CN111559776A - Self-floating demulsification degreasing agent and application thereof - Google Patents
Self-floating demulsification degreasing agent and application thereof Download PDFInfo
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Abstract
The invention discloses a self-floating demulsification deoiling agent, which takes hollow silicon dioxide microspheres, 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride and demulsifier polyether polyol 5010 as main raw materials to prepare the demulsification deoiling adsorbent with self-floating characteristic, excellent demulsification performance, high adsorption capacity and easy oil-water separation. By structural design and chemical modification, the surface of the hollow silica microsphere is subjected to graft modification under conventional conditions to obtain a demulsification-based polyether polyol 5010 and a microsphere structure wrapped by cationic quaternary ammonium salt, so that the oil-in-water type emulsified wastewater can be subjected to high-efficiency demulsification and decontamination and oil-water separation is promoted. Experiments show that the microsphere demulsification adsorbent with the self-floating property can realize efficient demulsification, adsorption and separation on machining cleaning emulsified oily wastewater, and has excellent removal performance on turbidity and Chemical Oxygen Demand (COD) in the emulsified wastewater.
Description
Technical Field
The invention relates to the technical field of water treatment agent preparation, in particular to a novel demulsification and deoiling agent with self-floating property and application thereof.
Background
With the rapid development of the industry in China, a large amount of oily wastewater is generated in petrochemical industry, mechanical processing and the like, and the oily wastewater enters an external environment due to the reasons of relatively late development of an oily wastewater treatment technology, insufficient management and the like, so that the water body and the soil environment are polluted, and the health and normal production and living activities of people are seriously influenced. Therefore, the effective treatment of the oily wastewater is an urgent problem to be solved in the field of environmental protection at present. Wherein, the treatment of the oily emulsified wastewater is the key and difficult point of the oily wastewater treatment. The emulsified wastewater generally refers to the stable dispersion of long-chain alkyl (more than or equal to 12) organic phase oil substances in water in an oil-in-water or water-in-oil mode, wherein the oil-in-water type is the most common and the most serious pollution is caused. The emulsified oil in the emulsified wastewater has small granularity, the density is lower than that of a water body, the emulsified oil generally presents 0.1-3 mu m of superfine oil drops, and due to the existence of an amphiphilic surfactant with an emulsifying effect on an oil-water interface, the emulsified oil is stably dispersed in a water phase and is difficult to be demulsified and separated and removed.
In the machining industry, emulsions and the like are used to cool the work pieces, for which reason a pile of waste emulsions and waste water with grease, machine oil and the like is produced. The waste water mainly contains emulsion, grease, engine oil, surfactant and the like, but because the interface of liquid drops in the waste emulsion and the waste water is provided with a stable film, the oil and the water are not easy to separate. Therefore, the waste emulsion and the waste water need to be subjected to a series of treatments so as to be discharged into the nature, otherwise, the waste emulsion and the waste water are directly discharged into the water body in the nature to pollute the water body, so that the water body is lack of oxygen to influence the survival of fishes and other aquatic animals, and meanwhile, suspended matters in the waste water are easy to decompose under anaerobic conditions to generate odor, so that the water quality is deteriorated.
At present, partial research is carried out on the treatment of oily wastewater, and the main treatment technologies comprise a coagulation method, a flotation method, a membrane separation method, a biological method and the like. Among them, the coagulation method is widely used for the treatment of oily wastewater because of its strong adaptability and the ability to remove emulsified oil and dissolved oil. Inorganic coagulants are widely used as water treatment effects, but because the density of emulsified oil is lower than that of water, the density of flocs treated by the inorganic coagulants is lower, the sedimentation speed is slow, and the amount of sludge generated after coagulation treatment is large, so that the problem of secondary environmental pollution is caused. Organic flocculant represented by cationic polyacrylamide is generally applied to the treatment of the current oily wastewater, but the demulsification effect is poor, the removal efficiency of turbidity and COD is low, and the floating speed of flocs after demulsification is slow.
Therefore, how to provide an oil removing agent with high demulsification and pollutant removal efficiency and good separation effect is a problem to be solved by the technical personnel in the field. In addition, no related research report of the demulsifying and degreasing agent with self-floating property exists at present.
Disclosure of Invention
Aiming at the defects of low oil removal efficiency and poor separation effect of the existing treating agent for oily wastewater, the invention aims to provide a demulsifying and deoiling agent which has self-floating property and is easy for oil-water separation.
Further, the invention also provides application of the demulsification and oil removal agent.
The invention adopts the following technical scheme:
the self-floating demulsification degreaser is characterized by being prepared by the following method:
1) activating the silica microspheres: putting 1-1.5 g of hollow silica microspheres with the particle size of 10-20 microns into a NaOH solution with the concentration of 0.5-3 mol/L, heating in a water bath, stirring, taking out, cooling to room temperature, eluting with deionized water, and drying;
2) modified silica microspheres: mixing the activated hollow silica microspheres obtained in the step 1) with absolute ethyl alcohol, adding 97% by mass of 3- (2, 3-glycidoxy) propyl trimethoxy silane and 50% by mass of trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride solution under stirring, and stirring for 3-5 hours at 70-90 ℃ by adopting a condensation reflux method;
3) oleophylic and hydrophobic grafting: adding polyether polyol 5010 accounting for 90% of the mass fraction and 4-dimethylaminopyridine accounting for 97% of the mass fraction into the step 2), and continuously stirring for 3-5 hours at 70-90 ℃ by adopting a condensation reflux method so as to maximally graft a demulsifying group to the surface of the microsphere;
4) and (3) purification: and (3) purifying the graft polymer by adopting absolute ethyl alcohol and deionized water, and drying at the temperature of 70-90 ℃ for 3-5 hours to obtain the product.
Wherein the water bath heating temperature in the step 1) is 70-90 ℃, the activation time is 2-3 hours, and the drying temperature is 50-120 ℃.
Further, the mass ratio of the absolute ethyl alcohol, the 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and the trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride in the step 2) is 100: (0.3-1.0): (0.3-1.0); the above components are converted according to the purity of 100%.
Further, the adding amount of the polyether polyol 5010 and the 4-dimethylaminopyridine in the step 3) is 0.3-1.0ml and 0.3-1.0ml respectively, and the adding amounts are calculated according to the purity of 100%.
Further, the purity of the absolute ethyl alcohol in the step 4) is 99.5%, and the conductivity of the deionized water is less than or equal to 20 mu S/cm.
The invention also provides application of the self-floating demulsification deoiling agent, and the self-floating demulsification deoiling agent obtained by the method is used for treating the machining oil-containing emulsified wastewater.
The demulsifying and deoiling agent disclosed by the invention is used for treating machining emulsified wastewater, the adding amount is 40-45 mg/L, the stirring speed is 100-200 rpm, the stirring time is 3-5 min, the standing and floating time is 20-30 min, and a clear liquid 5-10 cm below the liquid level is taken for detection and analysis.
The hollow silicon dioxide material adopted in the invention is a hollow totally-enclosed structure material, has the advantages of low cost, stable structure and easy preparation, and is widely applied to industries such as decoration, paint and the like. Due to the hollow structure, the density of the micron-sized hollow silica is about 0.5g/mL, and the micron-sized hollow silica has strong self-floating property in a water body.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention takes hollow silicon dioxide microspheres, 3- (2, 3-epoxypropoxy) propyl trimethoxy silane, trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride and demulsifier polyether polyol 5010 as main raw materials to prepare a demulsification and oil removal adsorbent which has the advantages of self-floating property, excellent demulsification performance, high adsorption capacity and easiness in oil-water separation; through structural design and chemical modification, the surface of the hollow silica microsphere is subjected to graft modification under conventional conditions to obtain a demulsification-based polyether polyol 5010 and a microsphere structure wrapped by cationic quaternary ammonium salt, so that the oil-in-water emulsified wastewater can be subjected to high-efficiency demulsification and decontamination, and oil-water separation is promoted, and the purpose of high-efficiency decontamination is achieved. Moreover, the self-floating demulsification degreaser has wide applicable pH range and stable structure.
2. The invention creatively carries out oleophylic and hydrophobic modification on the surface of the hollow silica microsphere for improving the demulsification and adsorption performances of the hollow silica microsphere, and effectively demulsifies and decontaminates emulsified oily wastewater according to the characteristic that the hollow silica microsphere is lower than water, thereby realizing automatic floating and decontamination. Aiming at the density difference of an organic phase and water in the oil-in-water type oil-containing emulsified wastewater, the surface of the hollow silica microsphere with the self-floating property is functionally modified to obtain the demulsification and deoiling agent which automatically floats to realize oil-water separation. Compared with the common inorganic coagulant polyaluminium chloride (PAC) in the current demulsification and degreasing application, the self-floating demulsification and degreasing agent has the advantages of good demulsification effect, low sludge amount, no secondary pollution risk to the external environment and the like; compared with Cationic Polyacrylamide (CPAM) flocculant, the flocculant has the advantages of good self-floating demulsification effect, high adsorption capacity, obvious decontamination performance, easy oil stain separation due to automatic floating, and the like.
3. The self-floating demulsifying and deoiling agent has excellent treatment efficiency on oily emulsified wastewater such as machining cleaning wastewater and the like. Experiments show that the turbidity removal rate of the emulsified oily wastewater subjected to mechanical processing and cleaning reaches 79.1-85.3%, the COD removal rate is 59.5-63.9%, and the turbidity removal rate is far higher than that of an inorganic coagulant, namely polyaluminium chloride and cationic polyacrylamide.
4. The self-floating demulsifying and deoiling agent can be purified by gasoline, ethanol and deionized water in sequence under certain conditions, so that the reutilization is realized.
5. The preparation method has the advantages of low raw material cost, simple preparation process, mild reaction condition, easy control and the like.
Detailed Description
The present invention will be further described with reference to specific examples. It is worth to be noted that the mass percentages of the raw materials and the effective components in the invention are respectively as follows: 3- (2, 3-glycidoxy) propyltrimethoxysilane (97%), trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride (50%), polyether polyol 5010 (90%), 4-dimethylaminopyridine (97%), absolute ethanol (99.5%) purity.
Example 1:
a self-floating demulsification degreasing agent is obtained by adopting the following method:
1) putting 1g of hollow silica microspheres (with the particle size of 16 mu m) into 100mL of NaOH solution with the concentration of 2mol/L, heating in a water bath to 80 ℃, stirring for 2h, taking out, cooling to room temperature, eluting with deionized water, and drying at 70 ℃ for 3 h;
2) dispersing the activated hollow silica microspheres obtained in the step 1) in a triangular flask filled with 100mL of absolute ethyl alcohol, and building a reaction device with heating, stirring and condensing reflux functions.
3) Adding 1.0mL of 3- (2, 3-epoxypropoxy) propyl trimethoxy silane with the mass fraction of 97% into the Erlenmeyer flask in the step 2) under the stirring condition, and stirring for 4 hours at 80 ℃ to graft enough 3- (2, 3-epoxypropoxy) propyl trimethoxy silane on the surface of the silica microsphere;
4) taking out the 3- (2, 3-epoxypropoxy) propyl trimethoxy silane modified hollow silica microspheres, washing with deionized water for 3 times, and vacuum drying at 60 ℃ for 1 h;
5) dispersing the modified hollow silica obtained in the step 4) into a triangular flask filled with 100ml of absolute ethyl alcohol, adding 0.5ml of polyether polyol 5010 with the mass fraction of 90% and 0.5ml of 4-dimethylaminopyridine with the mass fraction of 97%, and continuously stirring for 3 hours in a condensation reflux method device at the temperature of 75 ℃;
6) the graft polymer is purified by absolute ethyl alcohol and deionized water, and is dried for 3 hours at the temperature of 80 ℃ to obtain the product.
The adsorption test result shows that when the demulsifying and deoiling agent is used for treating the emulsified wastewater (1) produced in machining of certain precision instrument factory of Yaan, the adding amount is 45mg/L, the stirring speed is 150rpm, the stirring time is 3min, the standing and floating time is 20min, and the clear liquid at the position 6cm below the liquid level is taken for detection and analysis. Through analysis, the turbidity removal rate reaches 79.1 percent, and the COD removal rate is 59.5 percent; the COD removal rate after the second cycle of use is 41.5%. In the treatment test of the emulsified wastewater (2) processed by machinery in certain precision instrument factory of Yaan, when the dosage is 40mg/L, the turbidity removal rate reaches 74.6%, the COD removal rate is 55.4%, and the COD removal rate after the second cycle use is 38.6%.
Example 2:
a self-floating demulsification degreasing agent is obtained by adopting the following method:
1) putting 1g of hollow silica microspheres (with the particle size of 16 mu m) into 100mL of NaOH solution with the concentration of 2mol/L, heating in a water bath to 80 ℃, stirring for 2h, taking out, cooling to room temperature, eluting with deionized water, and drying at 70 ℃ for 3 h;
2) dispersing the activated hollow silica microspheres obtained in the step 1) in a triangular flask filled with 100mL of absolute ethyl alcohol, and building a reaction device with heating, stirring and condensing reflux functions.
3) Adding 1.0mL of 97 mass percent 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and 2.0mL of 50 mass percent trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride solution into the Erlenmeyer flask in the step 2) under stirring, and stirring at 80 ℃ for 4 hours to graft sufficient 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and cationic quaternary ammonium salt trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride groups on the surface of the silica microspheres;
4) taking out the 3- (2, 3-epoxypropoxy) propyl trimethoxy silane modified hollow silica microspheres, washing with deionized water for 3 times, and vacuum drying at 60 ℃ for 1 h;
5) dispersing the modified hollow silica obtained in the step 4) into a triangular flask filled with 100ml of absolute ethyl alcohol, adding 0.5ml of polyether polyol 5010 with the mass fraction of 90% and 0.5ml of 4-dimethylaminopyridine with the mass fraction of 97%, and continuously stirring for 3 hours in a condensation reflux method device at the temperature of 75 ℃;
6) the graft polymer is purified by absolute ethyl alcohol and deionized water, and is dried for 3 hours at the temperature of 80 ℃ to obtain the product.
The adsorption test result shows that when the demulsifying and deoiling agent is used for treating emulsified wastewater (1) produced in machining of certain precision instrument factory of Yaan, the adding amount is 47mg/L, the stirring speed is 180rpm, the stirring time is 4min, the standing and floating time is 25min, and clear liquid 5cm below the liquid level is taken for detection and analysis. Through analysis, the turbidity removal rate reaches 82.9 percent, and the COD removal rate is 62.2 percent; the COD removal rate after the second cycle of use is 42.7%. In the treatment test of the emulsified wastewater (2) processed by machinery in certain precision instrument factory of Yaan, when the dosage is 45mg/L, the turbidity removal rate reaches 79.1%, the COD removal rate is 58.4%, and the COD removal rate after the second cycle of use is 39.5%.
Example 3:
a self-floating demulsification degreasing agent is obtained by adopting the following preparation method:
1) putting 1g of hollow silica microspheres (with the particle size of 16 mu m) into 100mL of NaOH solution with the concentration of 2mol/L, heating in a water bath to 80 ℃, stirring for 2h, taking out, cooling to room temperature, eluting with deionized water, and drying at 70 ℃ for 3 h;
2) dispersing the activated hollow silica microspheres obtained in the step 1) in a triangular flask filled with 100mL of absolute ethyl alcohol, and building a reaction device with heating, stirring and condensing reflux functions.
3) Adding 1.0mL of 97 mass percent 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and 2.0mL of 50 mass percent trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride solution into the Erlenmeyer flask in the step 2) under stirring, and stirring at 80 ℃ for 4 hours to graft sufficient 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and cationic quaternary ammonium salt trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride groups on the surface of the silica microspheres;
4) adding 0.5ml of polyether polyol 5010 with the mass fraction of 90% and 0.5ml of 4-dimethylamino pyridine with the mass fraction of 97% into the step 3), and continuously stirring for 4 hours at 80 ℃ by adopting a condensation reflux method to maximally graft a demulsifying group to the surface of the microsphere;
5) the graft polymer is purified by absolute ethyl alcohol and deionized water, and is dried for 3 hours at the temperature of 80 ℃ to obtain the product.
The adsorption test result shows that when the demulsifying and deoiling agent is used for treating emulsified wastewater (1) produced in machining of certain precision instrument factory in Yaan, the adding amount is 42mg/L, the stirring speed is 120rpm, the stirring time is 5min, the standing and floating time is 25min, and clear liquid 5-10 cm below the liquid level is taken for detection and analysis. The turbidity removal rate reaches 84.1 percent, and the COD removal rate is 63.3 percent; the COD removal rate after the second cycle of use is 43.8%. In the treatment test of the emulsified wastewater (2) processed by machinery in certain precision instrument factory of Yaan, when the dosage is 46mg/L, the turbidity removal rate reaches 85.2 percent, the COD removal rate is 61.4 percent, and the COD removal rate after the second cycle use is 40.9 percent.
Example 4:
example 4 was prepared in the same manner as example 3 except that the amounts of 3- (2, 3-glycidoxy) propyltrimethoxysilane and trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride added in step 4) were different.
Comparative example 1 adopts the treatment of common inorganic coagulant polyaluminium chloride (PAC), in the treatment test of the emulsified wastewater (1) of mechanical processing in a precision instrument factory of Yaan, the dosage is 70mg/L, the stirring speed is 160rpm, the stirring time is 5min, the standing floating time is 30min, the clear liquid 5cm below the liquid level is taken for detection and analysis, the turbidity removal rate reaches 84.5%, the COD removal rate is 47.5%, and the waste water can not be recycled for the second time. In the treatment test of the emulsified wastewater (2) in mechanical processing of certain precision instrument factory of Yaan, when the dosage is 65mg/L, the turbidity removal rate reaches 81.6 percent, the COD removal rate is 44.6 percent, and the emulsified wastewater cannot be recycled for the second time. In addition, the sludge yield after the inorganic coagulant treatment is high, and secondary pollution risk to the external environment is also caused.
Comparative example 2 adopts cationic polyacrylamide flocculant, and in the treatment test of the emulsified wastewater (1) from mechanical processing in a precision instrument factory of Yaan, when the dosage is 50mg/L, the stirring speed is 150rpm, the stirring time is 5min, the standing and floating time is 30min, and the clear liquid 5-10 cm below the liquid level is taken for detection and analysis. Through analysis, the turbidity removal rate reaches 50.6%, the COD removal rate is 28.1%, and the waste water can not be recycled. In the treatment test of the emulsified wastewater (2) in mechanical processing of certain precision instrument factory in Yaan, when the dosage is 52mg/L, the turbidity removal rate reaches 47.7 percent, the COD removal rate is 26.8 percent, and the emulsified wastewater cannot be recycled for the second time.
TABLE 1
The comparative experiment of the table 1 shows that the self-floating demulsification and oil removal agent has wide applicable pH range and stable structure; the price of the main raw materials is low, and the preparation process is simple. Compared with comparative examples 1 and 2, the method has remarkable advantages in turbidity removal rate, COD removal rate and reusability. The self-floating demulsifying and deoiling agent can realize high-efficiency demulsification, adsorption and separation on machining cleaning emulsified oily wastewater, and provides a better choice for high-efficiency treatment of oil-in-water emulsified wastewater.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (7)
1. The self-floating demulsification degreaser is characterized by being prepared by the following method:
1) activating the silica microspheres: putting 1-1.5 g of hollow silica microspheres with the particle size of 10-20 microns into a NaOH solution with the concentration of 0.5-3 mol/L, heating in a water bath, stirring, taking out, cooling to room temperature, eluting with deionized water, and drying;
2) modified silica microspheres: mixing the activated hollow silica microspheres obtained in the step 1) with absolute ethyl alcohol, adding 97% by mass of 3- (2, 3-glycidoxy) propyl trimethoxy silane and 50% by mass of trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride solution under stirring, and stirring for 3-5 hours at 70-90 ℃ by adopting a condensation reflux method;
3) oleophylic and hydrophobic grafting: adding polyether polyol 5010 accounting for 90% by mass and 4-dimethylaminopyridine accounting for 97% by mass into the step 2), and continuously stirring for 3-5 hours at 70-90 ℃ by adopting a condensation reflux method so as to maximally graft a demulsifying group to the surface of the microsphere;
4) and (3) purification: and (3) purifying the graft polymer by adopting absolute ethyl alcohol and deionized water, and drying at the temperature of 70-90 ℃ for 3-5 hours to obtain the product.
2. The self-floating demulsification deoiling agent as claimed in claim 1, wherein the water bath heating temperature in the step 1) is 70-90 ℃, the activation time is 2-3 hours, and the drying temperature is 50-120 ℃.
3. The self-floating demulsifying and degreasing agent as claimed in claim 1, wherein the mass ratio of the absolute ethyl alcohol, the 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and the trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride in the step 2) is 100: (0.3-1.0): (0.3-1.0); the above components are converted according to the purity of 100%.
4. The self-floating demulsifying and degreasing agent as claimed in claim 1, wherein the addition amount of the polyether polyol 5010 and the 4-dimethylaminopyridine in the step 3) is 0.3-1.0ml and 0.3-1.0ml respectively, and the addition amounts are calculated according to the purity of 100%.
5. The self-floating demulsifying and degreasing agent as claimed in claim 1, wherein the purity of the absolute ethyl alcohol in the step 4) is 99.5%, and the conductivity of the deionized water is less than or equal to 20 μ S/cm.
6. The use of the self-floating demulsifying and deoiling agent is characterized in that the self-floating demulsifying and deoiling agent as claimed in claims 1-5 is used for treating oily emulsified wastewater of mechanical processing.
7. The application of the self-floating demulsification and oil removal agent as claimed in claim 6, wherein the demulsification and oil removal agent is used for treating machining emulsified wastewater, the adding amount is 40-45 mg/L, the stirring speed is 100-200 rpm, the stirring time is 3-5 min, the standing and floating time is 20-30 min, and the clear liquid 5-10 cm below the liquid surface is taken for detection and analysis.
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| CN112915592A (en) * | 2021-02-09 | 2021-06-08 | 天津大学 | Magnetic nano material and preparation method and application thereof |
| CN112960875A (en) * | 2021-02-25 | 2021-06-15 | 广西博世科环保科技股份有限公司 | Treatment method and treatment system for high-temperature thermochemical cleaning of heavy oil sludge |
| CN115028288A (en) * | 2022-06-30 | 2022-09-09 | 四川农业大学 | Self-separation hydrophilic and hydrophobic regulating and controlling flocculant and application thereof |
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