CN107892909A - A kind of high efficiency composition sulphur removal corrosion inhibitor and preparation method thereof - Google Patents
A kind of high efficiency composition sulphur removal corrosion inhibitor and preparation method thereof Download PDFInfo
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- CN107892909A CN107892909A CN201711483613.5A CN201711483613A CN107892909A CN 107892909 A CN107892909 A CN 107892909A CN 201711483613 A CN201711483613 A CN 201711483613A CN 107892909 A CN107892909 A CN 107892909A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/54—Compositions for in situ inhibition of corrosion in boreholes or wells
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/32—Anticorrosion additives
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Abstract
The invention discloses a kind of high efficiency composition sulphur removal corrosion inhibitor and preparation method thereof, the sulphur removal corrosion inhibitor is made up of following component by weight：22 parts of ferrous gluconate, 18 parts of ferrous sulfate, 30 parts of zinc oxide, 10 parts of stearmide.The present invention in water-base drilling fluid can high dissolution, pH value be 12 when be less likely to occur to precipitate, drilling fluid system pH value be 9 10, temperature be 70 DEG C when, sulfur removal effectiveness can reach 99.4%.Ferrous ion is easily absorbed by organic matter in the present invention simultaneously, and the complex compound of formation and drilling fluid containing iron ion filtrate and drilling cuttings etc. effectively reduce H in former oil and gas all without the pollution for causing environment2S content.
Description
Technical field
The present invention relates to petrochemical industry, and in particular to a kind of to be used to remove what is carried in down-hole formation in drilling process
Wet contains H2S、CO2Deng pernicious gas and add iron-based zinc-base mixing sulphur removal corrosion inhibitor in drilling fluid and its preparation side
Method.
Background technology
According to statistics, the waste of the average drilling rod in the whole nation is per 1 meter of drilling well, and drilling rod 4kg is lost, and 75%-95% drilling rod damages
Mistake is due to caused by corrosion, and Sichuan gas field containing coloured glaze drill tool corrosion speed is 1.3-2.6mm/a, serious even more than 3.9mm/
A, H present in drilling fluid2S is the serious threat to drilling technology.H2S is a kind of extremely toxic substance, when concentration in an atmosphere surpasses
When crossing 20/1000000ths, people just can not normal work.H2S intrusion completion fluids can cause serious corrosion, content to downhole pipeline
For 5mg/L when with regard to that can be corroded carbon steel, cause downhole pipeline to be broken in a few minutes.With oil-gas Layer（Or target zone）Contact
Various fluid systems are referred to as completion fluid.Contain H boring2During S Oil/gas Wells, drill in fluid H same first2S contact, afterwards each
The various completion fluids used in item underground work will also contact H2S, so, compared with other systems, completion fluid is by H2S intrusions
Chance is most, causes the probability of corrosion maximum.Depending merely on raising borehole fluid density and pH value prevents H2The method of S corrosion can not
Lean on.And appropriate desulfurizer and corrosion inhibitor is reused under the conditions of high density, high ph-values, then it can drill safely containing H2S layers, smoothly
Completion.
At present, tackling the main method of hydrogen sulfide corrosion has undercoating method, chemical method, addition corrosion inhibitor and selects anti-sulphur
The methods of material, but for being completed the oil gas oil field gone into operation, more suitable method is to be subtracted using addition corrosion inhibiter to reach
The purpose of slow corrosion.The issuing and implementation of simultaneously increasingly strict environmental legislation will cause efficient, pollution-free, recycling to turn into desulfurization
The main flow of technological development.The concentration of Air Hydrogen Sulfide is more than 50ppm, will stimulate tracheae, cause conjunctivitis, currently require that
Concentration of hydrogen sulfide is less than 2ppm in natural gas and crude oil.But the used alkaline sulfur elimination in oil field, to reach 2ppm standard, need
More sulfur elimination is added, and these alkali formula sulfur eliminations can generate sediment with hydrogen sulfide effect, block gas channel, shadow
Ring the production of Oil/gas Well.So the sulfur elimination that development can effectively absorb hydrogen sulfide is necessary.Domestic adopted solid extensively
Sulfur elimination, main active iron oxide, zinc oxide and basic zinc carbonate.The advantages of solid desulfurating agent of activated ferric oxide class is sulphur
Rong great, cost is low, but desulfuration efficiency is not high, is mainly used in thick desulfurization and half fine de-sulfur, treated exit gas vulcanization
Hydrogen concentration is less than 20ppm；The advantages of zinc oxide and the solid desulfurating agent of basic zinc carbonate class is desulfuration efficiency height, is mainly used in essence
Desulfurization, treated exit gas concentration of hydrogen sulfide are generally below 1ppm.
Based on above-mentioned analysis, a kind of preparation technology is simple, cost input is low, practical, easily and H2S-phase combines, generation
The high efficiency composition sulphur removal corrosion inhibitor for the normal production that thing is water-soluble, does not pollute the environment, does not influence oil gas field is in the industry
It is badly in need of.
The content of the invention
It is an object of the present invention to provide a kind of preparation technology is simple, cost input is low, practical, easily and H2S-phase knot
Close, product is water-soluble, the high efficiency composition sulphur removal corrosion inhibitor of normal production that does not pollute the environment, do not influence oil gas field and its
Preparation method.
In order to achieve the above object, present invention employs following technical scheme, the dosage of each component of the present invention is also process
Inventor is carried out largely groping to summarize what is drawn, and the high efficiency composition sulphur removal that each component dosage is prepared in the range of following weight is delayed
Erosion agent is respectively provided with the effect of desulfuration efficiency normal production that is high, free from environmental pollution, not influenceing oil gas field.
A kind of efficient sulphur removal corrosion inhibitor, is made up of the raw material of following weight：
Ferrous gluconate 18-24 parts, ferrous sulfate 16-20 parts, zinc oxide 28-32 parts, stearmide 8-12 parts.
Further, the sulphur removal corrosion inhibitor is made up of the raw material of following weight：
22 parts of ferrous gluconate, 18 parts of ferrous sulfate, 30 parts of zinc oxide, 10 parts of stearmide.
A kind of preparation method of efficiently sulphur removal corrosion inhibitor, is by the ferrous gluconate, ferrous sulfate, oxygen of above-mentioned formula ratio
Change in zinc, Stearyl Amine addition batch mixer, be stirred 1 hour, discharging packaging is made.
The present invention is combined with ferrous ion, zinc oxide.The condition of optimal sulfur removal effectiveness：PH value is 9 ~ 10,
Temperature is 70 DEG C, the dosage of inorganic agent and vulcanized sodium（The amount of material）Than for 1.2:1.Under the conditions of optimal sulphur removal, sulfur removal effectiveness
It can reach 99.4%.
The present invention reacts with sulfide completely by the affinity between iron, zinc and sulfide, its moment.
1st, the selection of formula
The complex compound of 1.1 ferrous irons and the derivative of sugar makees sulfur elimination corrosion inhibiter（Remove H2S）
Ca(C6H11O7)2+FeSO4→Fe(C6H11O7)2+CaSO4
1.2 zinc oxide and hydrogen sulfide reaction generation zinc sulphide and water, remove hydrogen sulfide
ZnO+H2S=ZnS ↓+H2O
The fixed H of many of drill in fluid that 1.3 usual sulphur removal corrosion inhibitors are used in petroleum drilling and mining2S mechanism
(1) copper-based sulfur elimination (forming insoluble CuS)；
(2) oxidation iron-based sulfur elimination (forms insoluble Fe2S3)；
(3) formaldehyde/methanol (forming episulfide compounds not soluble in water)；
(4) glyoxal (forming Thioacetal and other compounds)；
(5) nitrite is (by H2S is oxidized to Sulfur)；
(6) reacted with amine (generation thiamines compound)；
(7) with sulphite reaction (by Oxidation of Hydrogen Sulfide into Sulfur)；
(8) (generating compound epithio/nitrogen compound) is reacted with diazine.
These reactions are easy to desulfurization rather than fixed hydrogen sulfide in drilling fluid mostly, meanwhile, these reactants and generation
Thing can cause the problem of significant health, safety and environment aspect.
For simplicity and complicated and possible product is avoided, preferably selection is to utilize the parent between iron, zinc and sulphur
And power, it is due to that they are that environment is subjected to reason, its small toxicity that iron, zinc are especially recommended.
1.4 preferable iron, the compound sulfur elimination of zinc should possess two main characters:
(1) reaction speed is very fast；
(2) it is big with the amount of reaction of Salmon-Saxl（Iron is in the form of a solution）.
Other requirements are as follows:
(1) iron compound is solvable in the salt solution of water or high saliferous；
(2) dissolubility is kept, Fe (OH) is not contained under conditions of pH12 or higher is reached for3Precipitation；
(3) FeS, ZnS precipitation can be also formed when making sulphion concentration very low；
(4) it is minimum to the performance impact of mud after before the reaction；
(5) with reaction of Salmon-Saxl before and after, it is substantially pollution-free to environment.
The porous Fe of selection index system3O4, this method begins to use from early stage in 20th century, but due to reaction speed and journey
Degree is restricted, and some reports show that only 30% iron reacts, and as pH≤8, reaction speed is optimal（It is or lower）, pH
It is higher, make reaction speed slower.
It is under development, H2Concentration in the production liquid of S after the reaction is expected to be 20% even more high, therefore, highly concentrated to reduce
Spend dangerous caused by gas ease table, the danger during pH of drilling fluid≤8, preferably adjust higher pH (12) and add effective sulphur removal
Agent is to be reacted rapidly, in this case, Fe3O4The processing method of base is not ideal enough, so as to need another chemical combination of iron
Thing.
Soluble inorganic molysite is unavailable, because they can produce colloidal metal hydroxide in pH≤7, then we
The feasibility of iron complex can only be determined, due to the stability by available iron couplings and Fe (OH)3It is deliquescent with FeS
Limitation, optional species are reduced, and this method will estimate whether pH limitation has to the influence and sulfide that give Stability of Metal Complexes
The possibility of precipitation.
The oxidizing process of part iron is concerned about first, and ferric iron has bigger vigor than ferrous iron, because it can be with more
More sulfide reactions, such as
The reaction of ferrous iron and equimolar sulfide：Fe2++S2-=FeS↓(1)
And it is ferric reaction it is increasingly complex：2Fe3++3S2-=Fe2S3↓(2)
Part sulphur is oxidized to single element sulphur (S) by ferric iron：Fe2S3→2FeS+S(3)
In a word, Fe3+Than etc. weight Fe2+The amount of sulphur compound is eliminated more than 50%, this illustrates that it has bigger superiority.
However, Fe (OH)3Dissolubility than Fe (OH)2Much lower, this allows for the stabilization that needs are issued in high pH situations
Property becomes more difficult.It is estimated that the divalence iron complex containing amino hydroxy acid is very limited to high ph-values ability to bear.
It is a kind of that stable Fe complex compounds are Fe at least when pH is 113+[ethylenediamine-N, dinitrogen], but this compound is in mud
Serious gelatinization reaction (being probably because polymer crosslinking effect causes) is generated in slurry composition.
Ferrous complex compound is influenceed the smaller Rheological Problems that can't cause drilling fluid in oxidizing process by pH value.Base
The compatibility of stability and mud system under validity, high pH and the influence to environment, the compound of final choice is two
The complex compound (complex) of valency iron and the derivative of sugar.
From environmentally saying, the compound has superperformance, is because the sugar in the molecule is easy to point by bacterial action
Solution, while iron is changed into active Fe2+, it is to compare Fe3+More efficiently organic matter.
Zn2++S2-→ZnS↓
Zinc ion forms product zinc sulphide with sulphur, and ZnS is only in pH<H can be just generated when 32S, but be in most cases can not
Can occur.
ZnCO3、ZnO、Zn(OH)2At a temperature of atmospheric condition, when high ph-values or low ph value, solubility increases quickly, because of this
It is its characteristic.ZnO is when pH value reaches 9-11, with H2S reaction generations ZnS and H2O, reaction equation are as follows：
ZnO+H2S→ZnS↓+ H2O
Effect from pH value be 11-13 when, water-soluble curve sees ZnO water soluble zinc ion, has very high balanced capacity,
Under room temperature condition, control ph, due to such phenomenon, even if the zinc oxide sulfur elimination for having dissolving can solve high ph-values mud
Problem.The zincic acid ion of high concentration is provided, because zincic acid ion can be changed into zinc ion, can be reacted with hydrogen sulfide, as sulphur removal
Agent solves mud problems.
In the drilling fluid of routine, it is impossible to be worked below pH=4 in sour environment, and zinc oxide is stablized at a high ph,
Until ZnS precipitations, it is swift in response effectively.
The beneficial effects of the present invention are：
（1）Sulphur removal reaction speed is very fast；
（2）It is big with the amount of reaction of Salmon-Saxl；
（3）Iron compound is solvable in the salt solution of water or high saliferous；
（4）Keep dissolubility, reach pH for 12 or it is higher under conditions of be free of Fe (OH)3Precipitation；
（5）Make that FeS precipitations can be formed when sulphion concentration is very low；
（6）After before the reaction, property of drilling fluid is influenceed small；
（7）With reaction of Salmon-Saxl before and after, it is substantially pollution-free to environment.
From environmentally saying, the present invention has good characteristic, is because sugared in the molecule is easy to point by bacterial action
Solution, while iron is changed into active Fe2+, it is to compare Fe3+More useful organic matter.
By experiment, sulphur removal corrosion inhibitor of the present invention is insensitive to pH, and the rheological characteristic of drilling fluid will not be had an impact,
It is simultaneously good with other inorganic agent compatibilities in drilling fluid.Ferrous ion is easily by organic matter institute in sulphur removal corrosion inhibitor of the present invention
Absorb, the complex compound of ferrous ion and organic acid is environment-friendly, the row of drilling fluid and drilling cuttings containing iron ion filtrate
Put all without initiation environmental problem.
Embodiment
Embodiment 1
A kind of efficient sulphur removal corrosion inhibitor
Ferrous gluconate 22kg, ferrous sulfate 18kg, zinc oxide 30kg, stearmide 10kg are added in batch mixer, stirring
Mixing 1 hour, discharging packaging are made.
Embodiment 2
A kind of efficient sulphur removal corrosion inhibitor
Ferrous gluconate 18kg, ferrous sulfate 16kg, zinc oxide 28kg, stearmide 8kg are added in batch mixer, stirring is mixed
Close 1 hour, discharging packaging is made.
Embodiment 3
A kind of efficient sulphur removal corrosion inhibitor
Ferrous gluconate 24kg, ferrous sulfate 20kg, zinc oxide 32kg, stearmide 12kg are added in batch mixer, stirring
Mixing 1 hour, discharging packaging are made.
Test example
Calcium gluconate 26kg, ferrous sulfate 18kg, water 37kg are added in engagement machine, heating, stirring engagement, are reacted at 90 DEG C
Reactant is obtained after 1 hour；It is transferred to after drying in pulverizer, adds basic zinc carbonate 10kg, stearmide 9kg is sufficiently stirred, powder
Broken 1 hour, pack, discharging.
The corrosion inhibiter prepared in Example 1 by two aspect laboratory is evaluated, one for the present invention to sulfide
Removing degree and speed；Two potential impacts for the present invention to property of drilling fluid.
1st, removing degree and speed trial of the present invention to sulfide:
The saturated sodium-chloride salt solution that proportion is 1.2, which adds KOH, makes pH reach 12, then by the Na of known quantity2S is dissolved in high ph-values
In salt solution, in this case, H2S mainly exists with ionic condition, therefore, adds ionic state sulfide and simplifies process simultaneously
Keep away rabbit and use H2The difficulty of S gases and harm.
Add sulphur removal corrosion inhibitor and monitor reduction of the sulfide concentration with the time, while also test the influence of order of addition,
As a result show, order of addition is on reacting without influence.
As a result quickly, reacting dose is very big, is surveying for the reaction speed of discovery sulfide and ferrous iron carbohydrate complex
In examination, the brine sample of two pH=12 of beginning is subject to the Na of equivalent concentration2S, then, equivalent is separately added into two samples
Sulphur removal corrosion inhibitor of the present invention and porous Fe3O4, it as a result can draw the reaction speed of soluble iron quickly, and the opposing party, although solid
Body Fe3O4Initial action speed quickly, but speed reduce quickly and only have 30% participation reaction.It is obvious that using the present invention
Sulphur removal corrosion inhibitor only needs the time of 8-10 minutes to remove the maximum amount of sulfide, and Fe3O4At least 70 minutes are needed, is tested
Show, sulphur removal corrosion inhibitor of the present invention is on performance without influence.
2nd, the present invention is tested the potential impact of property of drilling fluid, and table 1 is the composition that sulfide tests drilling fluid, and table 2 is
Sulphur removal corrosion inhibitor or the performance without sulphur removal corrosion inhibitor drilling fluid liquid be present, table 3 includes three kinds of experiments：1 is that drilling fluid only has sulphur
Change sodium；2 be that drilling fluid only has sulphur removal corrosion inhibitor；3 be that the existing vulcanized sodium of drilling fluid has sulphur removal corrosion inhibitor again.Concrete outcome is shown in Table 1,
Table 2 and table 3.
The sulfide of table 1 tests the composition of drilling fluid
。
Sulphur removal corrosion inhibitor or the performance without sulphur removal corrosion inhibitor drilling fluid liquid be present in table 2
。
Performance of the vulcanized sodium with sulphur removal corrosion inhibitor to liquid in the drilling fluid of table 3 be present
。
Find out that sulphur removal corrosion inhibitor of the present invention does not have harmful effect to property of drilling fluid by table 1, table 2 and table 3.In drilling fluid
After the middle addition present invention, the viscosity and shear force of drilling fluid have declined, but unobvious, and this is the powered feelings in end face of the material itself
Result caused by condition.Adding sulphion and sulphur removal corrosion inhibitor of the present invention does not have harmful effect to property of drilling fluid, adds sulphion
With, due to generating FeS, drilling fluid rapidly goes to black after sulphur removal corrosion inhibitor of the present invention.
3rd, the corrosion inhibiter field experiment prepared in Example 1：
Table 4, table 5 list first well drilling fluid composition and performance.Carbon dioxide in oil reservoir in addition to hydrogen sulfide also be present, added
The oxide control carbon dioxide of amount, GGT are used to monitoring the dissolution degree of sour gas, the network containing iron in mud (drilling fluid)
Compound sulfur elimination, the vestige of any hydrogen sulfide is not found on ground after trip-out.But it is dense to find that carbon dioxide is measured after making a trip
Spend for 3000mg/L.
The fresh-water drilling fluid composition of table 4
。
Experimental liquid performance on table 5 plus sulphur removal corrosion inhibitor well
。
Table 6, table 7 list second mouthful of property of drilling fluid, wherein sulfide hydrogen is 36% in the gas phase, carbon dioxide 6%.
Contain 6% hydrogen sulfide, 2% carbon dioxide in oil phase.GGT, which tests, does not find the vestige of any hydrogen sulfide in earth's surface, and dioxy
Change carbon and measure 200ppm, second mouthful of well core experiment is similar to first well, containing 6% hydrogen sulfide and 2% titanium dioxide in oil phase
Carbon.
The property of drilling fluid of table 6
。
Experimental liquid performance on table 7 plus sulfur elimination well
。
Claims (3)
1. a kind of efficient sulphur removal corrosion inhibitor, it is characterised in that the sulphur removal corrosion inhibitor is made up of the raw material of following weight：Portugal
Grape saccharic acid ferrous iron 18-24 parts, ferrous sulfate 16-20 parts, zinc oxide 28-32 parts, stearmide 8-12 parts.
2. a kind of efficient sulphur removal corrosion inhibitor, it is characterised in that the sulphur removal corrosion inhibitor is made up of the raw material of following weight：Portugal
Grape saccharic acid is ferrous 22 parts, 18 parts of ferrous sulfate, 30 parts of zinc oxide, 10 parts of stearmide.
3. a kind of preparation method of efficiently sulphur removal corrosion inhibitor according to claim 1 or 2, it is characterised in that this method is
The ferrous gluconate of above-mentioned formula ratio, ferrous sulfate, zinc oxide, Stearyl Amine are added in batch mixer, it is small to be stirred 1
When, discharging packaging is made.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109536265A (en) * | 2018-12-21 | 2019-03-29 | 中国石油集团渤海钻探工程有限公司 | Except sulfur type coiled tubing drag reducer |
| CN109777392A (en) * | 2019-03-04 | 2019-05-21 | 重庆科技学院 | A kind of New drilling fluid hydrogen sulfide scavenger and preparation method thereof |
| CN110331951A (en) * | 2019-06-28 | 2019-10-15 | 中国石油集团川庆钻探工程有限公司 | The method for removing hydrogen sulfide in oil base drilling fluid using basic zinc carbonate aqueous solution |
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| CN109777392A (en) * | 2019-03-04 | 2019-05-21 | 重庆科技学院 | A kind of New drilling fluid hydrogen sulfide scavenger and preparation method thereof |
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