CN106719681A - A kind of oil field disinfecting corrosion inhibitor and preparation method thereof - Google Patents
A kind of oil field disinfecting corrosion inhibitor and preparation method thereof Download PDFInfo
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- CN106719681A CN106719681A CN201611026243.8A CN201611026243A CN106719681A CN 106719681 A CN106719681 A CN 106719681A CN 201611026243 A CN201611026243 A CN 201611026243A CN 106719681 A CN106719681 A CN 106719681A
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- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/50—1,3-Diazoles; Hydrogenated 1,3-diazoles
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- 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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/02—Amines; Quaternary ammonium compounds
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- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/10—Aromatic or araliphatic carboxylic acids, or thio analogues thereof; Derivatives thereof
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- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/08—Corrosion inhibition
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Abstract
The invention belongs to chemical sterilization technical field of anticorrosion, a kind of oil field disinfecting corrosion inhibitor and preparation method thereof is disclosed, first mix tertiary amine with Ornidazole, heated up after synthesis under normal pressure；Water-soluble organic amine is added, control temperature continues reaction and obtains disinfecting corrosion inhibitor intermediate A；After intermediate A is diluted with solvent, hexamethylenetetramine, benzoate and disodium ethylene diamine tetraacetate are sequentially added, stirring at normal temperature is uniform, that is, oil field disinfecting corrosion inhibitor is obtained.Not only bactericidal action mechanism is different from bactericide conventional at present for oil field disinfecting corrosion inhibitor of the invention, the resistance to the action of a drug is small, and with chemical feeding quantity it is small, inhibition sterilizing rate is high the features such as, it is highly suitable for the oil field especially bacterial control of offshore oilfield and preservative treatment, its preparation method is relatively simple simultaneously, technological requirement is not high, it is easy to produce in batches.
Description
Technical field
The invention belongs to chemical sterilization technical field of anticorrosion, and in particular to a kind of oil field disinfecting corrosion inhibitor and its preparation side
Method.
Background technology
With the continuous exploitation in oil field, water content constantly rises, and the problem of bacteria breed and corrosion becomes increasingly conspicuous, every year all
Huge economic loss can be caused.Addition bactericide and corrosion inhibiter not only can reach effectively but also economically anti-corrosion and bacterial control
Purpose, therefore, filling bactericide with corrosion inhibiter into domestic many oil gas fields together must row operation.
The corrosion inhibitor product commonly used in current oil field oil water processing procedure have quaternary ammonium salt, amide-type, imidazolines and
Some other organic compound containing N, P, S, also there is a small number of inorganic inhibitors.Consumption maximum is imidazoles in various organic inhibitors
Quinoline class corrosion inhibiter and its derivative.Conventional bactericide product has quaternary ammonium salt, bi-quaternary ammonium salt class, polyquaternary amine salt, quaternary phosphonium salt
Class, aldehydes and some heterocyclic compounds, but due to reasons such as the resistances to the action of a drug, oil field is incrementally increased using the consumption of bactericide.Nitre
Base imidazoles disinfecting corrosion inhibitor not only contains imidazoline ring, with preferable corrosion inhibition, while by the nitro in its molecule,
Amino or the formation for passing through free radical are reduced into oxygen-free environment, are interacted with cell component, cause microorganism dead, from
And play a part of to kill bacterium, to killing anaerobic bacteria excellent effect, such as oil field SRB bacteriums.Ornidazole is after metronidazole, for nitre
Third generation nitro imidazole derivatives after azoles, with more excellent bactericidal property, but either which kind of nitroimidazole, its water
Solubility is minimum, and because offshore oilfield transports inconvenience and the small only a small amount of chemical agent parking space of working space, therefore
So far seldom in oil field especially offshore oilfield popularization and application.
The content of the invention
Based in existing offshore oilfield bacterial control and preservative treatment, disinfecting corrosion inhibitor needs that the resistance to the action of a drug is small, chemical feeding quantity is small,
A kind of sterilized corrosion inhibition rate requirement high, there is provided oil field disinfecting corrosion inhibitor and preparation method thereof, the oil field disinfecting corrosion inhibitor is not only
Bactericidal action mechanism is different from bactericide conventional at present, and the resistance to the action of a drug is small, and with chemical feeding quantity is small, the spy such as inhibition sterilizing rate is high
Point, is highly suitable for the oil field especially bacterial control of offshore oilfield and preservative treatment, while its preparation method is relatively simple, work
Skill is less demanding, it is easy to produce in batches.
In order to solve the above-mentioned technical problem, the present invention is achieved by following technical scheme：
A kind of oil field disinfecting corrosion inhibitor, the pour point depressant for crude oil is obtained by following preparation method：
(1) it is 3 by the amount ratio of material:5-1:1 tertiary amine mixes with Ornidazole, is warming up to 100-130 DEG C, in synthesis under normal pressure
4-9 hours；
(2) it is 1 to add with the amount ratio of the material of Ornidazole:4-1:2 water-soluble organic amine, in 100-130 DEG C, continues
Reaction 2-5 hours, obtains disinfecting corrosion inhibitor intermediate A；
(3) after the disinfecting corrosion inhibitor intermediate A obtained by step (2) is diluted with solvent, A mass 10%- is sequentially added
25% hexamethylenetetramine, the benzoate of A mass 10%-25%, the disodium ethylene diamine tetraacetate of A mass 2.5%-5%,
Stirring at normal temperature is uniform, that is, oil field disinfecting corrosion inhibitor is obtained.
A kind of preparation method of oil field disinfecting corrosion inhibitor, the method is followed the steps below：
(1) it is 3 by the amount ratio of material:5-1:1 tertiary amine mixes with Ornidazole, is warming up to 100-130 DEG C, in synthesis under normal pressure
4-9 hours；
(2) it is 1 to add with the amount ratio of the material of Ornidazole:4-1:2 water-soluble organic amine, in 100-130 DEG C, continues
Reaction 2-5 hours, obtains disinfecting corrosion inhibitor intermediate A；
(3) after the disinfecting corrosion inhibitor intermediate A obtained by step (2) is diluted with solvent, A mass 10%- is sequentially added
25% hexamethylenetetramine, the benzoate of A mass 10%-25%, the disodium ethylene diamine tetraacetate of A mass 2.5%-5%,
Stirring at normal temperature is uniform, that is, oil field disinfecting corrosion inhibitor is obtained.
In above-mentioned oil field disinfecting corrosion inhibitor and preparation method thereof：
The tertiary amine is at least one in 18 tertiary amines, 16 tertiary amines, 14 tertiary amines, dodeca-tertiary amine, triethanolamine.
The water-soluble organic amine is DMF, DMA, diethylenetriamine, triethylene
At least one in tetramine, TEPA, AEEA.
The solvent is water, methyl alcohol, ethanol, ethylene glycol, isopropanol, DMF, N, N- dimethylacetamide
At least one in amine.
The benzoate is Sodium Benzoate or Potassium Benzoate.
The beneficial effects of the invention are as follows：
Not only bactericidal action mechanism is different from bactericide conventional at present for oil field disinfecting corrosion inhibitor of the invention, the resistance to the action of a drug
It is small, offshore oilfield is particularly suitable for, not only realize one multiplex, and usage amount is small, bactericidal property and corrosion inhibition
It is excellent, it is highly suitable for the oil field especially bacterial control of offshore oilfield and preservative treatment, while its preparation method is more simple
Single, technological requirement is not high, it is easy to produce in batches.When disinfecting corrosion inhibitor concentration in oil field of the invention is 30mg/L, for offshore oil
Field various field infected water sample, sterilizing rate is more than 99%, and controllable containing CO2/H2The corrosion of offshore oilfield scene water under S operating modes
Speed is less than 0.076mm/a, and corrosion inhibition rate is more than 90%.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail：
Following examples can make those skilled in the art that the present invention is more completely understood, but limit this never in any form
Invention.
The present invention does not do strict regulations to the multiple of disinfecting corrosion inhibitor intermediate A solvent dilution in step (3), can basis
Practical application request elects, and general recommendations extension rate is at 3-8 times.It is more preferably to contrast practical application in following embodiment
Performance difference, unified 5 times of dilution.The present invention does not also make strict regulations to mixing time in step (3), generally stirring 0.5 hour
Afterwards, product can dissolve uniform.
Embodiment 1：
(1) first by 128.0g (0.6mol) dodeca-tertiary amine, the mixing of 219.6g (1mol) Ornidazole is warming up to 130 DEG C, reaction
4h；
(2) 43.56g (0.5mol) DMA is added, in 120 DEG C, is reacted 5 hours, obtain sterilized slow
Erosion agent intermediate A 1；
(3) after disinfecting corrosion inhibitor intermediate A 1 is diluted with 1565g water (being diluted to 5.00 times), 97.79g is sequentially added
(the 25% of A1 mass) hexamethylenetetramine, 97.79g (the 25% of A1 mass) Potassium Benzoates and 9.779g be (A1 mass
2.5%) disodium ethylene diamine tetraacetate, stirring at normal temperature 0.5h obtains final product oil field disinfecting corrosion inhibitor.
Embodiment 2：
(1) first by the tertiary amines of 238g (0.8mol) 18, the mixing of 219.6g (1mol) Ornidazole is warming up to 120 DEG C, reaction
8h；
(2) 58.5g (0.4mol) triethylene tetramine is added, in 110 DEG C, is reacted 4 hours, obtained in the middle of disinfecting corrosion inhibitor
Body A2；
(3) by the 1000g DMFs of disinfecting corrosion inhibitor intermediate A 2,1065g water (is diluted to 5.00 times)
After dilution, 100g (the 19% of A2 mass) hexamethylenetetramine, 51.61g (the 10% of A2 mass) Sodium Benzoate are sequentially added
With 25.805g (the 5% of A2 mass) disodium ethylene diamine tetraacetate, stirring at normal temperature 0.5h obtains final product oil field disinfecting corrosion inhibitor.
Embodiment 3：
(1) first by 74.594g (0.5mol) triethanolamine, the tertiary amines of 134.755g (0.5mol) 16,219.6g (1mol)
Ornidazole mixes, and is warming up to 120 DEG C, reacts 7h；
(2) 18.931g (0.10mol) TEPA is added, 13.068g (0.15mol) DMA,
In 130 DEG C, react 2 hours, obtain disinfecting corrosion inhibitor intermediate A 3；
(3) by the 500g ethylene glycol of disinfecting corrosion inhibitor intermediate A 3,500gN, N- the dimethylacetylamide, (dilution of 844g water
To 5.00 times) dilution after, sequentially add 60g (the 13% of A3 mass) hexamethylenetetramine, 60g (the 13% of A3 mass) benzene first
Sour sodium and 15g (the 3.25% of A3 mass) disodium ethylene diamine tetraacetate, stirring at normal temperature 0.5h obtain final product oil field disinfecting corrosion inhibitor.
Embodiment 4：
(1) first by 149.188g (1mol) triethanolamine, the mixing of 219.6g (1mol) Ornidazole is warming up to 100 DEG C, reaction
9h；
(2) 31.245g (0.3mol) AEEA is added, in 100 DEG C, is reacted 4 hours, obtain disinfecting corrosion inhibitor
Intermediate A 4；
(3) by the 500g isopropanols of disinfecting corrosion inhibitor intermediate A 4,500g the DMFs, (dilution of 600g water
To 5.00 times) dilution after, sequentially add 60g (the 15% of A4 mass) hexamethylenetetramine, 50g Potassium Benzoates (A4 mass
12.5%) with 15g (the 3.7% of A4 mass) disodium ethylene diamine tetraacetate, stirring at normal temperature 0.5h obtains final product oil field disinfecting corrosion inhibitor.
Embodiment 5：
(1) first by the tertiary amines of 217g (0.9mol) 14, the mixing of 219.6g (1mol) Ornidazole is warming up to 120 DEG C, reaction
5h；
(2) 36.55g (0.5mol) DMA is added, in 120 DEG C, is reacted 4 hours, obtain sterilized slow
Erosion agent intermediate A 5；
(3) by 892 methyl alcohol of disinfecting corrosion inhibitor intermediate A 5, after 1000g water (being diluted to 5.00 times) dilution, then add successively
Enter 47.315g (the 10% of A5 mass) hexamethylenetetramine, 94.63g (the 20% of A5 mass) Sodium Benzoates and 20g (A5 mass
4.2%) disodium ethylene diamine tetraacetate, stirring at normal temperature 0.5h obtains final product oil field disinfecting corrosion inhibitor.
Embodiment 6：
(1) first by 149.38g (0.7mol) dodeca-tertiary amine, the mixing of 219.6g (1mol) Ornidazole is warming up to 120 DEG C, instead
Answer 6h；
(2) 29.24g (0.4mol) DMF is added, 10.317g (0.1mol) diethylenetriamine, in
120 DEG C, react 5 hours, obtain disinfecting corrosion inhibitor intermediate A 6；
(3) by the 400g DMAs of disinfecting corrosion inhibitor intermediate A 6,400g ethanol, 800g water (is diluted to
5.00 times) dilution after, sequentially add 102g (the 25% of A6 mass) hexamethylenetetramine, 100g (the 24.5% of A6 mass) benzene
Sodium formate and 15g (the 3.7% of A6 mass) disodium ethylene diamine tetraacetate, stirring at normal temperature 0.5h obtain final product oil field disinfecting corrosion inhibitor.
Experimental example 1：
Experimental raw：Certain offshore oilfield scene infected water sample, blank SRB bacterial contents are 0.5 × 104Individual/mL
Evaluation method：Dilution-to-extinction method
Experimental temperature：50℃
Test period：168 hours
Drug concentration：30mg/L
Test result is as follows：
The sterilization experiment result of table 1
Experimental example 2：
Experimental raw：Certain offshore oilfield scene infected water sample, blank SRB bacterial contents are 0.5 × 106Individual/mL
Evaluation method：Dilution-to-extinction method
Experimental temperature：60℃
Test period：168 hours
Drug concentration：30mg/L
Test result is as follows：
The sterilization experiment result of table 2
Experimental example 3：
Experimental raw：Certain offshore oilfield scene infected water sample, blank SRB bacterial contents are 0.5 × 105Individual/mL
Evaluation method：Dilution-to-extinction method
Experimental temperature：40℃
Test period：168 hours
Drug concentration：30mg/L
Test result is as follows：
The sterilization experiment result of table 3
Illustrated by experimental example 1-3, the present invention has good inhibition to the SRB bacteriums in the water of offshore oilfield scene, dense
Spend during for 30mg/L, sterilizing rate is more than 99%.
Experimental example 4：
Experimental raw：Certain offshore oilfield scene water
Evaluation method：Indoor 3 liters of C276 steel alloy kettles Dynamic Corrosions experiment
Experiment material：Q235 steel
Experimental temperature：91℃
Velocity of medium：1.0m/s
Experiment gas phase composition：0.2MPaCO2+2.0MPaN2+50ppmH2S
Test period：Laboratory experiment 72 hours
Drug concentration：50mg/L
Test result is as follows：
Dynamic corrosion test 1 in the Room of table 4
Illustrated by experimental example 4, corrosion of the present invention to offshore oilfield scene water has good inhibition, and concentration is
During 50mg/L, can control corrosion rate and be less than 0.076mm/a, corrosion inhibition rate is more than 90%.
Claims (10)
1. a kind of oil field disinfecting corrosion inhibitor, it is characterised in that the pour point depressant for crude oil is obtained by following preparation method：
(1) it is 3 by the amount ratio of material:5-1:1 tertiary amine mixes with Ornidazole, is warming up to 100-130 DEG C, in synthesis under normal pressure 4-9
Hour；
(2) it is 1 to add with the amount ratio of the material of Ornidazole:4-1:2 water-soluble organic amine, in 100-130 DEG C, continues to react
2-5 hours, obtain disinfecting corrosion inhibitor intermediate A；
(3) after the disinfecting corrosion inhibitor intermediate A obtained by step (2) is diluted with solvent, A mass 10%-25% is sequentially added
Hexamethylenetetramine, the benzoate of A mass 10%-25%, the disodium ethylene diamine tetraacetate of A mass 2.5%-5%, normal temperature
Stir, that is, oil field disinfecting corrosion inhibitor is obtained.
2. a kind of oil field disinfecting corrosion inhibitor according to claim 1, it is characterised in that the tertiary amine is 18 tertiary amines, ten
At least one in six tertiary amines, 14 tertiary amines, dodeca-tertiary amine, triethanolamine.
3. a kind of oil field disinfecting corrosion inhibitor according to claim 1, it is characterised in that the water-soluble organic amine is N, N-
Dimethylformamide, in DMA, diethylenetriamine, triethylene tetramine, TEPA, AEEA
At least one.
4. a kind of oil field disinfecting corrosion inhibitor according to claim 1, it is characterised in that the solvent is water, methyl alcohol, second
Alcohol, ethylene glycol, isopropanol, DMF, at least one in DMA.
5. a kind of oil field disinfecting corrosion inhibitor according to claim 1, it is characterised in that the benzoate is Sodium Benzoate
Or Potassium Benzoate.
6. a kind of preparation method of oil field disinfecting corrosion inhibitor, it is characterised in that the method is followed the steps below：
(1) it is 3 by the amount ratio of material:5-1:1 tertiary amine mixes with Ornidazole, is warming up to 100-130 DEG C, in synthesis under normal pressure 4-9
Hour；
(2) it is 1 to add with the amount ratio of the material of Ornidazole:4-1:2 water-soluble organic amine, in 100-130 DEG C, continues to react
2-5 hours, obtain disinfecting corrosion inhibitor intermediate A；
(3) after the disinfecting corrosion inhibitor intermediate A obtained by step (2) is diluted with solvent, A mass 10%-25% is sequentially added
Hexamethylenetetramine, the benzoate of A mass 10%-25%, the disodium ethylene diamine tetraacetate of A mass 2.5%-5%, normal temperature
Stir, that is, oil field disinfecting corrosion inhibitor is obtained.
7. the preparation method of a kind of oil field disinfecting corrosion inhibitor according to claim 6, it is characterised in that the tertiary amine is ten
At least one in eight tertiary amines, 16 tertiary amines, 14 tertiary amines, dodeca-tertiary amine, triethanolamine.
8. the preparation method of a kind of oil field disinfecting corrosion inhibitor according to claim 6, it is characterised in that the water solubility has
Machine amine is DMF, DMA, diethylenetriamine, triethylene tetramine, TEPA, hydroxyl second
At least one in base ethylenediamine.
9. the preparation method of a kind of oil field disinfecting corrosion inhibitor according to claim 6, it is characterised in that the solvent is
Water, methyl alcohol, ethanol, ethylene glycol, isopropanol, DMF, at least one in DMA.
10. a kind of preparation method of oil field disinfecting corrosion inhibitor according to claim 6, it is characterised in that the benzoic acid
Salt is Sodium Benzoate or Potassium Benzoate.
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| CN112646558A (en) * | 2020-12-18 | 2021-04-13 | 成都劳恩普斯科技有限公司 | Ecological safety sterilization corrosion inhibitor special for shale gas pipeline and preparation method thereof |
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| CN112646558A (en) * | 2020-12-18 | 2021-04-13 | 成都劳恩普斯科技有限公司 | Ecological safety sterilization corrosion inhibitor special for shale gas pipeline and preparation method thereof |
| CN112646558B (en) * | 2020-12-18 | 2022-08-16 | 成都劳恩普斯科技有限公司 | Ecological safety sterilization corrosion inhibitor special for shale gas pipeline and preparation method thereof |
| CN114747588A (en) * | 2021-08-26 | 2022-07-15 | 中海油(天津)油田化工有限公司 | Urea bactericide for oil field and preparation method thereof |
| CN114747588B (en) * | 2021-08-26 | 2023-07-28 | 中海油(天津)油田化工有限公司 | Urea bactericide for oil field and preparation method thereof |
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