CN106719681B - 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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- CN106719681B CN106719681B CN201611026243.8A CN201611026243A CN106719681B CN 106719681 B CN106719681 B CN 106719681B CN 201611026243 A CN201611026243 A CN 201611026243A CN 106719681 B CN106719681 B CN 106719681B
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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, is first mixed tertiary amine with Ornidazole, in synthesis under normal pressure after heating；Add water-soluble organic amine, the reaction was continued obtains disinfecting corrosion inhibitor intermediate A for control temperature；After intermediate A is diluted with solvent, hexamethylenetetramine, benzoate and disodium ethylene diamine tetraacetate are sequentially added, stirring at normal temperature is uniform, obtains oil field disinfecting corrosion inhibitor.Not only bactericidal effect mechanism is different from currently used fungicide for oil field disinfecting corrosion inhibitor of the invention, drug resistance is small, and have the characteristics that dosage is small, inhibition sterilizing rate is high, it is highly suitable for the bacterial control and preservative treatment of oil field especially offshore oilfield, preparation method is relatively simple simultaneously, technique is of less demanding, 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 technique
The problem of with the continuous exploitation in oil field, water content constantly rises, bacteria breed and corrosion becomes increasingly conspicuous, every year all
It will cause huge economic loss.Addition fungicide and corrosion inhibiter not only can reach effectively but also economically anti-corrosion and bacterial control
Purpose, therefore, filling fungicide and corrosion inhibiter at domestic many oil gas fields together with must row process.
At present in oil field oil water treatment process common corrosion inhibitor product have quaternary ammonium salt, amides, imidazolines and
Some other organic compound containing N, P, S, also there is a small number of inorganic inhibitors.Dosage maximum is imidazoles in various organic inhibitors
Quinoline class corrosion inhibiter and its derivative.Common fungicide 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 drug resistance etc., oil field is incrementally increased using the dosage of fungicide.Nitre
Base imidazoles disinfecting corrosion inhibitor not only contains imidazoline ring, has preferable corrosion inhibition, while passing through the nitro in its molecule,
It is reduced into amino or the formation by free radical in oxygen-free environment, interacts with cell component, causes microorganism dead, from
And play the role of killing bacterium, to anaerobic bacteria excellent effect is killed, such as oil field SRB bacterium.Ornidazole is after metronidazole, for nitre
Third generation nitro imidazole derivatives after azoles have superior bactericidal property, but either which kind of nitroimidazole, water
Solubility is minimum, and since offshore oilfield transports the small only a small amount of chemical agent parking space of inconvenient and working space,
So far seldom in oil field, especially offshore oilfield is promoted and applied.
Summary of the invention
Based in existing offshore oilfield bacterial control and preservative treatment, disinfecting corrosion inhibitor need drug resistance is small, dosage is small,
The high requirement of corrosion inhibition rate is sterilized, provides a kind of oil field disinfecting corrosion inhibitor and preparation method thereof, the oil field disinfecting corrosion inhibitor is not only
Bactericidal effect mechanism is different from currently used fungicide, and drug resistance is small, and has the spies such as small, the inhibition sterilizing rate height of dosage
Point is highly suitable for the bacterial control and preservative treatment of oil field especially offshore oilfield, while preparation method is relatively simple, work
Skill is of less demanding, is easy to produce in batches.
In order to solve the above-mentioned technical problem, the present invention is achieved by technical solution below:
A kind of oil field disinfecting corrosion inhibitor, the oil field disinfecting corrosion inhibitor are obtained by following preparation method:
(1) tertiary amine that the mass ratio of the material is 3:5-1:1 is mixed with Ornidazole, 100-130 DEG C is warming up to, in synthesis under normal pressure
4-9 hours；
(2) water-soluble organic amine for being 1:4-1:2 with the mass ratio of the material of Ornidazole is added, in 100-130 DEG C, is continued
Reaction 2-5 hours, obtains disinfecting corrosion inhibitor intermediate A；
(3) after diluting the resulting disinfecting corrosion inhibitor intermediate A of step (2) with solvent, A mass 10%- is sequentially added
25% hexamethylenetetramine, the benzoate of A mass 10%-25%, A mass 2.5%-5% disodium ethylene diamine tetraacetate,
Stirring at normal temperature is uniform, obtains oil field disinfecting corrosion inhibitor.
A kind of preparation method of oil field disinfecting corrosion inhibitor, this method follow the steps below:
(1) tertiary amine that the mass ratio of the material is 3:5-1:1 is mixed with Ornidazole, 100-130 DEG C is warming up to, in synthesis under normal pressure
4-9 hours；
(2) water-soluble organic amine for being 1:4-1:2 with the mass ratio of the material of Ornidazole is added, in 100-130 DEG C, is continued
Reaction 2-5 hours, obtains disinfecting corrosion inhibitor intermediate A；
(3) after diluting the resulting disinfecting corrosion inhibitor intermediate A of step (2) with solvent, A mass 10%- is sequentially added
25% hexamethylenetetramine, the benzoate of A mass 10%-25%, A mass 2.5%-5% disodium ethylene diamine tetraacetate,
Stirring at normal temperature is uniform, obtains oil field disinfecting corrosion inhibitor.
In above-mentioned oil field disinfecting corrosion inhibitor and preparation method thereof:
The tertiary amine is at least one of 18 tertiary amines, 16 tertiary amines, 14 tertiary amines, dodeca-tertiary amine, triethanolamine.
The water-soluble organic amine is n,N-Dimethylformamide, n,N-dimethylacetamide, diethylenetriamine, triethylene
At least one of tetramine, tetraethylenepentamine, hydroxyethyl ethylenediamine.
The solvent is water, methanol, ethyl alcohol, ethylene glycol, isopropanol, n,N-Dimethylformamide, N, N- dimethylacetamide
At least one of amine.
The benzoate is sodium benzoate or Potassium Benzoate.
The beneficial effects of the present invention are:
Not only bactericidal effect mechanism is different from currently used fungicide for oil field disinfecting corrosion inhibitor of the invention, drug resistance
It is small, particularly suitable for offshore oilfield, not only realize one multi-purpose, but also usage amount is small, bactericidal property and corrosion inhibition
It is excellent, it is highly suitable for the bacterial control and preservative treatment of oil field especially offshore oilfield, while preparation method is more simple
Single, technique is of less demanding, is easy to produce in batches.When oil field disinfecting corrosion inhibitor concentration of the invention is 30mg/L, for offshore oil
Field various field infected water sample, sterilizing rate are greater than 99%, and controllable containing CO2/H2The corrosion of offshore oilfield scene water under S operating condition
Rate is less than 0.076mm/a, and corrosion inhibition rate is greater than 90%.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail:
Following embodiment can make those skilled in the art that the present invention be more completely understood, but not limit this in any way
Invention.
The present invention does not do strict regulations with the diluted multiple of solvent to disinfecting corrosion inhibitor intermediate A in step (3), can basis
Practical application request elects, and general recommendations extension rate is at 3-8 times.In following embodiment, for more preferable comparison practical application
Performance difference, unified 5 times of dilution.The present invention does not also make strict regulations to mixing time in step (3), usually 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) n,N-dimethylacetamide is added, in 120 DEG C, reacts 5 hours, it is slow to obtain sterilization
Lose agent intermediate A 1；
(3) after diluting disinfecting corrosion inhibitor intermediate A 1 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 Benzoate and 9.779g be (A1 mass
2.5%) disodium ethylene diamine tetraacetate, stirring at normal temperature 0.5h is to get oil field disinfecting corrosion inhibitor.
Embodiment 2:
(1) first by 18 tertiary amine of 238g (0.8mol), 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, reacts 4 hours, obtains among disinfecting corrosion inhibitor
Body A2；
(3) by the 1000g n,N-Dimethylformamide 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 is to get oil field disinfecting corrosion inhibitor.
Embodiment 3:
(1) first by 74.594g (0.5mol) triethanolamine, 16 tertiary amine of 134.755g (0.5mol), 219.6g (1mol)
Ornidazole mixing, is warming up to 120 DEG C, reacts 7h；
(2) 18.931g (0.10mol) tetraethylenepentamine is added, 13.068g (0.15mol) n,N-dimethylacetamide,
In 130 DEG C, reacts 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 dimethyl acetamide, (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 is to get 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) hydroxyethyl ethylenediamine is added, in 100 DEG C, reacts 4 hours, obtains disinfecting corrosion inhibitor
Intermediate A 4；
(3) by the 500g isopropanol of disinfecting corrosion inhibitor intermediate A 4,500g the n,N-Dimethylformamide, (dilution of 600g water
To 5.00 times) dilution after, sequentially add 60g (the 15% of A4 mass) hexamethylenetetramine, 50g Potassium Benzoate (A4 mass
12.5%) with 15g (the 3.7% of A4 mass) disodium ethylene diamine tetraacetate, stirring at normal temperature 0.5h is to get oil field disinfecting corrosion inhibitor.
Embodiment 5:
(1) first by 14 tertiary amine of 217g (0.9mol), the mixing of 219.6g (1mol) Ornidazole is warming up to 120 DEG C, reaction
5h；
(2) 36.55g (0.5mol) n,N-dimethylacetamide is added, in 120 DEG C, reacts 4 hours, it is slow to obtain sterilization
Lose agent intermediate A 5；
(3) by 892 methanol of disinfecting corrosion inhibitor intermediate A 5, after 1000g water (being diluted to 5.00 times) dilution, then successively add
Enter 47.315g (the 10% of A5 mass) hexamethylenetetramine, 94.63g (the 20% of A5 mass) sodium benzoate and 20g (A5 mass
4.2%) disodium ethylene diamine tetraacetate, stirring at normal temperature 0.5h is to get 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) n,N-Dimethylformamide is added, 10.317g (0.1mol) diethylenetriamine, in
It 120 DEG C, reacts 5 hours, obtains disinfecting corrosion inhibitor intermediate A 6；
(3) by the 400g n,N-dimethylacetamide of disinfecting corrosion inhibitor intermediate A 6,400g ethyl alcohol, 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 is to get oil field disinfecting corrosion inhibitor.
Experimental example 1:
Experimental raw: certain offshore oilfield scene infected water sample, blank SRB bacterial content are 0.5 × 104A/mL
Evaluation method: dilution-to-extinction method
Experimental temperature: 50 DEG C
Test period: 168 hours
Drug concentration: 30mg/L
Test result is as follows:
1 sterilization experiment result of table
Experimental example 2:
Experimental raw: certain offshore oilfield scene infected water sample, blank SRB bacterial content are 0.5 × 106A/mL
Evaluation method: dilution-to-extinction method
Experimental temperature: 60 DEG C
Test period: 168 hours
Drug concentration: 30mg/L
Test result is as follows:
2 sterilization experiment result of table
Experimental example 3:
Experimental raw: certain offshore oilfield scene infected water sample, blank SRB bacterial content are 0.5 × 105A/mL
Evaluation method: dilution-to-extinction method
Experimental temperature: 40 DEG C
Test period: 168 hours
Drug concentration: 30mg/L
Test result is as follows:
3 sterilization experiment result of table
Illustrated by experimental example 1-3, the present invention has good inhibitory effect to the SRB bacterium in the water of offshore oilfield scene, dense
When degree is 30mg/L, sterilizing rate is greater than 99%.
Experimental example 4:
Experimental raw: certain offshore oilfield scene water
Evaluation method: indoor 3 liters of C276 steel alloy kettle Dynamic Corrosions experiment
Test material: Q235 steel
Experimental temperature: 91 DEG C
Velocity of medium: 1.0m/s
Test 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 table Room 4
Illustrated by experimental example 4, the present invention has good inhibitory effect to the corrosion of offshore oilfield scene water, and concentration is
When 50mg/L, corrosion rate can control to be less than 0.076mm/a, corrosion inhibition rate is greater than 90%.
Claims (6)
1. a kind of oil field disinfecting corrosion inhibitor, which is characterized in that the oil field disinfecting corrosion inhibitor is obtained by following preparation method:
(1) tertiary amine that the mass ratio of the material is 3:5-1:1 is mixed with Ornidazole, 100-130 DEG C is warming up to, in synthesis under normal pressure 4-9
Hour；
(2) water-soluble organic amine for being 1:4-1:2 with the mass ratio of the material of Ornidazole is added, in 100-130 DEG C, the reaction was continued
2-5 hours, obtain disinfecting corrosion inhibitor intermediate A；
(3) after diluting the resulting disinfecting corrosion inhibitor intermediate A of step (2) with solvent, A mass 10%-25% is sequentially added
Hexamethylenetetramine, the benzoate of A mass 10%-25%, A mass 2.5%-5% disodium ethylene diamine tetraacetate, room temperature
It stirs evenly, obtains oil field disinfecting corrosion inhibitor；
The tertiary amine is at least one of 18 tertiary amines, 16 tertiary amines, 14 tertiary amines, dodeca-tertiary amine, triethanolamine；
The water-soluble organic amine is n,N-Dimethylformamide, n,N-dimethylacetamide, diethylenetriamine, triethylene four
At least one of amine, tetraethylenepentamine, hydroxyethyl ethylenediamine.
2. a kind of oil field disinfecting corrosion inhibitor according to claim 1, which is characterized in that the solvent is water, methanol, second
Alcohol, ethylene glycol, isopropanol, n,N-Dimethylformamide, at least one of n,N-dimethylacetamide.
3. a kind of oil field disinfecting corrosion inhibitor according to claim 1, which is characterized in that the benzoate is sodium benzoate
Or Potassium Benzoate.
4. a kind of preparation method of oil field disinfecting corrosion inhibitor, which is characterized in that this method follows the steps below:
(1) tertiary amine that the mass ratio of the material is 3:5-1:1 is mixed with Ornidazole, 100-130 DEG C is warming up to, in synthesis under normal pressure 4-9
Hour；
(2) water-soluble organic amine for being 1:4-1:2 with the mass ratio of the material of Ornidazole is added, in 100-130 DEG C, the reaction was continued
2-5 hours, obtain disinfecting corrosion inhibitor intermediate A；
(3) after diluting the resulting disinfecting corrosion inhibitor intermediate A of step (2) with solvent, A mass 10%-25% is sequentially added
Hexamethylenetetramine, the benzoate of A mass 10%-25%, A mass 2.5%-5% disodium ethylene diamine tetraacetate, room temperature
It stirs evenly, obtains oil field disinfecting corrosion inhibitor；
The tertiary amine is at least one of 18 tertiary amines, 16 tertiary amines, 14 tertiary amines, dodeca-tertiary amine, triethanolamine；
The water-soluble organic amine is n,N-Dimethylformamide, n,N-dimethylacetamide, diethylenetriamine, triethylene four
At least one of amine, tetraethylenepentamine, hydroxyethyl ethylenediamine.
5. a kind of preparation method of oil field disinfecting corrosion inhibitor according to claim 4, which is characterized in that the solvent is
Water, methanol, ethyl alcohol, ethylene glycol, isopropanol, n,N-Dimethylformamide, at least one of n,N-dimethylacetamide.
6. a kind of preparation method of oil field disinfecting corrosion inhibitor according to claim 4, which is characterized in that the benzoate
For sodium benzoate or Potassium Benzoate.
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| CN109502774A (en) * | 2018-08-17 | 2019-03-22 | 滨州市丰泰技术开发有限公司 | A kind of manufacturing method of oil field composite multi-functional fungicide |
| CN109052676A (en) * | 2018-09-05 | 2018-12-21 | 石家庄长宏能源科技有限公司 | A kind of oil field reinjection water water treatment agent 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 |
| 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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