CN105694952A - Preparation method of compound microorganism demulsifying agent - Google Patents

Preparation method of compound microorganism demulsifying agent Download PDF

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Publication number
CN105694952A
CN105694952A CN201610144381.XA CN201610144381A CN105694952A CN 105694952 A CN105694952 A CN 105694952A CN 201610144381 A CN201610144381 A CN 201610144381A CN 105694952 A CN105694952 A CN 105694952A
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added
parts
mixture
preparation
culture fluid
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汪巍
盛艳花
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Changzhou Lanxu Chemical Co Ltd
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Changzhou Lanxu Chemical Co Ltd
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Priority to CN201610144381.XA priority Critical patent/CN105694952A/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G33/00Dewatering or demulsification of hydrocarbon oils
    • C10G33/04Dewatering or demulsification of hydrocarbon oils with chemical means

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Micro-Organisms Or Cultivation Processes Thereof (AREA)

Abstract

The invention discloses a preparation method of a compound microorganism demulsifying agent and belongs to the technical field of demulsifying agent preparation. Agar, glycerin and the like are taken for preparing a culture solution, the culture solution is added into bottom mud excavated from the bottom of the earth' surface of an oil field for cultivation, a fermentation solution is obtained by means of fermentation and centrifuging, soybean straw is washed and aired and then is smashed into straw fibers, the fermentation solution, dichloroethane and diisopropyl hydrogen phosphate are added for ultrasonic dispersion processing, the mixture is mixed with ethylene glycol monomethyl ether for heat-preserving processing, sodium alginate is added for packaging, and the demulsifying agent is prepared through spraying and drying. The preparation method has the advantages that preparation steps are simple, the dewatering rate of the obtained product is 20% or above higher than that of other products, and dewatering speed is high; the using amount is small, the effects is good, and it is avoided that the demulsifying agent is affected by electrolyte and accordingly the effect is reduced.

Description

A kind of preparation method of complex microorganism demulsifier
Technical field
The preparation method that the present invention relates to a kind of complex microorganism demulsifier, belongs to demulsifier preparing technical field。
Background technology
Demulsifier is a kind of surfactant, and it can make the liquid structure of emulsifying shape destroy, to reach respectively to be separated in emulsion the purpose come。Crude oil demulsification refers to that oil and water in the oil-water mixture of emulsifying shape are separated by the chemical action utilizing demulsifier, makes up to the purpose of the dehydration of crude oil, to ensure that crude oil exporting is containing water quality standard。Demulsifier of a great variety, can be divided into by the sorting technique of surfactant: cationic, anionic, non-ionic, amphitypy ionic demulsifying agent。Anionic demulsifier has metal carboxylate, Sulfonates and Polyoxyethylene fatty sulfuric acid etc., has that consumption is big, weak effect, is subject to Influence of Electrolyte and subtracts effect, the shortcomings such as dehydration rate is low, dewatering speed is slow;Cationic demulsifier mainly has quaternary ammonium salt, and thin oil is had positive effect by it, but is not suitable for viscous crude and ageing oil;Non-ionic mainly have the block polyether being initiator with amine, the block polyether being initiator with alcohols, alkyl phenolic resin block polyether, phenol amine aldehyde resin block polyether, silicon demulsifier, super-high relative molecular weight demulsifier, poly phosphate, the modified product of block polyether and the amphitypy ionic demulsifying agent being representative with imidazoline crude oil demulsifier。Non-ionic demulsifier key component conventional in current oil field is polyoxyethylene polyoxypropylene octadecanol ether, to the crude oil containing resin and asphalt higher (or moisture more than 20%), the breakdown of emulsion ability of SP type demulsifier is more weak, wettability and permeance property are poor, reason is that molecular structure is single, unbranched structure and aromatic structure。Therefore work out the demulsifier that a kind of dehydration rate is high, dewatering speed is fast on this basis, have great importance。
Summary of the invention
The technical problem to be solved: big for anionic demulsifier consumption, weak effect, it is subject to Influence of Electrolyte and subtracts effect, dehydration rate is low, the drawback that dewatering speed is slow, provide one and take agar, the prepared culture fluid such as glycerol, it is added into the bed mud taken bottom earth's surface, oil field and cultivates, fermented, it is centrifuged to obtain fermentation liquid, take soybean stalk again, rinse air-dry after be ground into stalk fibre, add fermentation liquid, dichloroethanes and diisopropyl phosphite ultrasonic disperse process, with glycol monoethyl ether mixing isothermal holding, add sodium alginate to wrap up, the method of spray-dried prepared demulsifier。Preparation process of the present invention is simple, and products obtained therefrom dehydration rate is higher than other products more than 20%, and dewatering speed is fast。
For solving above-mentioned technical problem, the present invention adopts the technical scheme as described below to be:
(1) counting by weight, choose 15~30 parts of agar, 5~10 parts of glycerol, 5~10 parts of glucoses, 10~15 parts of peptones and 35~65 parts of water, under 160r/min, stirring mixing, is placed in shaking table oscillation treatment 50~60min, prepares culture fluid;
(2) from 10~20m under earth's surface, oil field, take 1~2kg bed mud and put in culture dish, by bed mud and culture fluid solid-to-liquid ratio 2:1, being added in bed mud by culture fluid, controlling temperature is 20~24 DEG C, cultivates 3~5 days, change a culture fluid every 10~16h, obtain mixture;
(3) mixture of above-mentioned gained is put in fermentation tank, being added to the glycine betaine of mixture quality 3~5%, controlling fermentation temperature is 28~35 DEG C, sealing and fermenting 3~5 days simultaneously, it is subsequently placed in 3000r/min centrifuge centrifugation 10~15min, obtains fermentation liquid;
(4) 0.5~0.7kg soybean stalk is weighed, rinse 2~3 times with clear water, it is placed in ventilation natural air drying, put into after air-dry in pulverizer and be ground into the stalk fibre that length is 1~2cm, stalk fibre is added in the fermentation liquid of above-mentioned gained, it is added to 30~50mL dichloroethanes and 20~30mL diisopropyl phosphite simultaneously respectively, 300~500W ultrasonic dispersers carries out ultrasonic disperse and processes 30~50min;
(5) after ultrasonic disperse processes, the stalk fibre mixture of gained will add 30~50mL glycol monoethyl ether, it is placed at 30~38 DEG C and is incubated 4~6h, after being incubated, being added to 20~30g sodium alginate, stirring makes it be sufficiently mixed uniformly, is placed in 500~550W ultrasonic dispersers ultrasonic disperse process 30~40min, it is placed in spray dryer again and carries out spray drying 1~2h, namely prepare a kind of complex microorganism demulsifier。
The application process of the present invention: the complex microorganism demulsifier present invention prepared is added in crude oil, addition is 3~5mg/L, is 40~45 DEG C in temperature, and rotating speed is that under 80r/min, stirring makes it be sufficiently mixed uniformly, stands 3~5h,。This By Demulsifier is good, and consumption is few, and dehydration rate is higher than other products more than 20%, and dewatering speed is fast, is worthy to be popularized and use。
The present invention is compared with additive method, and Advantageous Effects is:
(1) preparation process of the present invention is simple, and products obtained therefrom dehydration rate is higher than other products more than 20%, and dewatering speed is fast;
(2) consumption is few, effective, is susceptible to Influence of Electrolyte and subtracts effect。
Detailed description of the invention
First counting by weight, choose 15~30 parts of agar, 5~10 parts of glycerol, 5~10 parts of glucoses, 10~15 parts of peptones and 35~65 parts of water, under 160r/min, stirring mixing, is placed in shaking table oscillation treatment 50~60min, prepares culture fluid;Then from 10~20m under earth's surface, oil field, take 1~2kg bed mud and put in culture dish, by bed mud and culture fluid solid-to-liquid ratio 2:1, being added in bed mud by culture fluid, controlling temperature is 20~24 DEG C, cultivates 3~5 days, change a culture fluid every 10~16h, obtain mixture;The mixture of above-mentioned gained is put in fermentation tank, being added to the glycine betaine of mixture quality 3~5%, controlling fermentation temperature is 28~35 DEG C, sealing and fermenting 3~5 days simultaneously, it is subsequently placed in 3000r/min centrifuge centrifugation 10~15min, obtains fermentation liquid;Weigh 0.5~0.7kg soybean stalk, rinse 2~3 times with clear water, it is placed in ventilation natural air drying, put into after air-dry in pulverizer and be ground into the stalk fibre that length is 1~2cm, stalk fibre is added in the fermentation liquid of above-mentioned gained, it is added to 30~50mL dichloroethanes and 20~30mL diisopropyl phosphite simultaneously respectively, 300~500W ultrasonic dispersers carries out ultrasonic disperse and processes 30~50min;Finally after ultrasonic disperse processes, the stalk fibre mixture of gained will add 30~50mL glycol monoethyl ether, it is placed at 30~38 DEG C and is incubated 4~6h, after being incubated, being added to 20~30g sodium alginate, stirring makes it be sufficiently mixed uniformly, is placed in 500~550W ultrasonic dispersers ultrasonic disperse process 30~40min, it is placed in spray dryer again and carries out spray drying 1~2h, namely prepare a kind of complex microorganism demulsifier。
Example 1
First counting by weight, choose 15 parts of agar, 5 parts of glycerol, 5 parts of glucoses, 10 parts of peptones and 65 parts of water, under 160r/min, stirring mixing, is placed in shaking table oscillation treatment 50min, prepares culture fluid;Then from 10m under earth's surface, oil field, taking 1kg bed mud and put in culture dish, by bed mud and culture fluid solid-to-liquid ratio 2:1, be added in bed mud by culture fluid, controlling temperature is 20 DEG C, cultivates 3 days, changes a culture fluid every 10h, obtains mixture;Putting in fermentation tank by the mixture of above-mentioned gained, be added to the glycine betaine of mixture quality 3% simultaneously, controlling fermentation temperature is 28 DEG C, sealing and fermenting 3 days, is subsequently placed in 3000r/min centrifuge centrifugation 10min, obtains fermentation liquid;Weigh 0.5kg soybean stalk, rinse 2 times with clear water, it is placed in ventilation natural air drying, put into after air-dry in pulverizer and be ground into the stalk fibre that length is 1cm, stalk fibre is added in the fermentation liquid of above-mentioned gained, it is added to 30mL dichloroethanes and 20mL diisopropyl phosphite simultaneously respectively, 300W ultrasonic dispersers carries out ultrasonic disperse and processes 30min;Finally after ultrasonic disperse processes, the stalk fibre mixture of gained will add 30mL glycol monoethyl ether, it is placed at 30 DEG C and is incubated 4h, after being incubated, being added to 20g sodium alginate, stirring makes it be sufficiently mixed uniformly, is placed in 500W ultrasonic dispersers ultrasonic disperse process 30min, it is placed in spray dryer again and carries out spray drying 1h, namely prepare a kind of complex microorganism demulsifier。
The complex microorganism demulsifier present invention prepared is added in crude oil, and addition is 3mg/L, is 40 DEG C in temperature, and rotating speed is that under 80r/min, stirring makes it be sufficiently mixed uniformly, stands 3h,。This By Demulsifier is good, and consumption is few, and dehydration rate is higher than other products 20.3%, and dewatering speed is fast, is worthy to be popularized and use。
Example 2
First counting by weight, choose 23 parts of agar, 7 parts of glycerol, 8 parts of glucoses, 12 parts of peptones and 50 parts of water, under 160r/min, stirring mixing, is placed in shaking table oscillation treatment 55min, prepares culture fluid;Then from 15m under earth's surface, oil field, taking 2kg bed mud and put in culture dish, by bed mud and culture fluid solid-to-liquid ratio 2:1, be added in bed mud by culture fluid, controlling temperature is 22 DEG C, cultivates 4 days, changes a culture fluid every 13h, obtains mixture;Putting in fermentation tank by the mixture of above-mentioned gained, be added to the glycine betaine of mixture quality 4% simultaneously, controlling fermentation temperature is 32 DEG C, sealing and fermenting 4 days, is subsequently placed in 3000r/min centrifuge centrifugation 13min, obtains fermentation liquid;Weigh 0.6kg soybean stalk, rinse 3 times with clear water, it is placed in ventilation natural air drying, put into after air-dry in pulverizer and be ground into the stalk fibre that length is 2cm, stalk fibre is added in the fermentation liquid of above-mentioned gained, it is added to 40mL dichloroethanes and 25mL diisopropyl phosphite simultaneously respectively, 400W ultrasonic dispersers carries out ultrasonic disperse and processes 40min;Finally after ultrasonic disperse processes, the stalk fibre mixture of gained will add 40mL glycol monoethyl ether, it is placed at 34 DEG C and is incubated 5h, after being incubated, being added to 25g sodium alginate, stirring makes it be sufficiently mixed uniformly, is placed in 525W ultrasonic dispersers ultrasonic disperse process 35min, it is placed in spray dryer again and carries out spray drying 2h, namely prepare a kind of complex microorganism demulsifier。
The complex microorganism demulsifier present invention prepared is added in crude oil, and addition is 4mg/L, is 43 DEG C in temperature, and rotating speed is that under 80r/min, stirring makes it be sufficiently mixed uniformly, stands 4h,。This By Demulsifier is good, and consumption is few, and dehydration rate is higher than other products 20.9%, and dewatering speed is fast, is worthy to be popularized and use。
Example 3
First counting by weight, choose 30 parts of agar, 10 parts of glycerol, 10 parts of glucoses, 15 parts of peptones and 35 parts of water, under 160r/min, stirring mixing, is placed in shaking table oscillation treatment 60min, prepares culture fluid;Then from 20m under earth's surface, oil field, taking 2kg bed mud and put in culture dish, by bed mud and culture fluid solid-to-liquid ratio 2:1, be added in bed mud by culture fluid, controlling temperature is 24 DEG C, cultivates 5 days, changes a culture fluid every 16h, obtains mixture;Putting in fermentation tank by the mixture of above-mentioned gained, be added to the glycine betaine of mixture quality 5% simultaneously, controlling fermentation temperature is 35 DEG C, sealing and fermenting 5 days, is subsequently placed in 3000r/min centrifuge centrifugation 15min, obtains fermentation liquid;Weigh 0.7kg soybean stalk, rinse 3 times with clear water, it is placed in ventilation natural air drying, put into after air-dry in pulverizer and be ground into the stalk fibre that length is 2cm, stalk fibre is added in the fermentation liquid of above-mentioned gained, it is added to 50mL dichloroethanes and 30mL diisopropyl phosphite simultaneously respectively, 500W ultrasonic dispersers carries out ultrasonic disperse and processes 50min;Finally after ultrasonic disperse processes, the stalk fibre mixture of gained will add 50mL glycol monoethyl ether, it is placed at 38 DEG C and is incubated 6h, after being incubated, being added to 30g sodium alginate, stirring makes it be sufficiently mixed uniformly, is placed in 550W ultrasonic dispersers ultrasonic disperse process 40min, it is placed in spray dryer again and carries out spray drying 2h, namely prepare a kind of complex microorganism demulsifier。
The complex microorganism demulsifier present invention prepared is added in crude oil, and addition is 5mg/L, is 45 DEG C in temperature, and rotating speed is that under 80r/min, stirring makes it be sufficiently mixed uniformly, stands 5h,。This By Demulsifier is good, and consumption is few, and dehydration rate is higher than other products 21.1%, and dewatering speed is fast, is worthy to be popularized and use。

Claims (1)

1. the preparation method of a complex microorganism demulsifier, it is characterised in that concrete preparation process is:
(1) counting by weight, choose 15~30 parts of agar, 5~10 parts of glycerol, 5~10 parts of glucoses, 10~15 parts of peptones and 35~65 parts of water, under 160r/min, stirring mixing, is placed in shaking table oscillation treatment 50~60min, prepares culture fluid;
(2) from 10~20m under earth's surface, oil field, take 1~2kg bed mud and put in culture dish, by bed mud and culture fluid solid-to-liquid ratio 2:1, being added in bed mud by culture fluid, controlling temperature is 20~24 DEG C, cultivates 3~5 days, change a culture fluid every 10~16h, obtain mixture;
(3) mixture of above-mentioned gained is put in fermentation tank, being added to the glycine betaine of mixture quality 3~5%, controlling fermentation temperature is 28~35 DEG C, sealing and fermenting 3~5 days simultaneously, it is subsequently placed in 3000r/min centrifuge centrifugation 10~15min, obtains fermentation liquid;
(4) 0.5~0.7kg soybean stalk is weighed, rinse 2~3 times with clear water, it is placed in ventilation natural air drying, put into after air-dry in pulverizer and be ground into the stalk fibre that length is 1~2cm, stalk fibre is added in the fermentation liquid of above-mentioned gained, it is added to 30~50mL dichloroethanes and 20~30mL diisopropyl phosphite simultaneously respectively, 300~500W ultrasonic dispersers carries out ultrasonic disperse and processes 30~50min;
(5) after ultrasonic disperse processes, the stalk fibre mixture of gained will add 30~50mL glycol monoethyl ether, it is placed at 30~38 DEG C and is incubated 4~6h, after being incubated, being added to 20~30g sodium alginate, stirring makes it be sufficiently mixed uniformly, is placed in 500~550W ultrasonic dispersers ultrasonic disperse process 30~40min, it is placed in spray dryer again and carries out spray drying 1~2h, namely prepare a kind of complex microorganism demulsifier。
CN201610144381.XA 2016-03-15 2016-03-15 Preparation method of compound microorganism demulsifying agent Pending CN105694952A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106244237A (en) * 2016-08-16 2016-12-21 上海贵通新材料科技有限公司 Prevent the preparation method of the burnt antisludging agent of resistance that in petrochemical production process, burnt dirt is formed
CN106566580A (en) * 2016-11-10 2017-04-19 仇颖莹 Preparation method for composite biological oilfield demulsifier

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101434925A (en) * 2008-12-22 2009-05-20 哈尔滨工业大学 Method for separating and screening flocculation and demulsification double-function bacterial strain and culture medium used thereby
CN101724579A (en) * 2008-10-15 2010-06-09 同济大学 Rhodococcus sp., lipopeptid extra-cellular bio-demulsifier, preparation method and application thereof
CN102391847A (en) * 2011-10-07 2012-03-28 李立文 Composite microbe oil displacement agent and use thereof
CN105293717A (en) * 2015-11-04 2016-02-03 高大元 Preparation method of creeper leaves curing water denitrification microorganism preparation
CN105368875A (en) * 2015-12-19 2016-03-02 仇颖超 Method for preparing bio-demulsifier based on rapeseed dreg cultured microorganisms

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101724579A (en) * 2008-10-15 2010-06-09 同济大学 Rhodococcus sp., lipopeptid extra-cellular bio-demulsifier, preparation method and application thereof
CN101434925A (en) * 2008-12-22 2009-05-20 哈尔滨工业大学 Method for separating and screening flocculation and demulsification double-function bacterial strain and culture medium used thereby
CN102391847A (en) * 2011-10-07 2012-03-28 李立文 Composite microbe oil displacement agent and use thereof
CN105293717A (en) * 2015-11-04 2016-02-03 高大元 Preparation method of creeper leaves curing water denitrification microorganism preparation
CN105368875A (en) * 2015-12-19 2016-03-02 仇颖超 Method for preparing bio-demulsifier based on rapeseed dreg cultured microorganisms

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106244237A (en) * 2016-08-16 2016-12-21 上海贵通新材料科技有限公司 Prevent the preparation method of the burnt antisludging agent of resistance that in petrochemical production process, burnt dirt is formed
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

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