CN101709277A - Method for preparing biological compound demulsifying agent - Google Patents
Method for preparing biological compound demulsifying agent Download PDFInfo
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- CN101709277A CN101709277A CN200910073131A CN200910073131A CN101709277A CN 101709277 A CN101709277 A CN 101709277A CN 200910073131 A CN200910073131 A CN 200910073131A CN 200910073131 A CN200910073131 A CN 200910073131A CN 101709277 A CN101709277 A CN 101709277A
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- demulsifying agent
- seed liquor
- biological compound
- bacillus
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Abstract
The invention discloses a method for preparing a biological compound demulsifying agent, which relates to a method for preparing a demulsifying agent. The method solves the problems that the harms to the environment caused by a chemical demulsifying agent still exist although the conventional biological demulsifying agent is compounded with the chemical demulsifying agent or auxiliary agents with other functions, and the biological demulsifying agent has low demulsifying efficiency, poor stability and high cost. The method comprises the following steps: firstly, preparing a bacillus mojavensis seed solution; secondly, preparing a bacillus subtillis seed solution; and finally, mixing the bacillus mojavensis seed solution and the bacillus subtillis seed solution, and inoculating the mixture into a culture medium for culture to obtain the biological compound demulsifying agent. The biological compound demulsifying agent has an oil expulsion rate up to 100 percent, reduces the addition and the cost, has high stability which is shown by good demulsifying effect on emulsions under the condition of the pH value of 3 to 9, and the change of the oil expulsion rate of not more than 10 percent when the temperature of the emulsions changes between 20 and 120 DEG C.
Description
Technical field
The present invention relates to a kind of preparation method of emulsion splitter.
Background technology
Emulsion splitter has important effect in fields such as crude production, transportation and greasy dirt separation, removals.The main chemical demulsifier that uses carries out oily water separation in the industry for a long time.Yet chemical demulsifier shows stronger specificity, and a large amount of inorganic salt or organic residue can be brought in the crude oil waste water.The waste water that discharging contains chemical residue can cause serious harm to environment, can improve production cost greatly and such waste water handled.The biological demulsifying technology utilizes microorganism cells itself or its metabolic process, meta-bolites to realize emulsion breakdown, and it is simple to have production technique, the advantage that energy consumption is little.The more important thing is that biological demulsifying agent is nontoxic, easily be degraded, its feature of environmental protection is that chemical demulsifier is incomparable, is one of important directions of emulsion splitter research and development.There have report that the auxiliary agent of biological demulsifying agent and chemical demulsifier or other functions is carried out to be composite, reducing the consumption of chemical demulsifier, but still the harm that can not avoid chemical demulsifier that environment is caused.
At present, biological demulsifying agent exists breakdown of emulsion efficient low, the problem of less stable, and also because usage quantity causes the cost height more greatly, these have all restricted biological demulsifying agent scale operation and application.
Summary of the invention
The present invention seeks to carry out compositely, but still exist chemical demulsifier that environment is worked the mischief in order to solve existing auxiliary agent with biological demulsifying agent and chemical demulsifier or other functions; And biological demulsifying agent exists breakdown of emulsion efficient low, less stable, the problem that cost is high, and the preparation method of a kind of biological compound demulsifying agent that provides.
The preparation method of biological compound demulsifying agent carries out according to the following steps: one, Mo Haiwei genus bacillus (Bacillus mojavensis) is inoculated in the MMSM liquid nutrient medium, under being 28～32 ℃, the condition of 140r/min, temperature cultivates 24h, De Mohaiwei genus bacillus seed liquor; Two, Bacillus subtillis (Bacillus subtilis) is inoculated in the MMSM liquid nutrient medium, under temperature is 28～32 ℃, the condition of 140r/min, cultivates 20h, the Bacillus subtillis seed liquor; Three, the Mo Haiwei genus bacillus seed liquor of 3～4ml and the Bacillus subtillis seed liquor of 1.5～2.5ml are inoculated in respectively in the MMSM liquid nutrient medium of 100ml, in temperature is that 32～35 ℃, shaking table revolution are that 80～160r/min, pH value are to cultivate 10～16h under 7～8 the condition, promptly gets biological compound demulsifying agent; Wherein the absorbancy of Mo Haiwei genus bacillus seed liquor at 620nm wavelength place is 3.4～4.7 in the step 1; The absorbancy of Bacillus subtillis seed liquor at 620nm wavelength place is 0.08～0.3 in the step 2; MMSM liquid culture based component is identical in the step 1, two and three, and the MMSM liquid nutrient medium is by the NH of 3.0～4.0g
4NO
3, 3.0～4.0g K
2HPO
4, 4.0～6.0g KH
2PO
4, 0.1～0.2g MgSO
4H
2The yeast extract paste of the trace element solution of O, 0.5～1mL, the whiteruss of 40mL, 0.5～1.0g and the glucose of 8.0～10.0g are dissolved in the distilled water of 1000mL to be formed, and described trace element solution is by the CaCl of 1000mg
2H
2The FeSO of O, 1000mg
47H
2The EDTA of O and 1400mg is dissolved in the distilled water of 1000mL and forms.
Biological compound demulsifying agent of the present invention is compared with the emulsion splitter that single culture is formed, and has improved the breakdown of emulsion efficient of biological demulsifying agent, and under the same conditions, lower dosage can reach the breakdown of emulsion top efficiency, and the oil extraction rate is up to 100%.Biological compound demulsifying agent of the present invention can be directly used in the processing to oil field waste, and whole process is carried out at normal temperatures, has reduced the working cost of technology.Biological compound demulsifying agent of the present invention is compared with present widely used chemical demulsifier, and demulsification meets or exceeds chemical demulsifier fully.Composite type biological emulsion splitter of the present invention adopts microorganism to carry out composite demulsification fully, do not contain any chemical demulsifier or auxiliary agent, avoided chemical demulsifier that environment is worked the mischief fully, can degrade fully, and behind the breakdown of emulsion, it is residual not have a large amount of chemical substances in the waste water, has reduced the difficulty of subsequent wastewater treatment, has saved cost.Biological compound demulsifying agent of the present invention has improved breakdown of emulsion efficient than using single inoculum breakdown of emulsion to reduce the add-on of emulsion splitter, can reduce production costs significantly.Biological compound demulsifying agent of the present invention is under 3～9 the condition O/W pattern type milk sap all to be had demulsification preferably in the pH value.The breakdown of emulsion ability of biological compound demulsifying agent is floated little with variation of temperature among the present invention, the milk sap temperature changes in 20～120 ℃, the oil extraction rate variation of emulsion splitter is no more than 10%, as seen the stability of biological compound demulsifying agent of the present invention is high, help being positioned at the extremely frigid zones crude oil extraction liquid breakdown of emulsion in winter, can save the required energy consumption of heating and further reduce cost, can utilize the oil field existing installation to add simultaneously, be easy to large-scale application.
Description of drawings
Fig. 1 be in the embodiment four biological compound demulsifying agent and single inoculum at dosage not simultaneously to the demulsification comparison diagram of O/W pattern type milk sap, wherein ■ is the demulsification curve of biological compound demulsifying agent, ▲ be the demulsification curve of Mo Haiwei bacillus nutrient solution; ● be the demulsification curve of Bacillus subtillis nutrient solution; Fig. 2 be in the embodiment four biological compound demulsifying agent and single inoculum under different pH condition to the demulsification comparison diagram of O/W pattern type milk sap, wherein ■ is the demulsification curve of biological compound demulsifying agent, ▲ be the demulsification curve of Mo Haiwei bacillus nutrient solution; ● be the demulsification curve of Bacillus subtillis nutrient solution; Fig. 3 be in the embodiment four biological compound demulsifying agent and single inoculum under condition of different temperatures to the demulsification comparison diagram of O/W pattern type milk sap, wherein ■ is the demulsification curve of biological compound demulsifying agent, ▲ be the demulsification curve of Mo Haiwei bacillus nutrient solution; ● be the demulsification curve of Bacillus subtillis nutrient solution.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of present embodiment biological compound demulsifying agent carries out according to the following steps: one, the Mo Haiwei genus bacillus is inoculated in the MMSM liquid nutrient medium, under being 28～32 ℃, the condition of 140r/min, temperature cultivates 24h, De Mohaiwei genus bacillus seed liquor; Two, Bacillus subtillis is inoculated in the MMSM liquid nutrient medium, under temperature is 28～32 ℃, the condition of 140r/min, cultivates 20h, the Bacillus subtillis seed liquor; Three, the Mo Haiwei genus bacillus seed liquor of 3～4ml and the Bacillus subtillis seed liquor of 1.5～2.5ml are inoculated in respectively in the MMSM liquid nutrient medium of 100ml, in temperature is that 32～35 ℃, shaking table revolution are that 80～160r/min, pH value are to cultivate 10～16h under 7～8 the condition, promptly gets biological compound demulsifying agent; Wherein the absorbancy of Mo Haiwei genus bacillus seed liquor at 620nm wavelength place is 3.4～4.7 in the step 1; The absorbancy of Bacillus subtillis seed liquor at 620nm wavelength place is 0.08～0.3 in the step 2; MMSM liquid culture based component is identical in the step 1, two and three, and the MMSM liquid nutrient medium is by the NH of 3.0～4.0g
4NO
3, 3.0～4.0g K
2HPO
4, 4.0～6.0g KH
2PO
4, 0.1～0.2g MgSO
4H
2The yeast extract paste of the trace element solution of O, 0.5～1mL, the whiteruss of 40mL, 0.5～1.0g and the glucose of 8.0～10.0g are dissolved in the distilled water of 1000mL to be formed, and described trace element solution is by the CaCl of 1000mg
2H
2The FeSO of O, 1000mg
47H
2The EDTA of O and 1400mg is dissolved in the distilled water of 1000mL and forms.
Bacillus subtillis obtains for directly buying in the present embodiment.
The Mo Haiwei genus bacillus obtains for gathering voluntarily, also can directly buying in the present embodiment.
The MMSM liquid nutrient medium is at 112 ℃ of 20min that sterilize down in the present embodiment.
Embodiment two: what present embodiment and embodiment one were different is in the step 3 Mo Haiwei genus bacillus seed liquor of 3.5ml to be mixed with the Bacillus subtillis seed liquor of 2ml.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is in the step 3 Mo Haiwei genus bacillus seed liquor of 3ml to be mixed with the Bacillus subtillis seed liquor of 1.5ml.Other step and parameter are identical with embodiment one.
Embodiment four: the preparation method of present embodiment biological compound demulsifying agent carries out according to the following steps: one, the Mo Haiwei genus bacillus is inoculated in the MMSM liquid nutrient medium, under being 30 ℃, the condition of 140r/min, temperature cultivates 24h, De Mohaiwei genus bacillus seed liquor; Two, Bacillus subtillis is inoculated in the MMSM liquid nutrient medium, under temperature is 30 ℃, the condition of 140r/min, cultivates 20h, the Bacillus subtillis seed liquor; Three, the Mo Haiwei genus bacillus seed liquor of 3.5ml and the Bacillus subtillis seed liquor of 2ml are inoculated in respectively in the MMSM liquid nutrient medium of 100ml, in temperature is that 30 ℃, shaking table revolution are that 140r/min, pH value are to cultivate 10～16h under 8 the condition, promptly gets biological compound demulsifying agent; Wherein the absorbancy of Mo Haiwei genus bacillus seed liquor at 620nm wavelength place is 4.0 in the step 1; The absorbancy of Bacillus subtillis seed liquor at 620nm wavelength place is 0.1 in the step 2; MMSM liquid nutrient medium composition is identical in the step 1, two and three, and the MMSM liquid nutrient medium is by the NH of 3.5g
4NO
3, 3.5g K
2HPO
4, 5.0g KH
2PO
4, 0.15g MgSO
4H
2The yeast extract paste of the trace element solution of O, 0.8mL, the whiteruss of 40mL, 0.8g and the glucose of 9.0g are dissolved in the distilled water of 1000mL to be formed, and described trace element solution is by the CaCl of 1000mg
2H
2The FeSO of O, 1000mg
47H
2The EDTA of O and 1400mg is dissolved in the distilled water of 1000mL and forms.
Present embodiment gained biological compound demulsifying agent and the demulsification contrast of adopting single Mo Haiwei bacillus nutrient solution or Bacillus subtillis nutrient solution, the result as shown in Figure 1, present embodiment gained biological compound demulsifying agent just can reach the breakdown of emulsion best effect under the situation of consumption 2.5ml, the oil extraction rate reaches 100%; The add-on of Mo Haiwei bacillus nutrient solution is that 4ml can reach best oil extraction effect, 48h oil extraction rate 63%; The optimal addn of Bacillus subtillis nutrient solution is then higher, and when adding the full nutrient solution of 6ml, the oil extraction rate reaches 65%; This shows that present embodiment gained biological compound demulsifying agent has improved breakdown of emulsion efficient than using single inoculum breakdown of emulsion to reduce the add-on of emulsion splitter, can reduce cost significantly.
The adaptive faculty that present embodiment gained biological compound demulsifying agent changes milk sap pH value, as shown in Figure 2, present embodiment gained biological compound demulsifying agent is under 3～9 the condition O/W pattern type milk sap all to be had demulsification preferably in the pH value.
The right breakdown of emulsion ability of present embodiment gained biological compound demulsifying agent is floated little with variation of temperature, as shown in Figure 3, the milk sap temperature changes in 20～120 ℃, and the oil extraction rate variation of present embodiment gained biological compound demulsifying agent is no more than 10%; This shows that the stability of present embodiment gained biological compound demulsifying agent is high, helps being positioned at the extremely frigid zones crude oil extraction liquid breakdown of emulsion in winter, can save the required energy consumption of heating and further reduce cost.
Present embodiment gained biological compound demulsifying agent is for the treatment effect of Daqing oil field oily(waste)water (crude oil waste water oleaginousness is 153.217mg/L), as shown in table 1, present embodiment gained biological compound demulsifying agent is compared with the demulsification of independent use Mo Haiwei bacillus nutrient solution or Bacillus subtillis nutrient solution, under the equal conditions, can improve the oil extraction rate more than 13%; Compare with present widely used chemical demulsifier (chemistry-1 composition is the polyoxyethylene polyoxypropylene propylene glycol, and chemistry-2 compositions are poly-ethylene group polyquaternium), demulsification meets or exceeds chemical demulsifier fully.
Table 1
Claims (3)
1. the preparation method of a biological compound demulsifying agent, the preparation method who it is characterized in that biological compound demulsifying agent carries out according to the following steps: one, the Mo Haiwei genus bacillus is inoculated in the MMSM liquid nutrient medium, under being 28～32 ℃, the condition of 140r/min, temperature cultivates 24h, De Mohaiwei genus bacillus seed liquor; Two, Bacillus subtillis is inoculated in the MMSM liquid nutrient medium, under temperature is 28～32 ℃, the condition of 140r/min, cultivates 20h, the Bacillus subtillis seed liquor; Three, the Mo Haiwei genus bacillus seed liquor of 3～4ml is mixed with the Bacillus subtillis seed liquor of 1.5～2.5ml, be inoculated in then in the MMSM liquid nutrient medium of 100ml, in temperature is that 32～35 ℃, shaking table revolution are that 80～160r/min, pH value are to cultivate 10～16h under 7～8 the condition, promptly gets biological compound demulsifying agent; Wherein the absorbancy of Mo Haiwei genus bacillus seed liquor at 620nm wavelength place is 3.4～4.7 in the step 1; The absorbancy of Bacillus subtillis seed liquor at 620nm wavelength place is 0.08～0.3 in the step 2; MMSM liquid culture based component is identical in the step 1, two and three, and the MMSM liquid nutrient medium is by the NH of 3.0～4.0g
4NO
3, 3.0～4.0g K
2HPO
4, 4.0～6.0g KH
2PO
4, 0.1～0.2g MgSO
4H
2The yeast extract paste of the trace element solution of O, 0.5～1mL, the whiteruss of 40mL, 0.5～1.0g and the glucose of 8.0～10.0g are dissolved in the distilled water of 1000mL to be formed, and described trace element solution is by the CaCl of 1000mg
2H
2The FeSO of O, 1000mg
47H
2The EDTA of O and 1400mg is dissolved in the distilled water of 1000mL and forms.
2. the preparation method of a kind of biological compound demulsifying agent according to claim 1 is characterized in that in the step 3 Mo Haiwei genus bacillus seed liquor of 3.5ml being mixed with the Bacillus subtillis seed liquor of 2ml.
3. the preparation method of a kind of biological compound demulsifying agent according to claim 1 is characterized in that in the step 3 Mo Haiwei genus bacillus seed liquor of 3ml being mixed with the Bacillus subtillis seed liquor of 1ml.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350261A (en) * | 2011-07-14 | 2012-02-15 | 同济大学 | Extraction method of cell wall bound biodemulsifier |
| CN102796613A (en) * | 2012-08-14 | 2012-11-28 | 东北农业大学 | Demulsification method by soybean grease microbe extraction through aqueous enzymatic method |
| CN105255582A (en) * | 2015-11-04 | 2016-01-20 | 北京科慧通智慧科技有限公司 | Bitter apricot kernel oil with high extraction rate and extraction method thereof |
| CN105296139A (en) * | 2015-11-04 | 2016-02-03 | 邵素英 | High-demulsification-rate bitter almond oil and extraction method thereof |
| CN106566580A (en) * | 2016-11-10 | 2017-04-19 | 仇颖莹 | Preparation method for composite biological oilfield demulsifier |
| CN112473187A (en) * | 2021-01-07 | 2021-03-12 | 东北农业大学 | Hydrophobic modified protein biological demulsifier |
| CN115785940A (en) * | 2022-12-01 | 2023-03-14 | 克拉玛依中科恒信科技有限责任公司 | Demulsification cleanup additive for fracture acidizing and preparation method and use method thereof |
-
2009
- 2009-11-03 CN CN200910073131A patent/CN101709277A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350261A (en) * | 2011-07-14 | 2012-02-15 | 同济大学 | Extraction method of cell wall bound biodemulsifier |
| CN102350261B (en) * | 2011-07-14 | 2014-09-17 | 同济大学 | Extraction method of cell wall bound biodemulsifier |
| CN102796613A (en) * | 2012-08-14 | 2012-11-28 | 东北农业大学 | Demulsification method by soybean grease microbe extraction through aqueous enzymatic method |
| CN105255582A (en) * | 2015-11-04 | 2016-01-20 | 北京科慧通智慧科技有限公司 | Bitter apricot kernel oil with high extraction rate and extraction method thereof |
| CN105296139A (en) * | 2015-11-04 | 2016-02-03 | 邵素英 | High-demulsification-rate bitter almond oil and extraction method thereof |
| CN106566580A (en) * | 2016-11-10 | 2017-04-19 | 仇颖莹 | Preparation method for composite biological oilfield demulsifier |
| CN106566580B (en) * | 2016-11-10 | 2018-12-07 | 胜利油田德利实业有限责任公司 | A kind of preparation method of compound bio oil field demulsifier |
| CN112473187A (en) * | 2021-01-07 | 2021-03-12 | 东北农业大学 | Hydrophobic modified protein biological demulsifier |
| CN115785940A (en) * | 2022-12-01 | 2023-03-14 | 克拉玛依中科恒信科技有限责任公司 | Demulsification cleanup additive for fracture acidizing and preparation method and use method thereof |
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Open date: 20100519 |