CN102533237B - Preparation method of novel organic amine adsorbed film type corrosion inhibitor for oil field - Google Patents
Preparation method of novel organic amine adsorbed film type corrosion inhibitor for oil field Download PDFInfo
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- CN102533237B CN102533237B CN201210010433.6A CN201210010433A CN102533237B CN 102533237 B CN102533237 B CN 102533237B CN 201210010433 A CN201210010433 A CN 201210010433A CN 102533237 B CN102533237 B CN 102533237B
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Abstract
The invention discloses a preparation method of a novel organic amine adsorbed film type corrosion inhibitor for an oil field. The preparation method comprises the following steps of: carrying out condensation reaction on mixed fatty acid and polyethylene polyamine reagents in the presence of a catalyst under microwave refluxing, and then reacting the reaction product with an iodinated product of ethylene glycol monobutyl ether (or diethylene glycol butyl ether) to obtain a novel organic amine mixture. According to the invention, the obtained novel organic amine compound has the characteristics of excellent water solubility, low use amount and high corrosion inhibition efficiency; a microwave heating device is used for heating and the catalyst is added, thus the condensation reaction time is shortened, required reaction conditions are reduced, and the reaction yield is increased; and a recovering device is arranged, thus excessive reaction reagents can be recycled and the cost is saved.
Description
Technical field
The present invention relates to oil-field development field, be specifically related to a kind of preparation method of novel organic amine adsorbed film type corrosion inhibitor for oil field.
Background technology
At present, the exploitation in China oil field, mainly adopts water flood recover petroleum.Underground by a large amount of water is injected, then from underground, crude oil is being extracted out together with water.No matter the water injecting is to be water outlet or supplementary fresh water from oil field, all need strictly to process, reach the requirement of oil-field flooding standard.Owing to containing the materials such as dissolved oxygen, carbonic acid gas, salt, sulfide, grease, mushroom in the water of oil field, and water temperature is higher, and metallic conduit and the relevant device carried are had to very large corrodibility.Therefore transport pipe and equipment are taked to anticorrosive measure, be the problem that domestic and international each oil field is paid special attention to and studied always.
In many anticorrosive measures; except large-scale line equipment employing erosion shield, lining, sacrifice sun level, cathode protection and anti-corrosion material are manufactured; but topmost measure is to use inhibiter to carry out inhibition processing to oilfield injection water, and whole system is protected.Injected water inhibiter is the chemical agent that a class can reduce injected water erosion rate.This class chemical agent is of a great variety, by corrosion Inhibition Mechanism, can be divided into following three classes:
(1) type oxide film inhibiter: this class inhibiter is to produce fine and close protective membrane by oxidation to play corrosion inhibition;
(2) precipitation membranous type inhibiter, this class inhibiter is to play corrosion inhibition by forming precipitation membrane on the anode at corrosion cell and cathode surface;
(3) absorption membranous type inhibiter, this class inhibiter is to play corrosion inhibition by forming adsorption film on the anode surface at corrosion cell and negative electrode.
At present, on oil field, application mostly is adsorption film type inhibiter, and absorption membranous type inhibiter is all organic compound.Why they can play corrosion inhibition is because have the hydrophilic radical that can be adsorbed on metallic surface and the hydrophobic grouping that covers metallic surface in its molecular structure.Hydrophilic radical is directionally adsorbed on metallic surface, and hydrophobic grouping hinders water and dissolved oxygen to metal diffusing, thereby reaches the effect of inhibition.When metallic surface is active and clean, absorption membranous type inhibiter forms satisfied adsorption film and shows good corrosion protection result.If but in metallic surface, have corrosion product lid or have dirt deposition thing, just can not provide suitable condition to adsorb membranous type corrosion protection film to form.So this class inhibiter is in use, can add wetting agent, with the metallic surface infiltration that helps inhibiter to cover to iron rust. improve corrosion mitigating effect.
Novel organic amine inhibiter of the present invention is the one in absorption membranous type inhibiter, uses microwave heating, has both shortened the process time, has improved again quality product.The most of imidazoline and its derivative that uses of current absorption membranous type inhibiter, its synthetic method mainly contains solvent method and vacuum method.Solvent method needs temperature of reaction low, and product just undergoes no deterioration, but temperature is low, the water generating in reaction is unsuitable separated, affects reaction process, if excess Temperature, reaction product again can be oxidized, and adopt aquifer yield and product acid number to judge that the needed time of reaction terminating point is long, and yield is low; Although vacuum method does not need to consider the recovery problem of solvent, the reaction times is shorter, and raw material is easy to be pumped, and is difficult to adjust the relation of temperature and pressure.The target product making in all preparation methods both domestic and external is in addition single, and the use range in reality is narrow.
Summary of the invention
The object of this invention is to provide a kind of preparation method of novel organic amine adsorbed film type corrosion inhibitor for oil field, its product making is lipid acid, polyethylene polyamine, the synthetic mixture of butyl glycol ether (or Diethylene Glycol butyl ether) iodo product, its productive rate is high, and the use range that makes product is extensive.
For achieving the above object, the present invention has adopted following technical scheme: the preparation method of novel organic amine absorption membranous type inhibiter for a kind of oil field, is characterized in that: comprise the following steps,
S1: under the effect of catalyzer, microwave refluxes and carries out condensation reaction by mixed fatty acid and polyethylene polyamine;
S2: the mixture in S1 is mixed and carries out condensation reaction with butyl glycol ether (or Diethylene Glycol butyl ether) iodo product;
Microwave reflux described in S1 comprises the reactor that microwave heating installation and Qi Nei arrange, and is provided with in addition solvent recovery unit, and the vacuum pump arranging on microwave heating installation is connected between reactor and solvent recovery unit.
Before S1 reaction is carried out, first reaction raw materials and catalyzer are added in reactor, after reactor is evacuated, keep vacuumizing, start the switch of microwave heating installation and solvent recovery unit, set temperature of reaction and carry out condensation reaction.
By mixing S1, have different rust inhibitions from the novel organic amine product S that S2 carries out condensation, this novel organic amine product S can be to H
2s, CO
2play corrosion inhibition with the simultaneous oil of water, gas well and pipeline, can prevent that settling from sticking on metallic surface.By the novel organic amine mixture of preparing, the range of application of the absorption membranous type inhibiter finished product making is improved greatly.Utilize in addition microwave heating installation to heat the time, the required condition of reduction reaction, the raising reaction yield that greatly shorten condensation reaction with the use of catalyzer.Setting up of retrieving arrangement can make unnecessary reaction reagent be recycled, and saves the cost of reaction.
Further scheme is:
The preparation method of organic amine absorption membranous type inhibiter for described oil field, is characterized in that: described catalyzer is Sn or Zn.
The preparation method of organic amine absorption membranous type inhibiter for described oil field, is characterized in that: described mixed fatty acid is the composite synthetic mixture of reagent at least two or more in lauric acid, TETRADECONIC ACID, octadecyl lipid acid.
The preparation method of organic amine absorption membranous type inhibiter for described oil field, is characterized in that: described butyl glycol ether (or Diethylene Glycol butyl ether) the iodo product iodo product that to be ethylene glycol (or Diethylene Glycol butyl ether) make with iodine and phosphorus back flow reaction.
The preparation method of organic amine absorption membranous type inhibiter for described oil field, is characterized in that: the polyethylene polyamine described in S1 is the composite synthetic mixture of reagent at least two or more in diethylenetriamine, triethylene tetramine, tetraethylene pentamine.
The preparation method of organic amine absorption membranous type inhibiter for described oil field, is characterized in that: the described vacuum tightness vacuumizing is 0.1-0.001Mpa.
The preparation method of organic amine absorption membranous type inhibiter for described oil field, is characterized in that: described microwave design temperature is 140-200 ℃.
Embodiment
By specific embodiment, illustrate below:
Embodiment 1:
The reactor arranging in microwave vacuum drying case is connected with pipeline with vacuum pump and solvent recovery unit, to reactor, add mixed fatty acid and the triethylene tetramine of lauric acid and TETRADECONIC ACID, both mol ratios are 2: 1, adding a small amount of catalyst Z n in reactor, reactor is evacuated, vacuum tightness is 0.1Mpa, maintenance vacuumizes, start the switch of microwave drier and solvent recovery unit, set 140-160 ℃ of temperature of reaction and carry out condensation reaction, after reaction finishes, cancel and vacuumize, in reactor, add butyl glycol ether iodo product, and add 20% water and react at 90-100 ℃, obtain yield and be 95% corrosion inhibitor product.
Embodiment 2:
The reactor arranging in microwave vacuum drying case is connected with pipeline with vacuum pump and solvent recovery unit, to reactor, add palmitic acid and stearic mixed fatty acid and diethylenetriamine, both mol ratios are 2: 1, adding a small amount of catalyst Z n in reactor, reactor is evacuated, vacuum tightness is 0.1Mpa, maintenance vacuumizes, start the switch of microwave drier and solvent recovery unit, set 140-160 ℃ of temperature of reaction and carry out condensation reaction, after reaction finishes, cancel and vacuumize, in reactor, add Diethylene Glycol butyl ether iodo product, and add 20% water and react at 80-90 ℃, obtain yield and be 94% corrosion inhibitor product.
Embodiment: product is carried out to corrosion inhibition rate test:
(1) measure and undertaken by SY/T5273-2000;
(2) probe temperature: 65 ℃;
(3) test period: 72H;
(4) the data of water quality preparation Simulated Water that water quality provides by certain oil field.
Result is as follows:
| Addition (ppm) | Average corrosion rate (mm/a) | Corrosion inhibition rate (%) |
| 0 (blank) | 0.278 | --- |
| 4 | 0.05591 | 79.9 |
| 6 | 0.04733 | 82.9 |
| 8 | 0.03985 | 85.6 |
| 10 | 0.03543 | 87.2 |
By above data, can find out, corrosion inhibitor product addition provided by the present invention is when 10ppm, and average inhibition speed can drop to 0.03543mm/a, and corrosion inhibition rate is up to 87.2%.
This product effect and benefit is compared with prior art:
(1) with microwave heating, shorten the reaction times, improved quality product.
(2) inhibition efficiency of products obtained therefrom is high.
(3) the water-soluble spy of products obtained therefrom is good.
Claims (7)
1. a preparation method for novel organic amine adsorbed film type corrosion inhibitor for oil field, is characterized in that: comprises the following steps,
S1: under the effect of catalyzer, microwave refluxes and carries out condensation reaction by mixed fatty acid and polyethylene polyamine;
S2: the reaction product of lipid acid and polyethylene polyamine is reacted with butyl glycol ether iodo product or Diethylene Glycol butyl ether iodo product again;
Microwave reflux described in S1 comprises the reactor that microwave heating installation and Qi Nei arrange, and is provided with in addition solvent recovery unit, and the vacuum pump arranging on microwave heating installation is connected between reactor and solvent recovery unit;
Before S1 reaction is carried out, first reaction raw materials and catalyzer are added in reactor, after reactor is evacuated, keep vacuumizing, start the switch of microwave heating installation and solvent recovery unit, set temperature of reaction and carry out condensation reaction.
2. the preparation method of novel organic amine absorption membranous type inhibiter for oil field as claimed in claim 1, is characterized in that: described catalyzer is Sn or Zn.
3. the preparation method of novel organic amine absorption membranous type inhibiter for oil field as claimed in claim 1, is characterized in that: described mixed fatty acid is the mixture that in lauric acid, TETRADECONIC ACID, octadecyl lipid acid, at least two or more reagent fits in.
4. polyethylene polyamine as claimed in claim 1 is the mixture that reagent at least two or more in diethylenetriamine, triethylene tetramine, tetraethylene pentamine fits in.
5. the preparation method of novel organic amine absorption membranous type inhibiter for oil field as claimed in claim 1, is characterized in that: described butyl glycol ether iodo product or Diethylene Glycol butyl ether iodo product are the iodo product that ethylene glycol or Diethylene Glycol butyl ether and iodine and phosphorus back flow reaction make.
6. the preparation method of novel organic amine absorption membranous type inhibiter for oil field as claimed in claim 1, is characterized in that: the described vacuum tightness vacuumizing is 0.1-0.001Mpa.
7. the preparation method of novel organic amine absorption membranous type inhibiter for oil field as claimed in claim 1, is characterized in that: described microwave design temperature is 140 ℃-200 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182410A (en) * | 2007-11-22 | 2008-05-21 | 张煜 | Oil field inhibitor |
| CN101608310A (en) * | 2008-06-16 | 2009-12-23 | 南京科润工业介质有限公司 | Long-acting emulsion-type antirust fluid |
| CN101760188A (en) * | 2009-12-31 | 2010-06-30 | 山东德仕化工集团有限公司 | Formula of DSS-1 corrosion inhibiter and processing technique |
| CN102020978A (en) * | 2010-12-22 | 2011-04-20 | 夹江县龙兴投资有限公司 | Gas well corrosion inhibitor and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US8250931B2 (en) * | 2008-03-28 | 2012-08-28 | Global Process Technologies, Inc. | Methods and compositions for inhibiting corrosion in non-aqueous, non-conductive liquids |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182410A (en) * | 2007-11-22 | 2008-05-21 | 张煜 | Oil field inhibitor |
| CN101608310A (en) * | 2008-06-16 | 2009-12-23 | 南京科润工业介质有限公司 | Long-acting emulsion-type antirust fluid |
| CN101760188A (en) * | 2009-12-31 | 2010-06-30 | 山东德仕化工集团有限公司 | Formula of DSS-1 corrosion inhibiter and processing technique |
| CN102020978A (en) * | 2010-12-22 | 2011-04-20 | 夹江县龙兴投资有限公司 | Gas well corrosion inhibitor and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 徐兵等.脂肪酸氨基酰胺高温缓蚀剂的研究.《镇江高专学报》.2011,第24卷(第2期),58-60. |
| 脂肪酸氨基酰胺高温缓蚀剂的研究;徐兵等;《镇江高专学报》;20110430;第24卷(第2期);58-60 * |
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