closed reaction for 1h to obtain a polymerization reaction product.
Step 4, adding n-butylamine into the polymerization reaction product, and stirring at a constant speed to obtain a cross-linking polymerization reaction system; adjusting the temperature of the crosslinking polymerization reaction system to 80 ℃; introducing nitrogen into the crosslinking polymerization reaction system, uniformly mixing, carrying out closed reaction for 6 hours, and cooling to room temperature after the reaction is completed to obtain a crosslinking polymerization product; wherein, the n-butylamine is used as an initiator, and the mass fraction of the n-butylamine is 1% in a crosslinking polymerization reaction system.
Step 5, washing the crosslinked polymer product by adopting absolute ethyl alcohol and acetone, centrifugally separating, and purifying to obtain a purified product; and (3) carrying out freeze drying, crushing and screening on the purified product by using a freezing drying agent to obtain the demulsification material LY-01.
Step 6, dissolving gelatin in deionized water to obtain a gelatin solution; adding a metal magnetic powder material and citric acid into the gelatin solution to obtain a mixed system, and carrying out ultrasonic stirring on the mixed system to obtain a magnetic colloid; in the mixed system, the mass fraction of gelatin is 4%, the mass fraction of deionized water is 85%, the mass fraction of magnetic powder material is 8%, and the mass fraction of citric acid is 3%.
Step 7, adding the demulsifying material into the magnetic colloid in a constant-temperature water bath kettle at the temperature of 35 ℃, and stirring and reacting at the speed of 400-700r/min for 12 hours to obtain a black solution; wherein the mass ratio of the demulsifying material to the magnetic colloid is 1: 25.
And 8, carrying out magnetic adsorption separation on the black solution to obtain a separation product, washing the separation product for multiple times by using ethanol-acetone, and carrying out cold drying and grinding to obtain black powder to obtain the aggregation material LY-02.
Example 4
The embodiment 4 provides a demulsification coalescing material for oil sludge in coal chemical industry wastewater, which specifically comprises the following steps:
step 1, weighing dimethyl diallyl ammonium chloride, isodecyl methacrylate and polytriethanolamine according to requirements, and adding into a three-neck flask under the condition of water bath to obtain a mixed system; wherein, in the mixed system, the mass percent of the dimethyl diallyl ammonium chloride is 30%, the mass percent of the methacrylic acid isodecyl ester is 30%, and the mass percent of the polytriethanolamine is 40%.
Step 2, adding deionized water into the mixed system, stirring for dissolving, then adding ammonia water for adjusting the pH value to be neutral until the ammonia water is completely dissolved to obtain a mixed solution; wherein the mass fraction of the ammonia water is 25%.
Step 3, adding ammonium persulfate into the mixed solution, and stirring at a constant speed to obtain a polymerization reaction system; wherein, ammonium persulfate is taken as an initiator; in a polymerization reaction system, the mass fraction of ammonium persulfate is 4%; and adjusting the temperature of the polymerization reaction system to 60 ℃, introducing nitrogen into the polymerization reaction system, uniformly mixing, and carrying out closed reaction for 2 hours to obtain a polymerization reaction product.
Step 4, adding n-butylamine into the polymerization reaction product, and stirring at a constant speed to obtain a cross-linking polymerization reaction system; adjusting the temperature of a crosslinking polymerization reaction system to 85 ℃; introducing nitrogen into the crosslinking polymerization reaction system, uniformly mixing, carrying out closed reaction for 7 hours, and cooling to room temperature after the reaction is completed to obtain a crosslinking polymerization product; wherein, the n-butylamine is used as an initiator, and the mass fraction of the n-butylamine is 2% in a crosslinking polymerization reaction system.
Step 5, washing the crosslinked polymer product by adopting absolute ethyl alcohol and acetone, carrying out centrifugal separation and purification treatment to obtain a purified product; and (3) carrying out freeze drying, crushing and screening on the purified product by using a freezing drying agent to obtain the demulsification material LY-01.
Step 6, dissolving gelatin in deionized water to obtain a gelatin solution; adding a ferromagnetic oxide powder material and citric acid into a gelatin solution to obtain a mixed system, and carrying out ultrasonic stirring on the mixed system to obtain a magnetic colloid; in the mixing system, the mass fraction of gelatin is 7%, the mass fraction of deionized water is 75%, the mass fraction of magnetic powder material is 13%, and the mass fraction of citric acid is 5%.
Step 7, adding the demulsifying material into the magnetic colloid in a constant-temperature water bath kettle at 40 ℃, and stirring and reacting at the speed of 400-700r/min for 24 hours to obtain a black solution; wherein the mass ratio of the demulsifying material to the magnetic colloid is 1: 30.
And 8, carrying out magnetic adsorption separation on the black solution to obtain a separation product, washing the separation product for multiple times by using ethanol-acetone, and carrying out cold drying and grinding to obtain black powder to obtain the aggregation material LY-02.
Example 5
The embodiment 5 provides a demulsification coalescing material for oil sludge in coal chemical industry wastewater, which specifically comprises the following steps:
step 1, weighing methacrylamidoalkyl ammonium chloride, butyl methacrylate and polytriethanolamine according to requirements, and adding the weighed materials into a three-neck flask under the condition of water bath to obtain a mixed system; wherein, in the mixed system, the mass percent of the methacrylamide alkyl ammonium chloride is 35%, the mass percent of the butyl methacrylate is 25%, and the mass percent of the polytriethanolamine is 40%.
Step 2, adding deionized water into the mixed system, stirring for dissolving, then adding ammonia water for adjusting the pH value to be neutral until the ammonia water is completely dissolved to obtain a mixed solution; wherein the mass fraction of the ammonia water is 25%.
Step 3, adding hydrogen peroxide into the mixed solution, and stirring at a constant speed to obtain a polymerization reaction system; wherein, hydrogen peroxide is used as an initiator; in a polymerization reaction system, the mass fraction of hydrogen peroxide is 3 percent; and adjusting the temperature of the polymerization reaction system to 55 ℃, introducing nitrogen into the polymerization reaction system, uniformly mixing, and carrying out closed reaction for 1h to obtain a polymerization reaction product.
Step 4, adding polyethylene polyamine into the polymerization reaction product, and stirring at a constant speed to obtain a crosslinking polymerization reaction system; adjusting the temperature of the crosslinking polymerization reaction system to 75 ℃; introducing nitrogen into the crosslinking polymerization reaction system, uniformly mixing, carrying out closed reaction for 4 hours, and cooling to room temperature after the reaction is completed to obtain a crosslinking polymerization product; wherein, polyethylene polyamine is used as an initiator, and the mass fraction of the polyethylene polyamine in a crosslinking polymerization reaction system is 1 percent.
Step 5, washing the crosslinked polymer product by adopting absolute ethyl alcohol and acetone, centrifugally separating, and purifying to obtain a purified product; and (3) carrying out freeze drying, crushing and screening on the purified product by using a freezing drying agent to obtain the demulsification material LY-01.
Step 6, dissolving gelatin in deionized water to obtain a gelatin solution; adding a ferromagnetic oxide powder material and citric acid into a gelatin solution to obtain a mixed system, and carrying out ultrasonic stirring on the mixed system to obtain a magnetic colloid; in the mixing system, the mass fraction of gelatin is 5%, the mass fraction of deionized water is 84%, the mass fraction of magnetic powder material is 8%, and the mass fraction of citric acid is 3%.
Step 7, adding the demulsifying material into the magnetic colloid in a constant-temperature water bath kettle at the temperature of 35 ℃, and stirring and reacting at the speed of 400-700r/min for 12 hours to obtain a black solution; wherein the mass ratio of the demulsifying material to the magnetic colloid is 1: 15.
And 8, carrying out magnetic adsorption separation on the black solution to obtain a separation product, washing the separation product for multiple times by using ethanol-acetone, and carrying out cold drying and grinding to obtain black powder to obtain the aggregation material LY-02.
Example 6
The embodiment 6 provides a demulsification coalescing material for oil sludge in coal chemical industry wastewater, which specifically comprises the following steps:
step 1, weighing methacrylamidoalkyl ammonium chloride, butyl methacrylate and polytriethanolamine according to requirements, and adding the weighed materials into a three-neck flask under the condition of water bath to obtain a mixed system; wherein, in the mixed system, the mass percent of the methacrylamide alkyl ammonium chloride is 30 percent, the mass percent of the butyl methacrylate is 20 percent, and the mass percent of the polytriethanolamine is 50 percent.
Step 2, adding deionized water into the mixed system, stirring for dissolving, then adding ammonia water for adjusting the pH value to be neutral until the ammonia water is completely dissolved to obtain a mixed solution; wherein the mass fraction of the ammonia water is 25%.
Step 3, adding hydrogen peroxide into the mixed solution, and stirring at a constant speed to obtain a polymerization reaction system; wherein, hydrogen peroxide is used as an initiator; in a polymerization reaction system, the mass fraction of hydrogen peroxide is 4%; and (3) adjusting the temperature of the polymerization reaction system to 70 ℃, introducing nitrogen into the polymerization reaction system, uniformly mixing, and carrying out closed reaction for 2 hours to obtain a polymerization reaction product.
Step 4, adding polyethylene polyamine into the polymerization reaction product, and stirring at a constant speed to obtain a crosslinking polymerization reaction system; adjusting the temperature of the crosslinking polymerization reaction system to 90 ℃; introducing nitrogen into the crosslinking polymerization reaction system, uniformly mixing, carrying out closed reaction for 7 hours, and cooling to room temperature after the reaction is completed to obtain a crosslinking polymerization product; wherein, the polyethylene polyamine is used as an initiator, and the mass fraction of the polyethylene polyamine in a crosslinking polymerization reaction system is 3%.
Step 5, washing the crosslinked polymer product by adopting absolute ethyl alcohol and acetone, centrifugally separating, and purifying to obtain a purified product; and (3) carrying out freeze drying, crushing and screening on the purified product by using a freezing drying agent to obtain the demulsification material LY-01.
Step 6, dissolving gelatin in deionized water to obtain a gelatin solution; adding a ferromagnetic oxide powder material and citric acid into a gelatin solution to obtain a mixed system, and carrying out ultrasonic stirring on the mixed system to obtain a magnetic colloid; in the mixing system, the mass fraction of gelatin is 8%, the mass fraction of deionized water is 75%, the mass fraction of magnetic powder material is 12%, and the mass fraction of citric acid is 5%.
Step 7, adding the demulsifying material into the magnetic colloid in a constant-temperature water bath kettle at 40 ℃, and stirring and reacting at the speed of 400-700r/min for 24 hours to obtain a black solution; wherein the mass ratio of the demulsifying material to the magnetic colloid is 1: 25.
And 8, carrying out magnetic adsorption separation on the black solution to obtain a separation product, washing the separation product for multiple times by using ethanol-acetone, and carrying out cold drying and grinding to obtain black powder to obtain the aggregation material LY-02.
Test results
And (3) selecting coal chemical industry wastewater of a certain coal chemical industry plant to test the demulsification coalescence material for the oil sludge in the coal chemical industry wastewater, and removing the oil sludge substances in the wastewater to be treated.
The oil sludge treatment process specifically comprises the following steps:
s1, dissolving a demulsification material LY-01 in water to prepare a demulsification solution; dissolving an aggregation material LY-02 in water to prepare an aggregation solution; wherein the concentration of the demulsifying solution is 10g/L, and the concentration of the coalescence solution is 10 g/L.
S2, dropwise adding 50mL of the demulsifying solution into 1000mL of coal chemical wastewater to be treated; stirring and reacting for 5-10min at a stirring speed of 300-700 r/min until aggregates with smaller volume exist in the wastewater, so as to obtain the demulsified coal chemical wastewater;
s3, adding 5mL of the coalescence solution into the demulsified coal chemical industry wastewater in the step 2, stirring and reacting for 15-30min at a stirring speed of 100-400 r/min, standing and precipitating for 2h, separating and removing oil sludge, and taking supernatant to determine oil content and SS (suspended substance) of a water sample. The sludge removal effect is shown in table 1.
TABLE 1 sludge removal effectiveness of demulsifying coalescing materials made in examples 1-6
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Oil removal (%) | 45.8 | 46.3 | 48.8 | 47.8 | 44.4 | 48.3 |
| Removal Rate (%) of SS | 90.6 | 91.8 | 93.2 | 92.9 | 89.6 | 91.5 |
From the above table 1, it can be seen that the demulsification and coalescence material for oil sludge in coal chemical industry wastewater has high removal rate of the oil sludge and stable effect; the demulsification coalescence material for the oil sludge in the coal chemical industry wastewater can be applied to the process of removing the oil sludge in the coal chemical industry wastewater, particularly has a more remarkable oil sludge removing effect when the oil concentration is 1500-2000 mg/L and the particle size of the oil sludge is 0.1-200 mu m, and has important guiding significance for the sustainable and healthy development of the coal chemical industry;
according to the invention, the quaternary ammonium salt monomer, the oleophylic and hydrophobic monomer and the triethanolamine are adopted to form the high molecular compound, so that negative charges on the surfaces of colloid particles can be efficiently neutralized, the stability of colloid is damaged, the high molecular compound can be quickly adsorbed on an oil-water interface, an O/W emulsion is damaged, a surfactant and asphaltene molecules are replaced, and the interface tension and the interface film strength of oil water are reduced; the demulsification material LY-01 and the coalescence material LY-02 obtained by modifying the magnetic material have rich branched chain structures and specific functional groups, are macromolecular surfactants with excellent performance, and enable oil sludge particles dispersed in water to coalesce; the demulsification coalescence material has the functions of demulsification and coalescence, and has a strong promotion effect on the rapid separation of oil, water and mud phases; the demulsifying material LY-01 and the coalescing material LY-02 have a good effect on removing the oil sludge under the synergistic effect, and the efficient treatment of the oil sludge of the coal chemical industry wastewater is realized.
According to the invention, the surface of the demulsification coalescence material is provided with abundant positive charges and branched structures, the ions with the positive charges destabilize colloid particles with negative charges in the wastewater, and then small aggregates are coagulated into large aggregates by utilizing the specific performance of the coalescence material, so that the removal of oil sludge in the coal chemical industry wastewater is facilitated; meanwhile, the yield of the sludge is reduced, the sludge-water separation effect is enhanced, the water content of the oil sludge is reduced, and the overall effluent quality is improved.
The demulsification coalescence material can destroy insoluble solid particles, carries toxic and harmful substances such as heavy metals and aromatic substances in part of coal chemical industry wastewater while destabilizing coalescence, and is removed by separation of oil sludge; the raw materials are low in price, the whole production process is simple, the cost is low, the product is environment-friendly and pollution-free, can be recycled, and cannot generate secondary pollution.
The above-described embodiment is only one of the embodiments that can implement the technical solution of the present invention, and the scope of the present invention is not limited by the embodiment, but includes any variations, substitutions and other embodiments that can be easily conceived by those skilled in the art within the technical scope of the present invention disclosed.
Claims (10)
1. The demulsification coalescence material for the oil sludge in the coal chemical industry wastewater is characterized by comprising a demulsification material LY-01 and a coalescence material LY-02;
the demulsification material LY-01 is used for performing demulsification treatment on oil sludge substances in the coal chemical industry wastewater to be treated so as to enable the oil sludge substances to be aggregated to form aggregates with smaller volume; the demulsification material LY-01 is prepared from a quaternary ammonium salt cationic monomer, an oleophylic hydrophobic monomer and polyalcohol amine;
the coalescing material LY-02 for coalescing the smaller volume of aggregates to form a larger volume of coalesced bodies; wherein the coalescence material LY-02 is prepared from gelatin, a magnetic powder material, citric acid and a demulsification material LY-01.
2. The demulsification coalescence material for the oil sludge in the coal chemical industry wastewater as claimed in claim 1, wherein the demulsification material LY-01 is prepared by the following specific steps:
mixing quaternary ammonium salt cationic monomer, oleophilic hydrophobic monomer and polyalcohol amine to prepare a mixed solution;
adding an introducing agent into the mixed solution to carry out polymerization reaction to obtain a polymerization reaction product;
adding a cross-linking agent into the polymerization reaction product to carry out cross-linking polymerization reaction to obtain a cross-linked polymerization product;
and separating and purifying the crosslinked polymerization product to obtain the demulsification material LY-01.
3. The demulsification coalescing material for the oil sludge in the coal chemical industry wastewater as claimed in claim 2, wherein the quaternary ammonium salt cationic monomer is one of dimethyl diallyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride and methacrylaminoalkyl ammonium chloride; the oleophylic and hydrophobic monomer is one of lauryl methacrylate, isodecyl methacrylate and butyl methacrylate; the polyalcohol amine is polytriethanolamine.
4. The demulsification coalescence material for the oil sludge in the coal chemical industry wastewater as claimed in claim 2, is characterized in that the process of mixing the quaternary ammonium salt cationic monomer, the oleophylic hydrophobic monomer and the polyalcohol amine to prepare a mixed solution comprises the following specific steps:
mixing quaternary ammonium salt cationic monomer, oleophylic hydrophobic monomer and polyalcohol amine to obtain a mixed system; wherein, in the mixed system, the mass percent of quaternary ammonium salt cationic monomer is 30-50%, the mass percent of oleophylic and hydrophobic monomer is 20-30%, and the mass percent of polyalcohol amine is 40-60%;
under the condition of water bath, deionized water is added into the mixed system, stirred and dissolved, and then the pH is adjusted to be neutral until the deionized water is completely dissolved, so that a mixed solution is obtained.
5. The demulsification coalescing material for oil sludge in coal chemical industry wastewater according to claim 2, wherein an introducing agent is added into the mixed solution to perform a polymerization reaction, so as to obtain a polymerization reaction product, and the process comprises the following steps:
adding an initiator into the mixed solution, and stirring at a constant speed to obtain a polymerization reaction system; adjusting the temperature of a polymerization reaction system to 50-70 ℃, introducing nitrogen into the polymerization reaction system, uniformly mixing, and carrying out closed reaction for 1-2h to obtain a polymerization reaction product;
wherein, the initiator adopts one of ammonium persulfate, potassium persulfate and hydrogen peroxide; the mass percentage of the initiator in the polymerization reaction system is 1-5%.
6. The demulsification coalescence material for the oil sludge in the coal chemical industry wastewater as claimed in claim 2, wherein a cross-linking agent is added into a polymerization reaction product to perform a cross-linking polymerization reaction, so as to obtain a cross-linked polymerization product, and the process comprises the following steps:
adding a cross-linking agent into the polymerization reaction product, and stirring at a constant speed to obtain a cross-linking polymerization reaction system; adjusting the temperature of a crosslinking polymerization reaction system to 70-90 ℃, introducing nitrogen into the crosslinking polymerization reaction system, uniformly mixing, carrying out closed reaction for 4-7h, and cooling to room temperature after complete reaction to obtain a crosslinking polymerization product; wherein, the cross-linking agent is one of ethylenediamine, n-butylamine and polyethylene polyamine.
7. The demulsification coalescence material for the oil sludge in the coal chemical industry wastewater as claimed in claim 2, wherein the demulsification material LY-01 is obtained by separating and purifying the crosslinked polymerization product, and the process comprises the following steps:
washing, centrifugally separating and purifying the crosslinked polymer product to obtain a purified product; and (3) carrying out cold drying, crushing and screening on the purified product to obtain the demulsification material LY-01.
8. The demulsification coalescing material for the oil sludge in the coal chemical industry wastewater as claimed in claim 1, wherein the preparation process of the coalescing material LY-02 comprises the following specific steps:
dissolving gelatin in water to obtain a gelatin solution; adding a magnetic powder material and citric acid into the gelatin solution, and performing ultrasonic stirring to obtain a magnetic colloid;
adding the demulsifying material LY-01 into a magnetic colloid, and stirring to obtain a black solution;
and (3) carrying out magnetic adsorption separation on the black solution to obtain a separation product, washing the separation product, and carrying out cold dry grinding on the separation product into powder to obtain the agglomeration material LY-02.
9. The demulsification coalescing material for oil sludge in coal chemical industry wastewater according to claim 8, wherein gelatin is dissolved in water to obtain a gelatin solution; adding a magnetic powder material and citric acid into a gelatin solution, and performing ultrasonic stirring to obtain a magnetic colloid, wherein the mass fraction of the gelatin is 3% -7%, the mass fraction of the magnetic powder material is 5% -15%, and the mass fraction of the citric acid is 2% -5%; wherein the magnetic powder material is one of iron oxide magnetic powder, chromium dioxide magnetic powder and metal magnetic powder.
10. The demulsification coalescence material for the oil sludge in the coal chemical industry wastewater as claimed in claim 8, wherein the demulsification material LY-01 is added into the magnetic colloid and stirred to obtain a black solution, and the process comprises the following specific steps:
under the condition of constant-temperature water bath, adding the demulsifying material LY-01 into the magnetic colloid, and stirring to obtain a black solution; wherein the temperature of the constant-temperature water bath is 30-40 ℃; the mass ratio of the demulsifying material LY-01 to the magnetic colloid is 1 (10-30).
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