CN103611506B - May float on biodegradable multifunctional ceiling elaioleucite and the preparation method of the water surface - Google Patents

May float on biodegradable multifunctional ceiling elaioleucite and the preparation method of the water surface Download PDF

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CN103611506B
CN103611506B CN201310684720.XA CN201310684720A CN103611506B CN 103611506 B CN103611506 B CN 103611506B CN 201310684720 A CN201310684720 A CN 201310684720A CN 103611506 B CN103611506 B CN 103611506B
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mixed liquor
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CN103611506A (en
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豆俊峰
袁静
丁爱中
程莉蓉
云影
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Beijing Normal University
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Beijing Normal University
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Abstract

The invention discloses the biodegradable multifunctional ceiling elaioleucite and preparation method that may float on the water surface.By NH 4hCO 3solution, NH 4h 2pO 4solution, Ca (NO 3) 2solution, NH 4oH solution, hydrochloric acid solution, NH 4the Cl aqueous solution and Ca-EDTA potassium solution are prepared into mixed liquor F.Urea and formalin are prepared into mixed liquor L; Poly beta-hydroxybutyrate chloroformic solution and polyethylene glycol chloroformic solution are prepared into mixed liquor M.Mixed liquor L is added drop-wise in mixed liquor M and obtains mixed liquor N; Mixed liquor F is added drop-wise in mixed liquor N, obtains mixed liquor O; Mixed liquor O is added drop-wise in poly-vinyl alcohol solution and obtains mixed liquor P; Poly-vinyl alcohol solution is joined then centrifugation in mixed liquor P, freeze drying obtains the biodegradable multifunctional ceiling elaioleucite that may float on the water surface.Manufacture craft of the present invention is simple, and obtained oil suction particle has slow-release nitrogen phosphorus function, adsorbs the function of petroleum hydrocarbon and have biodegradable.

Description

May float on biodegradable multifunctional ceiling elaioleucite and the preparation method of the water surface
Technical field
The invention belongs to the processing technology field by oil spill water body, particularly a kind of biodegradable multifunctional ceiling elaioleucite and preparation method that may float on the water surface.
Background technology
In recent years, along with the demand that countries in the world day by day increase oil and goods thereof, exploit, load and unload, transport and utilize oil spill accident in oil process to happen occasionally at sea, a large amount of crude oil is not only caused to run off, also severe contamination is caused to environment, threaten the ecological environment of water body and land-based area with being on the rise, have long-term harm to water body environment, natural resources and culture resources etc., therefore, water body oil spill become people must faced by great environmental problem.
The method disposing water body oil spill at present 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, and has obtained propagation and employment widely.But adopt chemical method in water body oil spill is administered, need to add chemical agent in water body, the chemical agent wherein added may produce secondary pollution on the one hand, can produce short-term or long-term impact on the other hand on water ecological setting.The features such as bioremediation technology has efficiently, economy, safety, non-secondary pollution, become the on-the-spot important selection approach removing water body oil spill, particularly to the oil sheet that mechanical device cannot be removed, when simultaneously restriction uses chemical agent again, use and biological prostheticly 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 the method for secondary pollution and destruction to water ecological setting, can solve the problem existing for chemical method preferably.But, the cycle of bioremediation technology is long, physisorphtion faces the saturated rear problem needing to remarket adsorbent of absorption, if a kind of biodegradable adsorbent can be prepared, fix petroleum hydrocarbon degradation bacterium on the sorbent to improve the clearance of petroleum hydrocarbon simultaneously, after absorption is saturated, pass through the effect of microbe inoculation by adsorbent petroleum hydrocarbon degradation, and final biodegradable adsorbent itself also thoroughly can be degraded, then can address this problem.Physisorphtion and fixation of microbe being carried out enhancing degradation combine, larger advantage will be had for disposing water body oil spill.
In the process of microbial degradation petroleum hydrocarbon and adsorbent itself, need the participation of nitrogen and phosphorus nutrition element, the nutrients such as nitrogen contained in oil spill water body under normal circumstances and phosphorus cannot meet the needs of microorganism, but the adsorbent with slow-release nitrogen and phosphorus function can meet this requirement.The technology combined to physisorphtion and fixation of microbe be carried out enhancing degradation obtains further propagation and employment in the process of water body oil spill, need to develop the material simultaneously with slow-release nitrogen and P elements and physical absorption-biodegradation of petroleum hydrocarbon function, this has great importance for raising water body oil spill treatment effeciency, reduction environmental pollution, but the technology also lacking this aspect is at present reported with research.
Summary of the invention
The object of this invention is to provide a kind of biodegradable multifunctional ceiling elaioleucite and the preparation method that may float on the water surface, this oil suction particle has the slow-release function of nitrogen and phosphorus.Its concrete steps are as follows:
(1) be the NH of 0.35mol/L by 100mL concentration 4hCO 3solution and 100mL concentration are the NH of 0.62mol/L 4h 2pO 4mixing, obtain mixed liquor A 1, is then the NH of 0.01mol/L by concentration 4oH solution and concentration are that the hydrochloric acid solution of 0.01mol/L regulates the pH value of mixed liquor A 1 to be 9.0, obtain mixed liquor A;
(2) 200mL mixed liquor A is slowly added drop-wise under agitation the Ca (NO that 300mL concentration is 0.025mol/L 3) 2in solution, obtain mixed liquid B;
(3) in mixed liquid B, dense HNO is dropwise added 3to clarification, obtain mixed liquor C;
(4) regulate the pH value of mixed liquor C to be 3.5 with the salpeter solution of concentration to be the NaOH solution of 0.01mol/L and concentration be 0.01mol/L, obtain mixed liquor D;
(5) in mixed liquor D, add the aqueous solution of urea that 100mL concentration is 1.2mol/L, after mixing, obtain mixed liquor E;
(6) in mixed liquor E, add the calcio-disodium edetate solution that 50mL concentration is 0.15mol/L, after mixing, obtain mixed liquor F;
(7) by 60mL mass fraction be 45% aqueous solution of urea be placed in 43 DEG C of water-bath constant temperature and obtain mixed liquor G in 35 minutes; By 10mL mass fraction be 35% formalin be placed in 43 DEG C of water-bath constant temperature and obtain mixed liquor H in 35 minutes;
(8) in mixed liquor G, drip the HCl solution that the NaOH solution that concentration is 0.01mol/L and concentration are 0.005mol/L under 1000r/min stirring condition, the pH value making solution is 7.2 ~ 7.4, obtains mixed liquor I;
(9) mixed liquor H is joined in mixed liquor I under 1000r/min stirring condition, be then placed in 43 DEG C of water-baths and stir 90 ~ 100 minutes under 1000r/min condition, obtain mixed liquor J;
(10) in mixed liquor J, under 1000r/min stirring condition, drip the HCl solution that the NaOH solution that concentration is 0.01mol/L and concentration are 0.005mol/L, the pH value of solution is made to be 3.7 ~ 3.9, then be placed in 38 DEG C of water-baths to stir 90 ~ 100 minutes under 1000r/min condition, obtain mixed liquor K;
(11) 1600mL deionized water is added drop-wise in mixed liquor K under 1000r/min stirring condition, then under 1000r/min condition, stirs 8min, obtain mixed liquor L;
(12) by 240mL mass fraction be 8.5% poly beta-hydroxybutyrate chloroformic solution and 60mL mass fraction be 6.5% polyethylene glycol chloroformic solution fully mix, obtain mixed liquor M;
(13) 60mL mixed liquor L is added drop-wise in mixed liquor M under 1000r/min stirring condition, then under 1000r/min condition, stirs 8min, obtain mixed liquor N;
(14) 60mL mixed liquor F is added drop-wise in mixed liquor N under 1000r/min stirring condition, then under 1000r/min condition, stirs 8min, obtain mixed liquor O;
(15) 420mL mixed liquor O being added drop-wise to 210mL mass fraction under 1000r/min stirring condition is in the poly-vinyl alcohol solution of 5.5%, then under 1000r/min condition, stirs 8min, obtains mixed liquor P;
(16) by 1380mL mass fraction be 0.7% poly-vinyl alcohol solution join in mixed liquor P, 7 ~ 8h is stirred under 1000r/min condition, then under rotating speed is 6000r/min condition, centrifugation is carried out, then spend deionized water 3 times, freeze drying can obtain the biodegradable multifunctional ceiling elaioleucite that may float on the water surface.
The invention has the beneficial effects as follows, obtained oil suction particle has the function of slow-release nitrogen phosphorus function, absorption petroleum hydrocarbon, may float on the water surface simultaneously and has biodegradable, being applied to oil pollution scene and can not causing secondary pollution and destruction to water ecological setting.
Detailed description of the invention
The invention provides a kind of biodegradable multifunctional ceiling elaioleucite and the preparation method that may float on the water surface, with an embodiment, the present invention is described below.
Embodiment
Be the NH of 0.35mol/L by 100mL concentration 4hCO 3solution and 100mL concentration are the NH of 0.62mol/L 4h 2pO 4mixing, obtain mixed liquor A 1, is then the NH of 0.01mol/L by concentration 4oH solution and concentration are that the hydrochloric acid solution of 0.01mol/L regulates the pH value of mixed liquor A 1 to be 9.0, obtain mixed liquor A; 200mL mixed liquor A is slowly added drop-wise under agitation the Ca (NO that 300mL concentration is 0.025mol/L 3) 2in solution, obtain mixed liquid B; Dense HNO is dropwise added in mixed liquid B 3to clarification, obtain mixed liquor C; Regulate the pH value of mixed liquor C to be 3.5 with the salpeter solution of concentration to be the NaOH solution of 0.01mol/L and concentration be 0.01mol/L, obtain mixed liquor D; In mixed liquor D, add the aqueous solution of urea that 100mL concentration is 1.2mol/L, after mixing, obtain mixed liquor E; In mixed liquor E, add the calcio-disodium edetate solution that 50mL concentration is 0.15mol/L, after mixing, obtain mixed liquor F.
By 60mL mass fraction be 45% aqueous solution of urea be placed in 43 DEG C of water-bath constant temperature and obtain mixed liquor G in 35 minutes; By 10mL mass fraction be 35% formalin be placed in 43 DEG C of water-bath constant temperature and obtain mixed liquor H in 35 minutes; In mixed liquor G, drip the HCl solution that the NaOH solution that concentration is 0.01mol/L and concentration are 0.005moI/L under 1000r/min stirring condition, the pH value making solution is 7.2 ~ 7.4, obtains mixed liquor I; Mixed liquor H is joined in mixed liquor I under 1000r/min stirring condition, is then placed in 43 DEG C of water-baths and stirs 90 ~ 100 minutes under 1000r/min condition, obtain mixed liquor J; Under 1000r/min stirring condition, the HCl solution that the NaOH solution that concentration is 0.01mol/L and concentration are 0.005mol/L is dripped in mixed liquor J, the pH value of solution is made to be 3.7 ~ 3.9, then be placed in 38 DEG C of water-baths to stir 90 ~ 100 minutes under 1000r/min condition, obtain mixed liquor K; 1600mL deionized water is added drop-wise in mixed liquor K under 1000r/min stirring condition, then under 1000r/min condition, stirs 8min, obtain mixed liquor L.
By 240mL mass fraction be 8.5% poly beta-hydroxybutyrate chloroformic solution and 60mL mass fraction be 6.5% polyethylene glycol chloroformic solution fully mix, obtain mixed liquor M.
60mL mixed liquor L is added drop-wise in mixed liquor M under 1000r/min stirring condition, then under 1000r/min condition, stirs 8min, obtain mixed liquor N.
60mL mixed liquor F is added drop-wise in mixed liquor N under 1000r/min stirring condition, then under 1000r/min condition, stirs 8min, obtain mixed liquor O; It is in the poly-vinyl alcohol solution of 5.5% that 420mL mixed liquor O is added drop-wise to 210mL mass fraction under 1000r/min stirring condition, then under 1000r/min condition, stirs 8min, obtains mixed liquor P; By 1380mL mass fraction be 0.7% poly-vinyl alcohol solution join in mixed liquor P, 7 ~ 8h is stirred under 1000r/min condition, then under rotating speed is 6000r/min condition, centrifugation is carried out, then spend deionized water 3 times, freeze drying can obtain the biodegradable multifunctional ceiling elaioleucite that may float on the water surface.
Here is that the biodegradable multifunctional ceiling elaioleucite that may float on the water surface using the inventive method to obtain has carried out absorption and enhanced biodegradation test to the petroleum hydrocarbon in oil spill water body, further illustrates the present invention.
The biodegradable multifunctional ceiling elaioleucite that may float on the water surface using the inventive method to obtain has carried out absorption and enhanced biodegradation test to the petroleum hydrocarbon in oil spill water body, result shows that this oil suction particle effectively can adsorb and enhanced biodegradation the petroleum hydrocarbon in water body: when the initial concentration of polluted-water Petroleum Hydrocarbon is 86.4mg/L, 8g oil suction particle is added in the water body of 500mL, add petroleum hydrocarbon degradation bacterium, make the bacteria containing amount of solution be 5 × 10 7cFU/ml, after 10 hours, the concentration of water body Petroleum Hydrocarbon is reduced to 0.01mg/L, and after 45 days, oil suction particle Petroleum Hydrocarbon concentration does not detect, and after 150 days, the quality of oil suction particle reduces by 62%.

Claims (1)

1. may float on a preparation method for the biodegradable multifunctional ceiling elaioleucite of the water surface, it is characterized in that, the concrete steps of the method are as follows:
(1) be the NH of 0.35mol/L by 100mL concentration 4hCO 3solution and 100mL concentration are the NH of 0.62mol/L 4h 2pO 4mixing, obtain mixed liquor A 1, is then the NH of 0.01mol/L by concentration 4oH solution and concentration are that the hydrochloric acid solution of 0.01mol/L regulates the pH value of mixed liquor A 1 to be 9.0, obtain mixed liquor A;
(2) 200mL mixed liquor A is slowly added drop-wise under agitation the Ca (NO that 300mL concentration is 0.025mol/L 3) 2in solution, obtain mixed liquid B;
(3) in mixed liquid B, dense HNO is dropwise added 3to clarification, obtain mixed liquor C;
(4) regulate the pH value of mixed liquor C to be 3.5 with the salpeter solution of concentration to be the NaOH solution of 0.01mol/L and concentration be 0.01mol/L, obtain mixed liquor D;
(5) in mixed liquor D, add the aqueous solution of urea that 100mL concentration is 1.2mol/L, after mixing, obtain mixed liquor E;
(6) in mixed liquor E, add the calcio-disodium edetate solution that 50mL concentration is 0.15mol/L, after mixing, obtain mixed liquor F;
(7) by 60mL mass fraction be 45% aqueous solution of urea be placed in 43 DEG C of water-bath constant temperature and obtain mixed liquor G in 35 minutes; By 10mL mass fraction be 35% formalin be placed in 43 DEG C of water-bath constant temperature and obtain mixed liquor H in 35 minutes;
(8) in mixed liquor G, drip the HCl solution that the NaOH solution that concentration is 0.01mol/L and concentration are 0.005mol/L under 1000r/min stirring condition, the pH value making solution is 7.2 ~ 7.4, obtains mixed liquor I;
(9) mixed liquor H is joined in mixed liquor I under 1000r/min stirring condition, be then placed in 43 DEG C of water-baths and stir 90 ~ 100 minutes under 1000r/min condition, obtain mixed liquor J;
(10) in mixed liquor J, under 1000r/min stirring condition, drip the HCl solution that the NaOH solution that concentration is 0.01mol/L and concentration are 0.005mol/L, the pH value of solution is made to be 3.7 ~ 3.9, then be placed in 38 DEG C of water-baths to stir 90 ~ 100 minutes under 1000r/min condition, obtain mixed liquor K;
(11) 1600mL deionized water is added drop-wise in mixed liquor K under 1000r/min stirring condition, then under 1000r/min condition, stirs 8min, obtain mixed liquor L;
(12) by 240mL mass fraction be 8.5% poly beta-hydroxybutyrate chloroformic solution and 60mL mass fraction be 6.5% polyethylene glycol chloroformic solution fully mix, obtain mixed liquor M;
(13) 60mL mixed liquor L is added drop-wise in mixed liquor M under 1000r/min stirring condition, then under 1000r/min condition, stirs 8min, obtain mixed liquor N;
(14) 60mL mixed liquor F is added drop-wise in mixed liquor N under 1000r/min stirring condition, then under 1000r/min condition, stirs 8min, obtain mixed liquor O;
(15) 420mL mixed liquor O being added drop-wise to 210mL mass fraction under 1000r/min stirring condition is in the poly-vinyl alcohol solution of 5.5%, then under 1000r/min condition, stirs 8min, obtains mixed liquor P;
(16) by 1380mL mass fraction be 0.7% poly-vinyl alcohol solution join in mixed liquor P, 7 ~ 8h is stirred under 1000r/min condition, then under rotating speed is 6000r/min condition, centrifugation is carried out, then spend deionized water 3 times, freeze drying can obtain the biodegradable multifunctional ceiling elaioleucite that may float on the water surface.
CN201310684720.XA 2013-12-12 2013-12-12 May float on biodegradable multifunctional ceiling elaioleucite and the preparation method of the water surface Expired - Fee Related CN103611506B (en)

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WO2004058647A1 (en) * 2002-12-31 2004-07-15 Ku-Su Kim Wastewater disposal agent and process for preparing thereof
CN102500340B (en) * 2011-09-30 2013-05-01 北京师范大学 Porous particle with functions of adsorbing and biodegrading petroleum hydrocarbon and preparation method of porous particle
CN102408160B (en) * 2011-09-30 2013-01-02 北京师范大学 Biodegradable perforated plate for adsorption and biodegradation of petroleum hydrocarbon pollutants as well as preparation method thereof
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CN102963959B (en) * 2012-12-03 2013-11-13 北京师范大学 Preparation method of microsphere particles capable of slowly releasing nitrogen and adsorbing-biologically degrading petroleum hydrocarbon
CN102976499B (en) * 2012-12-03 2013-12-04 北京师范大学 Method for preparing composite board capable of simultaneously slowly releasing nitrogen and adsorbing/biologically degrading petroleum hydrocarbons

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