CN102963959B - Preparation method of microsphere particles capable of slowly releasing nitrogen and adsorbing-biologically degrading petroleum hydrocarbon - Google Patents
Preparation method of microsphere particles capable of slowly releasing nitrogen and adsorbing-biologically degrading petroleum hydrocarbon Download PDFInfo
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- CN102963959B CN102963959B CN2012105048277A CN201210504827A CN102963959B CN 102963959 B CN102963959 B CN 102963959B CN 2012105048277 A CN2012105048277 A CN 2012105048277A CN 201210504827 A CN201210504827 A CN 201210504827A CN 102963959 B CN102963959 B CN 102963959B
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Abstract
The invention discloses a preparation method of microsphere particles capable of slowly releasing nitrogen and adsorbing-biologically degrading petroleum hydrocarbon. The method comprises the following steps of: weighing a urea aqueous solution and a formaldehyde aqueous solution at a ratio of 6.5:1, and adjusting the pH value of the urea aqueous solution to 7.2-7.4; adding formaldehyde into the urea aqueous solution, stirring for 90-100 minutes, adjusting the pH value to 3.2-3.4, and adding deionized water to obtain mixed liquid M1; mixing the chloroform solutions of poly(beta)hydroxybutyrate and polyethylene glycol at a ratio of 5:1; dropwise adding M1 into the chloroform mixed liquid at a ratio of 1:4; dropwise adding the mixed liquid into a polyvinyl alcohol solution with mass fraction of 3.5% at a ratio of 1:1; dropwise adding a polyvinyl alcohol solution with mass fraction of 0.5% into the mixed liquid at a ratio of 2:1, stirring for 7-8 hours, separating, and freeze-drying to obtain microsphere particles; and culturing the microsphere particles in a petroleum hydrocarbon degrading bacterium culture solution for 24 hours, taking out and air-drying. Through the invention, the preparation technology is simple, the efficiency of the prepared microsphere particles for treating petroleum hydrocarbon pollutants is high, and secondary pollution and damage to the water body are avoided.
Description
Technical field
The invention belongs to the processing technology field that is subjected to the oil spill water body, particularly a kind of can slow-release nitrogen and the microsphere particle preparation method of Adsorption-Biodegradation petroleum hydrocarbon.
Background technology
In recent years, the demand that oil and goods thereof is day by day increased along with countries in the world, at sea exploit, load and unload, transport and utilize oil spill accident in the oil process to happen occasionally, not only cause a large amount of crude oil to run off, also environment is caused severe contamination, threatening the ecological environment of water body and land-based area with being on the rise, water body environment, natural resources and culture resources etc. are had long-term harm, therefore, the water body oil spill has become the great environmental problem that people must face.
The method of disposing at present the water body oil spill both at home and abroad mainly contains Physical, chemical method and bioanalysis.Chemical method is the technology path of comparative maturity in point-source pollution is administered, obtained propagation and employment widely.But adopt chemical method in the water body oil spill is administered, need to add chemical agent in water body, the chemical agent that wherein adds may produce secondary pollution on the one hand, can produce short-term or long-term impact to water ecological setting on the other hand.The characteristics such as bioremediation technology has efficiently, economy, safety, non-secondary pollution, become the on-the-spot important selection approach of removing the water body oil spill, the oil sheet that particularly to mechanical device, can't remove, when chemical agent is used in restriction again simultaneously, use biological restoration can show its larger superiority.Physisorphtion is that a kind for the treatment of effeciency is high, cost is low, without sediment pollution, simple to operate and can not cause to water ecological setting the method for secondary pollution and destruction, can solve preferably the existing problem of chemical method.But, the cycle of bioremediation technology is long, physisorphtion faces absorption needs the problem that adsorbent is remarketed after saturated, if can prepare a kind of biodegradable adsorbent, simultaneously on adsorbent fixedly petroleum hydrocarbon degradation bacterium to improve the clearance of petroleum hydrocarbon, effect by microbe inoculation after absorption is saturated is adsorbent petroleum hydrocarbon degradation, and final biodegradable adsorbent itself also can thoroughly degrade, and can address this problem.Physisorphtion and fixation of microbe are carried out enhancing degradation combine, be used for disposing the water body oil spill and will have larger advantage.
In the process of microbial degradation petroleum hydrocarbon and adsorbent itself, need the participation of nitrogen nutrition element, the needs that generally in the oil spill water body, contained nitrogen element can't meet microorganism are asked, yet the adsorbent with slow-release nitrogen function can meet this requirement.In processing, the water body oil spill obtains further propagation and employment for physisorphtion and fixation of microbe being carried out the technology that enhancing degradation combines, need to develop the material that has simultaneously slow-release nitrogen element and physical absorption-biodegradation petroleum hydrocarbon function, this has great importance, but also lacks the technology of this aspect at present and study and report for raising water body oil spill treatment effeciency, reduction environmental pollution.
Summary of the invention
Purpose of the present invention provide a kind of can slow-release nitrogen and the microsphere particle preparation method of Adsorption-Biodegradation petroleum hydrocarbon.Its concrete steps are as follows:
(1) the preparation mass fraction is 50% aqueous solution of urea, and the preparation mass fraction is 30% formalin; Volume ratio in aqueous solution of urea and formalin is the ratio of 6.5:1, and aqueous solution of urea is moved in the A container, and formalin is moved in the B container;
(2) formalin in aqueous solution of urea and B container in step (1) A container was placed in 45 ℃ of water-bath constant temperature 30～40 minutes;
(3) dripping molar concentration in the aqueous solution of urea that obtains to step (2) under the 1000r/min stirring condition is the NaOH solution of 0.01mol/L and the HCl solution that molar concentration is 0.005mol/L, and the pH value that makes solution is 7.2～7.4;
(4) formalin that step (2) is obtained joins in the aqueous solution of urea that step (3) obtains under the 1000r/min stirring condition, then be placed in 45 ℃ of water-baths and stirred under the 1000r/min condition 90～100 minutes;
(5) dripping molar concentration in the mixed solution that obtains to step (4) under the 1000r/min stirring condition is the NaOH solution of 0.01mol/L and the HCl solution that molar concentration is 0.005mol/L, and the pH value that makes solution is 3.2～3.4;
(6) mixed solution that step (5) is obtained is placed in 35 ℃ of water-baths and stirred under the 1000r/min condition 90～100 minutes;
(7), by volume for the ratio of 25:1 is added drop-wise to deionized water in the mixed solution that step (6) obtains under the 1000r/min stirring condition, then stir 4min under the 1000r/min condition, obtain mixed liquor M1;
(8) the preparation mass fraction is 7.5% poly beta-hydroxybutyrate chloroformic solution; The preparation mass fraction is 7.5% polyethylene glycol chloroformic solution; The ratio that is 5:1 in the volume ratio of poly beta-hydroxybutyrate chloroformic solution and polyethylene glycol chloroformic solution will both fully be mixed to get mixed solution;
(9) the mixed liquor M1 that for the ratio of 1:4, step (7) is obtained by volume is added drop-wise in the mixed solution that step (8) obtains under the 1000r/min stirring condition, then stir 4min under the 1000r/min condition;
(10) mixed liquor that for the ratio of 1:1, step (9) is obtained by volume is added drop-wise to mass fraction under the 1000r/min stirring condition be 3.5% poly-vinyl alcohol solution, then stirs 4min under the 1000r/min condition;
(11) poly-vinyl alcohol solution that is 0.5% for the ratio of 2:1 with mass fraction by volume joins in the mixed liquor that step (10) obtains, stir 7～8h under the 1000r/min condition, solvent is fully volatilized and cause polymerisation, be to carry out centrifugation under the 6000r/min condition at rotating speed, then with deionized water washing 3 times, freeze drying must have the microsphere particle of slow-release nitrogen function.
(12) microsphere particle with slow-release nitrogen function that step (11) is obtained is cultivated 24h in the petroleum hydrocarbon degradation bacteria culture fluid, petroleum hydrocarbon degradation bacterium is absorbed and fixed on microsphere particle, and wherein the bacteria containing amount of petroleum hydrocarbon degradation bacteria culture fluid is 5 * 10
10CFU/ml, the consisting of of nutrient solution: NH
4NO
3: 2.0gL
-1, NaC1:10.5g/L, KH
2PO
4: 2.5gL
-1, FeCl
3: 0.10gL
-1, MgSO
4: 3.5gL
-1, CaCl
22H
2O:0.15gL
-1
(13) microsphere particle in step (12) is taken out air-dry, can obtain can slow-release nitrogen and the microsphere particle of Adsorption-Biodegradation petroleum hydrocarbon.
The invention has the beneficial effects as follows, manufacture craft is simple, make can slow-release nitrogen and the microsphere particle of Adsorption-Biodegradation petroleum hydrocarbon high to the petroleum hydrocarbon contaminant treatment effeciency, and can not cause secondary pollution and destruction to water ecological setting.
The specific embodiment
The invention provides a kind of can slow-release nitrogen and the microsphere particle preparation method of Adsorption-Biodegradation petroleum hydrocarbon, below with two embodiment, the present invention is described.
Embodiment 1.
The aqueous solution of urea that is 50% with the 65mL mass fraction is moved in the A container, and the 10mL mass fraction is that 30% formalin is moved in the B container, then is placed on respectively in 45 ℃ of water-baths constant temperature 30 minutes; The dropping molar concentration is that the pH value of the NaOH solution of 0.01mol/L and the HCl solution adjusting aqueous solution of urea that molar concentration is 0.005mol/L is 7.2; Formalin in the B container is joined in above-mentioned aqueous solution of urea under the 1000r/min stirring condition, then be placed in 45 ℃ of water-baths and stirred 90 minutes under the 1000r/min condition; Be that the pH value that the NaOH solution of 0.01mol/L and HCl solution that molar concentration is 0.005mol/L are regulated mixed solution is 3.2 to dripping molar concentration in mixed liquor; Then being placed in 35 ℃ of water-baths stirred 90 minutes under the 1000r/min condition; The 1875mL deionized water is added drop-wise in above-mentioned 75mL mixed solution under the 1000r/min stirring condition and obtains 1950mL mixed liquor M1.
Mass fraction is 7.5% 200mL poly beta-hydroxybutyrate chloroformic solution and 40mL polyethylene glycol chloroformic solution and fully is mixed to get the 240mL mixed solution; 60mL mixed liquor M1 is added drop-wise in above-mentioned 240mL mixed solution and obtains the 300mL mixed solution under stirring condition, then stir 4min under the 1000r/min condition; It is to obtain the 600mL mixed solution in 3.5% poly-vinyl alcohol solution that the 300mL mixed liquor that obtains is added drop-wise to the 300mL mass fraction, then stirs 4min under the 1000r/min condition; The poly-vinyl alcohol solution that is 0.5% with the 1200mL mass fraction is added drop-wise in the mixed liquor of above-mentioned 600mL, stir 7h under the 1000r/min condition, solvent is fully volatilized and cause polymerisation, then be to carry out centrifugation under the 6000r/min condition at rotating speed, with deionized water washing 3 times, freeze drying must have the microsphere particle of slow-release nitrogen function.
Be 5 * 10 with the microsphere particle that obtains at bacteria containing amount
10Cultivate in the petroleum hydrocarbon degradation bacteria culture fluid of CFU/mL after 24h and take out air-dryly, can obtain can slow-release nitrogen and the microsphere particle of Adsorption-Biodegradation petroleum hydrocarbon.
Be below use that the inventive method makes can slow-release nitrogen and the microsphere particle of Adsorption-Biodegradation petroleum hydrocarbon the petroleum hydrocarbon in the oil spill water body has been carried out absorption and enhanced biodegradation test, further illustrate the present invention.
use that the inventive method makes can slow-release nitrogen and the microsphere particle of Adsorption-Biodegradation petroleum hydrocarbon the petroleum hydrocarbon in the oil spill water body has been carried out absorption and enhanced biodegradation test, result shows that this microsphere particle can effectively adsorb and enhanced biodegradation the petroleum hydrocarbon in water body: when the initial concentration of polluted-water Petroleum Hydrocarbon is 118.9mg/L, add the 10g microsphere particle in the water body of 1000mL, after 12 hours, the concentration of energy water body Petroleum Hydrocarbon is reduced to 0.01mg/L, after 14 days, microsphere particle Petroleum Hydrocarbon concentration does not detect, after 185 days, the quality of microsphere particle reduces by 51%.
Embodiment 2.
The aqueous solution of urea that is 50% with the 65mL mass fraction is moved in the A container, and the 10mL mass fraction is that 30% formalin is moved in the B container, then is placed on respectively in 45 ℃ of water-baths constant temperature 30 minutes; The dropping molar concentration is that the pH value of the NaOH solution of 0.01mol/L and the HCl solution adjusting aqueous solution of urea that molar concentration is 0.005mol/L is 7.4; Formalin in the B container is joined in above-mentioned aqueous solution of urea under the 1000r/min stirring condition, then be placed in 45 ℃ of water-baths and stirred 90 minutes under the 1000r/min condition; Be that the pH value that the NaOH solution of 0.01mol/L and HCl solution that molar concentration is 0.005mol/L are regulated mixed solution is 3.4 to dripping molar concentration in mixed liquor; Then being placed in 35 ℃ of water-baths stirred 90 minutes under the 1000r/min condition; The 1875mL deionized water is added drop-wise in above-mentioned 75mL mixed solution under the 1000r/min stirring condition and obtains 1950mL mixed liquor M1.
Mass fraction is 7.5% 200mL poly beta-hydroxybutyrate chloroformic solution and 40mL polyethylene glycol chloroformic solution and fully is mixed to get the 240mL mixed solution; 60mL mixed liquor M1 is added drop-wise in above-mentioned 240mL mixed solution and obtains the 300mL mixed solution under stirring condition, then stir 4min under the 1000r/min condition; It is to obtain the 600mL mixed solution in 3.5% poly-vinyl alcohol solution that the 300mL mixed liquor that obtains is added drop-wise to the 300mL mass fraction, then stirring the poly-vinyl alcohol solution that 4mini is 0.5% with the 1200mL mass fraction under the 1000r/min condition is added drop-wise in the mixed liquor of above-mentioned 600mL, stir 7h under the 1000r/min condition, solvent is fully volatilized and cause polymerisation, then be to carry out centrifugation under the 6000r/min condition at rotating speed, with deionized water washing 3 times, freeze drying must have the microsphere particle of slow-release nitrogen function.
Be 5 * 10 with the microsphere particle that obtains at bacteria containing amount
10Cultivate in the petroleum hydrocarbon degradation bacteria culture fluid of CFU/mL after 24h and take out air-dryly, can obtain can slow-release nitrogen and the microsphere particle of Adsorption-Biodegradation petroleum hydrocarbon.
Be below use that the inventive method makes can slow-release nitrogen and the microsphere particle of Adsorption-Biodegradation petroleum hydrocarbon the petroleum hydrocarbon in the oil spill water body has been carried out absorption and enhanced biodegradation test, further illustrate the present invention.
use that the inventive method makes can slow-release nitrogen and the microsphere particle of Adsorption-Biodegradation petroleum hydrocarbon the petroleum hydrocarbon in the oil spill water body has been carried out absorption and enhanced biodegradation test, result shows that this microsphere particle can effectively adsorb and enhanced biodegradation the petroleum hydrocarbon in water body: when the initial concentration of polluted-water Petroleum Hydrocarbon is 118.9mg/L, add the 10g microsphere particle in the water body of 1000mL, after 12 hours, the concentration of energy water body Petroleum Hydrocarbon is reduced to 0.01mg/L, after 14 days, microsphere particle Petroleum Hydrocarbon concentration does not detect, after 185 days, the quality of microsphere particle reduces by 59%.
Claims (1)
- One kind can slow-release nitrogen and the microsphere particle preparation method of Adsorption-Biodegradation petroleum hydrocarbon, it is characterized in that, the concrete steps of the method are as follows:(1) the preparation mass fraction is 50% aqueous solution of urea, and the preparation mass fraction is 30% formalin; Volume ratio in aqueous solution of urea and formalin is the ratio of 6.5:1, and aqueous solution of urea is moved in the A container, and formalin is moved in the B container;(2) formalin in aqueous solution of urea and B container in step (1) A container was placed in 45 ℃ of water-bath constant temperature 30～40 minutes;(3) dripping molar concentration in the aqueous solution of urea that obtains to step (2) under the 1000r/min stirring condition is the NaOH solution of 0.01mol/L and the HC1 solution that molar concentration is 0.005mol/L, and the pH value that makes solution is 7.2～7.4;(4) formalin that step (2) is obtained joins in the aqueous solution of urea that step (3) obtains under the 1000r/min stirring condition, then be placed in 45 ℃ of water-baths and stirred under the 1000r/min condition 90～100 minutes;(5) dripping molar concentration in the mixed solution that obtains to step (4) under the 1000r/min stirring condition is the NaOH solution of 0.01mol/L and the HCl solution that molar concentration is 0.005mol/L, and the pH value that makes solution is 3.2～3.4;(6) mixed solution that step (5) is obtained is placed in 35 ℃ of water-baths and stirred under the 1000r/min condition 90～100 minutes;(7), by volume for the ratio of 25:1 is added drop-wise to deionized water in the mixed solution that step (6) obtains under the 1000r/min stirring condition, then stir 4min under the 1000r/min condition, obtain mixed liquor M1;(8) the preparation mass fraction is 7.5% poly beta-hydroxybutyrate chloroformic solution; The preparation mass fraction is 7.5% polyethylene glycol chloroformic solution; The ratio that is 5:1 in the volume ratio of poly beta-hydroxybutyrate chloroformic solution and polyethylene glycol chloroformic solution will both fully be mixed to get mixed solution;(9) the mixed liquor M1 that for the ratio of 1:4, step (7) is obtained by volume is added drop-wise in the mixed solution that step (8) obtains under the 1000r/min stirring condition, then stir 4min under the 1000r/min condition;(10) mixed liquor that for the ratio of 1:1, step (9) is obtained by volume is added drop-wise to mass fraction under the 1000r/min stirring condition be 3.5% poly-vinyl alcohol solution, then stirs 4min under the 1000r/min condition;(11) poly-vinyl alcohol solution that is 0.5% for the ratio of 2:1 with mass fraction by volume joins in the mixed liquor that step (10) obtains, stir 7～8h under the 1000r/min condition, solvent is fully volatilized and cause polymerisation, be to carry out centrifugation under the 6000r/min condition at rotating speed, then with deionized water washing 3 times, freeze drying must have the microsphere particle of slow-release nitrogen function.(12) microsphere particle with slow-release nitrogen function that step (11) is obtained is cultivated 24h in the petroleum hydrocarbon degradation bacteria culture fluid, petroleum hydrocarbon degradation bacterium is absorbed and fixed on microsphere particle, and wherein the bacteria containing amount of petroleum hydrocarbon degradation bacteria culture fluid is 5 * 10 10CFU/ml, the consisting of of nutrient solution: NH 4NO 3: 2.0gL -1, NaC1:10.5g/L, KH 2PO 4: 2.5gL -1, FeCl 3: 0.10gL -1, MgSO 4: 3.5gL -1, CaCl 22H 2O:0.15gL -1(13) microsphere particle in step (12) is taken out air-dry, can obtain can slow-release nitrogen and the microsphere particle of Adsorption-Biodegradation petroleum hydrocarbon.
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