CN109232325A - A kind of fungicide and preparation method for disposing polluted water in oil - Google Patents
A kind of fungicide and preparation method for disposing polluted water in oil Download PDFInfo
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- CN109232325A CN109232325A CN201811246165.1A CN201811246165A CN109232325A CN 109232325 A CN109232325 A CN 109232325A CN 201811246165 A CN201811246165 A CN 201811246165A CN 109232325 A CN109232325 A CN 109232325A
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- fungicide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C277/00—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C277/08—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of substituted guanidines
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
- A01N47/42—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=CX2 groups, e.g. isothiourea
- A01N47/44—Guanidine; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C279/00—Derivatives of guanidine, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C279/04—Derivatives of guanidine, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups having nitrogen atoms of guanidine groups bound to acyclic carbon atoms of a carbon skeleton
- C07C279/12—Derivatives of guanidine, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups having nitrogen atoms of guanidine groups bound to acyclic carbon atoms of a carbon skeleton being further substituted by nitrogen atoms not being part of nitro or nitroso groups
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
- Plant Pathology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to disposing polluted water in oil technical fields, more particularly to a kind of fungicide and preparation method for disposing polluted water in oil, the fungicide generates intermediate by fatty acid, polyethylene polyamine amidation, and then intermediate is further reacted with guanidine hydrochloride, obtains final fungicide.The fatty acid, polyethylene polyamine, guanidine hydrochloride, p-methyl benzenesulfonic acid molar ratio be 1:1.0~1.05:1.0~1.05:0.02~0.05.The raw material of fungicide of the invention is easy to get, and synthetic method is simple, at low cost, and yield is high, is greater than 92%, and bactericidal effect is good, and sterilizing rate is greater than 99.0%.Therefore, present invention is generally applicable in the sterilization processing technique of oilfield sewage.
Description
Technical field
The present invention relates to disposing polluted water in oil technical fields, and in particular to a kind of fungicide for disposing polluted water in oil
And preparation method.
Background technique
Often contain a large amount of bacterium in oilfield sewage system, such as sulfate reducing bacteria, saprophytic bacteria, iron bacteria, sulfur bacteria, mould
Bacterium etc., wherein endangering maximum bacterium to oil field is sulfate reducing bacteria, saprophytic bacteria and iron bacteria.Control bacterial reproduction is can not
Missing link is such as dealt with improperly, and the bacterium meeting mass propagation in produced-water reinjection system causes water quality corrosion rate to increase, is outstanding
The consequence that floating object raising etc. deteriorates along journey, water quality deterioration will cause impurities in water blocking formation pore behind produced-water reinjection stratum, from
And reduce water injection capacity and oil well output.
Currently, the method for oil field control bacterium can be divided into physical method and chemical method two major classes.Physical method has ultraviolet
The methods of line irradiation, plasma method, ultrasonic sterilization.Chemical method has change media environment, adds the methods of fungicide.Physics
Method sterilization is consumed energy the disadvantages of big there are operating cost height, the less use in actual job.The method for adding fungicide has
It is economical, conveniently, it is quick the features such as, therefore in China's oil industry production actual motion, be used as main processing hand always
Section.Common fungicide such as tertiary amine, diamines etc., this kind of fungicide price is high, and is used for a long time and is easy to produce drug resistance, causes
Dosage rises year by year.
Summary of the invention
The present invention is directed to the deficiency of currently available technology and provides a kind of fungicide and its system for disposing polluted water in oil
The raw material of Preparation Method, the fungicide is easy to get, and synthetic method is simple, at low cost, and yield is high, is greater than 92%, and bactericidal effect is good, sterilization
Rate is greater than 99.0%.Therefore, present invention is generally applicable in the sterilization processing technique of oilfield sewage.
The purpose of the present invention is to provide a kind of fungicide for disposing polluted water in oil, the fungicide be by fatty acid,
Polyethylene polyamine amidation generates intermediate, and then intermediate is further reacted to form and be obtained with guanidine hydrochloride.
The molecular formula of the fungicide is as follows:
Wherein: R CmH2m+1, m=10~17；
N=2~4, preferably 3.
It is described it is another object of the present invention to provide a kind of preparation method of fungicide for disposing polluted water in oil
Preparation method specifically includes the following steps:
(1) fatty acid and polyethylene polyamine are weighed in four-hole boiling flask, turn on agitator, stirring rate be 300~
500rpm is then slowly added into catalyst p-methyl benzenesulfonic acid, stirs 10~20min, is then to slowly warm up to 150~160 DEG C, instead
2~3h is answered, intermediate is obtained；
(2) guanidine hydrochloride is added in intermediate while stirring, stirring rate be 300~500rpm, keep temperature 150~
160 DEG C, temperature risen to 170~180 DEG C after reacting 3~4h, 1~2h of isothermal reaction obtains crude product；
(3) above-mentioned crude product with water is diluted to the solution that mass concentration is 40~60% to get fungicide is arrived.
Preferably, the fatty acid, polyethylene polyamine, guanidine hydrochloride, p-methyl benzenesulfonic acid molar ratio be 1:1.0~
1.05:1.0~1.05:0.02~0.05, preferably 1:1.0:1.0:0.03.
Preferably, the fatty acid is capric acid, hendecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, pentadecane
One of acid, hexadecanoic acid, Heptadecanoic acide；The polyethylene polyamine is triethylene tetramine, tetraethylenepentamine and five ethylene
One of hexamine.
The reaction equation is as follows:
Wherein: n=2~4；R is CmH2m+1, m=10~17
The present invention synthesizes double sun for disposing polluted water in oil using fatty acid, polyethylene polyamine and guanidine hydrochloride as host agent
Ionic species fungicide, the fungicide charge density is high, and coverage rate is high, good with oilfield sewage compatibility；Sterilization of the invention simultaneously
Agent raw material is easy to get, and synthetic method is simple, at low cost, and yield is high, is greater than 95%, and bactericidal effect is good, and sterilizing rate is greater than 99.0%, now
Field test effect is good.Therefore, present invention is generally applicable in the sterilization processing technique of oilfield sewage.
The present invention is had the following advantages and beneficial effects: compared with prior art
(1) raw material sources of fungicide of the invention are extensive, synthesis technology is simple, and yield is high, reach 95% or more；
(2) the characteristics of fungicide of the invention has at low cost, Small side effects, adaptable, non-environmental-pollution, can meet
The needs of oil field development；
(3) fungicide of the invention has the characteristics that yield and sterilizing rate are high, and yield is greater than 95%, and sterilizing rate reaches 99%
More than.
Specific embodiment
The present invention is described in further detail below with reference to specific embodiment, and referring to data.It should be understood that these embodiments
It is of the invention solely for the purpose of illustration, rather than limit the scope of the invention in any way.
Embodiment 1:
(1) capric acid and triethylene tetramine are weighed in four-hole boiling flask, turn on agitator, stirring rate 300rpm, then
It is slowly added to catalyst p-methyl benzenesulfonic acid, stirs 10min, is then to slowly warm up to 150 DEG C, 2h is reacted, obtains intermediate；
(2) guanidine hydrochloride is added in intermediate, stirring rate 300rpm while stirring, is kept for 150 DEG C of temperature, reaction
Temperature is risen to 170 DEG C after 3h, isothermal reaction 1h obtains crude product；
(3) above-mentioned crude product with water is diluted to the solution that mass concentration is 40% to get fungicide L is arrived1, yield is
95.8%, molecular formula is as follows:
Wherein, R C10H21。
The capric acid, triethylene tetramine, guanidine hydrochloride and p-methyl benzenesulfonic acid molar ratio be 1:1.02:1.03:0.02.
Embodiment 2:
(1) tridecanoic acid and tetraethylenepentamine are weighed in four-hole boiling flask, turn on agitator, stirring rate 400rpm,
It is then slowly added into catalyst p-methyl benzenesulfonic acid, stirs 15min, is then to slowly warm up to 155 DEG C, 2.5h is reacted, obtains centre
Body；
(2) guanidine hydrochloride is added in intermediate, stirring rate 400rpm while stirring, is kept for 152 DEG C of temperature, reaction
Temperature is risen to 176 DEG C after 3h, isothermal reaction 2h obtains crude product；
(3) above-mentioned crude product with water is diluted to the solution that mass concentration is 50% to get fungicide L is arrived2, yield is
98.5%, molecular formula is as follows:
Wherein, R C13H27。
The tridecanoic acid, tetraethylenepentamine, the molar ratio of guanidine hydrochloride and p-methyl benzenesulfonic acid are 1:1.0:1.0:0.03.
Embodiment 3:
(1) Heptadecanoic acide and pentaethylene hexamine are weighed in four-hole boiling flask, turn on agitator, stirring rate 500rpm,
It is then slowly added into catalyst p-methyl benzenesulfonic acid, stirs 20min, is then to slowly warm up to 160 DEG C, 3h is reacted, obtains intermediate；
(2) guanidine hydrochloride is added in intermediate, stirring rate 500rpm while stirring, is kept for 160 DEG C of temperature, reaction
Temperature is risen to 180 DEG C after 4h, isothermal reaction 2h obtains crude product；
(3) above-mentioned crude product with water is diluted to the solution that mass concentration is 60% to get fungicide L is arrived3, yield is
97.0%, molecular formula is as follows:
Wherein, R C17H35。
The Heptadecanoic acide, pentaethylene hexamine, guanidine hydrochloride and p-methyl benzenesulfonic acid molar ratio be 1:1.05:1.05:
0.05。
The experiment of 4 Lab-evaluation of embodiment
Take Shengli Oil Field multi-purpose station A5Sewage, SRB (sulfate reducing bacteria) content 2 × 10 in sewage4A/mL, adds
The concentration of fungicide is 50mg/L in sewage after fungicide, according to the oil field produced water process of standard Q/SH10200688-2013
Evaluation of Germicidal Efficacy has been carried out to fungicide of the invention with fungicide general technical specifications, the results are shown in Table 1.
As it can be seen from table 1 fungicide L1、L2And L3Handle Shengli Oil Field multi-purpose station A5The sterilizing rate of sewage is respectively
99.50%, 99.75% and 99.25%, sterilizing rate is all larger than 99.0%, and bactericidal effect is good.
1 fungicide M of table1、M2And M3Handle the sterilizing rate of sewage
| Serial number | Fungicide | After processing, a/ml | Sterilizing rate, % |
| 1 | L1 | 100 | 99.50 |
| 2 | L2 | 50 | 99.75 |
| 3 | L3 | 150 | 99.25 |
5 fungicide L of embodiment1Field application
Shengli Oil Field multi-purpose station B2The sewage of processing is sewage after the water-oil separating of water drive Produced Liquid, and day output is
1500m3/ d, SRB (sulfate reducing bacteria) content 5 × 10 in sewage4A/mL adds fungicide L1Fungicide in sewage afterwards
Concentration is 50mg/L, and day dosage is 75kg, and SRB (sulfate reducing bacteria) content is 150/mL after processing, and sterilizing rate is
99.7%, fungicide L1Field test bactericidal effect it is good.
6 fungicide L of embodiment2Field application
Shengli Oil Field multi-purpose station B5The sewage of processing is sewage after the water-oil separating of water drive Produced Liquid, and day output is
1000m3/ d, SRB (sulfate reducing bacteria) content 2 × 10 in sewage4A/mL, fungicide is dense in the sewage after adding fungicide
Degree is 50mg/L, and day dosage is 50kg, and SRB (sulfate reducing bacteria) content is 50/mL after processing, and sterilizing rate is
99.75%, fungicide L2Field test bactericidal effect it is good.
7 fungicide L of embodiment3Field application
Shengli Oil Field multi-purpose station B15The sewage of processing is sewage after the water-oil separating of water drive Produced Liquid, and day output is
1200m3/ d, SRB (sulfate reducing bacteria) content 3 × 10 in sewage4A/mL, fungicide is dense in the sewage after adding fungicide
Degree is 50mg/L, and day dosage is 60kg, and SRB (sulfate reducing bacteria) content is 100/mL after processing, and sterilizing rate is
99.67%, fungicide L3Field test bactericidal effect it is good.
Claims (7)
1. a kind of fungicide for disposing polluted water in oil, which is characterized in that the molecular formula of the fungicide is as follows:
Wherein: R CmH2m+1, m=10~17；
N=2~4.
2. the fungicide according to claim 1 for disposing polluted water in oil, which is characterized in that point of the fungicide
Minor is as follows:
Wherein: R CmH2m+1, m=10~17；
N=3.
3. the preparation method of the fungicide according to claim 1 for disposing polluted water in oil, which is characterized in that described
Preparation method specifically includes the following steps:
(1) fatty acid and polyethylene polyamine are weighed in four-hole boiling flask, turn on agitator, stirring rate is 300~500rpm, so
After be slowly added to catalyst p-methyl benzenesulfonic acid, stir 10~20min, be then to slowly warm up to 150~160 DEG C, react 2~3h,
Obtain intermediate；
(2) guanidine hydrochloride is added in intermediate while stirring, stirring rate is 300~500rpm, keeps temperature 150~160
DEG C, temperature is risen to 170~180 DEG C after 3~4h of reaction, 1~2h of isothermal reaction obtains crude product；
(3) above-mentioned crude product with water is diluted to the solution that mass concentration is 40~60% to get fungicide of the invention is arrived.
4. the preparation method of the fungicide according to claim 3 for disposing polluted water in oil, it is characterised in that described
Fatty acid, polyethylene polyamine, guanidine hydrochloride, p-methyl benzenesulfonic acid molar ratio be 1:1.0~1.05:1.0~1.05:0.02~
0.05。
5. the preparation method of the fungicide according to claim 4 for disposing polluted water in oil, it is characterised in that described
Fatty acid, polyethylene polyamine, guanidine hydrochloride, p-methyl benzenesulfonic acid molar ratio be 1:1.0:1.0:0.03.
6. the preparation method of the fungicide according to claim 3 for disposing polluted water in oil, which is characterized in that its feature
Be the fatty acid be capric acid, hendecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid,
One of Heptadecanoic acide.
7. the preparation method of the fungicide according to claim 3 for disposing polluted water in oil, which is characterized in that its feature
It is that the polyethylene polyamine is one of triethylene tetramine, tetraethylenepentamine and pentaethylene hexamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811246165.1A CN109232325B (en) | 2018-10-24 | 2018-10-24 | Bactericide for oilfield sewage treatment and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811246165.1A CN109232325B (en) | 2018-10-24 | 2018-10-24 | Bactericide for oilfield sewage treatment and preparation method thereof |
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| CN109232325A true CN109232325A (en) | 2019-01-18 |
| CN109232325B CN109232325B (en) | 2021-04-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112080002A (en) * | 2020-08-21 | 2020-12-15 | 天津正达科技有限责任公司 | Water-soluble corrosion-inhibition and sterilization integrated agent and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1350022A (en) * | 2000-10-19 | 2002-05-22 | 上海塑杰科技有限公司 | Polyamine-guanidine salt polymer and its prepn |
| CN101955441A (en) * | 2010-04-06 | 2011-01-26 | 孙安顺 | Preparation method and application of fatty amide polyethylene polyamine amino acid for tertiary oil recovery |
-
2018
- 2018-10-24 CN CN201811246165.1A patent/CN109232325B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1350022A (en) * | 2000-10-19 | 2002-05-22 | 上海塑杰科技有限公司 | Polyamine-guanidine salt polymer and its prepn |
| CN101955441A (en) * | 2010-04-06 | 2011-01-26 | 孙安顺 | Preparation method and application of fatty amide polyethylene polyamine amino acid for tertiary oil recovery |
Non-Patent Citations (3)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112080002A (en) * | 2020-08-21 | 2020-12-15 | 天津正达科技有限责任公司 | Water-soluble corrosion-inhibition and sterilization integrated agent and preparation method thereof |
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