CN105929006B - Except the method that ammonia removes chlorine residue effect in a kind of evaluating oilfield brine - Google Patents
Except the method that ammonia removes chlorine residue effect in a kind of evaluating oilfield brine Download PDFInfo
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- CN105929006B CN105929006B CN201610259093.9A CN201610259093A CN105929006B CN 105929006 B CN105929006 B CN 105929006B CN 201610259093 A CN201610259093 A CN 201610259093A CN 105929006 B CN105929006 B CN 105929006B
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Abstract
Except the method that ammonia removes chlorine residue effect in a kind of evaluating oilfield brine, it is related to the brine in the control technology of oil field oil, especially oil field except ammonia technical field.The present invention measures the oxidation-reduction potential in brine by platinum electrode direct measuring method, judges the effect removed ammonia and remove chlorine residue in brine.Both realized in brine except ammonia is except the on-line checking of the effect of chlorine residue, and reduced the use of drug, saved cost, and eliminate large-scale cost of equipment, and secondary pollution not will cause to environment, at the same have it is sensitive, quickly, the advantages that accuracy is high.
Description
Technical field
The present invention relates to the brine in the control technology of oil field oil, especially oil field to remove ammonia technical field.
Background technique
Industrial brine is the aqueous solution of the salts such as chloride, sulfate, soluble carbonate salt.China's Brine resources are abundant,
Brine is all widely used in multiple fields.Using region each where brine, it is rich in the difference of element, can be used to extract
The elements such as boron, lithium, bromine, potassium.In recent years, brine in chlor-alkali industry using relatively broad, with brine as the original of chlor-alkali production
Material, there is very high economic value.But brine contains a certain amount of ammonia after two alkaline process removing calcium and magnesiums, in the production of chlorine industry,
Ammonia in brine enters electrolytic cell therewith, and agene can be generated in anolyte.Agene is easily in liquid chlorine tank bottom product
It is tired, it easily explodes under the conditions of heated, light-exposed or vibration.Therefore the ammonia that remove in brine seems extremely important.
Currently, industrially frequently with the ammonia nitrogen problem in air stripping method, large-scale ammonia removal equipment processing solution.Air is blown
The method of taking off provides gas-liquid contact interface using air as stripping medium, using packed tower, has reached the purpose for removing ammonia from solution.
The disadvantages of the method are as follows removal efficiency is low, treatment effeciency is lower under winter low temperature, and wind pressure height causes energy consumption high, takes off aliquant ammonia
Gas causes secondary pollution to atmosphere again.And not only complex process, cost are high for large-scale ammonia removal equipment, early investment fund is big,
And operating cost and maintenance cost are all high.
Summary of the invention
Object of the present invention is to propose except ammonia, except the online test method of chlorine residue effect in a kind of brine of oil field, to reduce medicine
The use of product, save the cost improve the safety of production.
The technical scheme is that: it is placed in that temperature is 30 DEG C, pH value is 10~12 with platinum plate electrode and saturated calomel electrode
Carried out in the brine of oil field except ammonia treatment, the oxidation reduction potential value of brine of oil field is measured using open circuit potential, works as survey
When the oxidation reduction potential value of the brine of oil field obtained is 510~530mV, the ammonia content in brine of oil field is then less than 1 mgL-1；
The oil field halogen handle except chlorine residue that temperature is 30 DEG C, pH value is 10~12 is placed in platinum plate electrode and saturated calomel electrode
In water, the oxidation reduction potential value of brine of oil field is measured using open circuit potential, when the redox electricity for the brine of oil field for surveying row
When place value≤10mV, the chlorinity in brine of oil field is then less than 10 mgL-1。
The present invention by platinum electrode direct measuring method measure brine in oxidation-reduction potential, judge in brine except ammonia removes
The effect of chlorine residue.Both realized in brine except ammonia except chlorine residue effect on-line checking, reduce the use of drug, saved at
This, and eliminates large-scale cost of equipment, and not will cause secondary pollution to environment, while having sensitive, and quickly, accuracy is high
The advantages that.
The invention has the following advantages:
1, ammonia effect is removed using oxidation-reduction potential detection sodium hypochlorite, can realizes on-line checking with computer, makes secondary
The dispensing of sodium chlorate is appropriate, will not cause to reduce at chlorine residue in brine containing a large amount of chlorine residue because sodium hypochlorite is excessive
The cost of reason, while the dispensing of sodium hypochlorite is decreased, improve business efficiency.
2, using chlorine residue effect is removed in oxidation-reduction potential detection brine, on-line checking oxidation-reduction potential makes sulfurous acid
Hydrogen sodium or sodium sulfite launch appropriate, the cost of saving chlorine residue processing.
3, sodium hypochlorite removes ammonia, the sodium hydrogensulfite cost of equipment large-scale except chlorine residue can not only be reduced, and save at
This, will not cause secondary pollution to environment.
Detailed description of the invention
When Fig. 1 is that the brine of variant ammonia content is reacted with liquor natrii hypochloritis, the additional amount of sodium hypochlorite and oxidation are also
The canonical plotting of former current potential value.
Fig. 2 is the relational graph of ammonia content in oxidation-reduction potential and brine.
Fig. 3 is that ammonium chloride concentration is 4 mgL-1Brine and sodium hypochlorite reaction ammonia electrode potential diagram.
Fig. 4 is the graph of relation of ammonia gas-sensing electrode potential value and the negative logarithm of ammonia density.
Fig. 5 is 8 mgL-1Ammonium chloride solution reacted with excessive liquor natrii hypochloritis, oxidation-reduction potential and hypochlorous acid
The relational graph of sodium amount.
Fig. 6 is the oxidation-reduction potential figure of aqueous salt brine and sodium hypochlorite reaction.
Fig. 7 is the amount of sodium hydrogensulfite and the relational graph of oxidation-reduction potential.
Fig. 8 is the amount of chlorine residue and the relational graph of oxidation-reduction potential.
Specific embodiment
The content of present invention is described in detail with reference to the accompanying drawings of the specification: attached drawing is only for reference and description, non-
To limit the present invention.
One, by platinum electrode direct measuring method measure brine in oxidation-reduction potential, judge in brine except ammonia effect
Fruit.
1. the early-stage preparations of platinum plate electrode and saturated calomel electrode:
The head of platinum plate electrode is immersed in nitric acid and water with volume ratio as in 1: 1 prepared aqueous solution of nitric acid
10min, then put it into and clean 3min in ultrasonic cleaner, the electrode after ultrasonic cleaning is rinsed 3 times with deionized water
More than.
Saturated calomel electrode is immersed in the 100mL beaker equipped with saturated potassium chloride solution using preceding needs, electrode interior
Solution should be with the presence of crystal.Saturated calomel electrode is using preceding with deionized water flushing 3 times or more.
2. the preparation of the brine of six kinds of ammonium chloride concentrations:
Electronic balance distinguishes six parts of 0.0788g chloride solids of precise, use the purification aqueous salt brine without ammonia as
Every part of chloride solid is dissolved in different amounts of purification aqueous salt brine by bottom liquid respectively, is respectively formed six parts of different ammonia contents
Brine, ammonia density (i.e. the concentration of ammonium chloride) is respectively 2mgL in every part of brine-1、4mg·L-1、6mg·L-1、8mg·L-1、
10mg·L-1、12mg·L-1。
3. the brine of above six parts different ammonia contents is made parallel test, measures and aoxidized in six kinds of different brine of ammonia content
Reduction potential value, and the relational graph of ammonia content in oxidation-reduction potential and brine is drawn, operating procedure is as follows:
A certain 50 mL of brine is first accurately pipetted with pipette in beaker, is placed the beaker in thermostat water bath, is adjusted and is burnt
The temperature of brine is to 30 DEG C in cup, and above treated the platinum plate electrode and saturated calomel electrode head are placed in brine, and with
Electrochemical workstation is connected, and the oxidation-reduction potential of brine is measured using open circuit potential, the time for adjusting open circuit potential sets
It is set to 90min.It reuses micropipette rifle and is slowly added to 1.0 molL-1NaOH solution controls beaker under magnetic stirring
The pH value of middle solution is 10~12.Under magnetic stirring, stablize the revolving speed of magneton.Then equally added by several times with micropipette rifle
Enter liquor natrii hypochloritis, measure the oxidation-reduction potential figure in the brine of six parts that electrochemical workstation provides different ammonia contents,
As shown in Figure 1.
Using ammonia content in each brine as abscissa, using oxidation-reduction potential as ordinate, redox electricity is drawn using Fig. 1
The relational graph of position and ammonia content in brine, as shown in Figure 2.
Linear relationship formula Y=- 1.272X+511.02 of oxidation-reduction potential Y Yu ammonia content X are obtained from Fig. 2.When
The oxidation-reduction potential of brine is within the scope of 510~530 mV, and ammonia content is less than 1 mgL in brine-1, sodium hypochlorite reaches except ammonia
To the production requirement of purification brine.
4. establishing ammonia density is 4 mgL-1Brine and sodium hypochlorite reaction ammonia electrode potential diagram:
Sodium hypochlorite is mixed with water in advance, it is 7.944 gL that concentration, which is made,-1Liquor natrii hypochloritis.
It is 4 mgL that ammonium chloride concentration is accurately pipetted with pipette-150 mL of brine in beaker, place the beaker 30
In DEG C thermostat water bath, continue to equal volume amounts to be slowly added to liquor natrii hypochloritis several times using micropipette rifle, in magnetic force
Under stirring, ammonia gas-sensing electrode potential value is recorded in real time, experimental result is shown in Fig. 3.
As shown in Figure 3 when liquor natrii hypochloritis's additional amount is to 120 μ L, solution oxide reduction potential reaches 510 ~ 530mV
In range, ammonia gas-sensing electrode potential value is and dense by Fig. 4 ammonia gas-sensing electrode potential value and ammonia in 0 mV or more according to Fig. 3
The relation curve for spending negative logarithm can calculate ammonia content at this time and be respectively less than 1 mgL-1, ammonia content has reached experiment in solution at this time
It is required that.
Fig. 4 is variation relation curve of the different brine of ammonia content with ammonia gas-sensing electrode current potential.When ammonia content 1.0 ×
10-5~1.0 × 10-1When mol/L, the negative logarithm of ammonia gas-sensing electrode current potential and ammonia ion concentration is in a linear relationship, ammonia electrode
Current potential V=41.69X-249.8, R2=0.99743(R is the related coefficient of linear equation).
5. the variation of solution oxide reduction potential after excessive sodium hypochlorite is added:
It is 8mgL that ammonia content is accurately pipetted with pipette-150 mL of brine in each beaker, place the beaker 30 DEG C
In thermostat water bath, the brine of the corresponding ammonium chloride concentration is directly added into last time oxidation-reduction potential within the scope of 510~530mV
The usage amount of liquor natrii hypochloritis observes the variation of the oxidation reduction potential value of solution, reuses micropipette rifle several times etc.
Continue to volume to be slowly added to liquor natrii hypochloritis, keeps liquor natrii hypochloritis excessive, under magnetic stirring, record brine in real time
The oxidation reduction potential value of solution, experimental result is shown in Fig. 5.
From Fig. 5 it is known that solution oxide reduction potential continues to rise after the liquor natrii hypochloritis's excess being added,
After excessive about 200 μ L, oxidation-reduction potential is quickly increased, and be can be used as control sodium hypochlorite addition and is done foundation, while making the amount of ammonia
Meet requirement of experiment.
6. the measurement pair practical bittern samples:
Sampled from a certain brine extraction and transportation pipe reason, and measured with ammonia gas-sensing electrode do not remove ammonia before in sample aqueous salt brine ammonia contain
Amount.
Platinum plate electrode and saturated calomel electrode head are placed in 50mL sample aqueous salt brine, sample aqueous salt brine temperature is adjusted
At 30 DEG C, pH value is connected degree 10~12, and with electrochemical workstation, is measured using open circuit potential.The reaction time about
At 200~300 s, magnetic agitation, stablize the revolving speed of magneton.Concentration, which is added, with micropipette rifle gradation equal volume amounts is
7.944 g·L-1Liquor natrii hypochloritis, record oxidation reduction potential value, experimental result is shown in Fig. 6.It is provided by electrochemical workstation
Oxidation-reduction potential Y1, and known linear relation formula Y=- 1.272X+511.02, can measure ammonia content is X1(value with
It is measured not using ammonia gas-sensing electrode except the content of ammonia is consistent in sample aqueous salt brine before ammonia before).The oxidation-reduction potential of solution
Within the scope of 510~530 mV, ammonia content is respectively less than 1mgL in solution-1, sodium hypochlorite reaches requirement except ammonia.It is quick to introduce ammonia
Electrode secondary proof, except the potential value of the aqueous salt brine after ammonia is 0 or more, sodium hypochlorite reaches requirement except ammonia.
Two, the oxidation-reduction potential in brine is measured by platinum electrode direct measuring method, judge in brine except chlorine residue
Effect.
Sodium hypochlorite is used due to removing ammonia in aqueous salt brine above, may cause except aqueous salt brine produces after ammonia
Chlorine, so to brine after removing ammonia must handle except chlorine residue.
The removal of chlorine residue relies primarily on addition sodium hydrogensulfite and is reacted with the mixed solution after dechlorination.Solution oxide is also
Former current potential is quickly down to 8mV, is detected with chlorine residue test paper, and test paper color is white, and solution is almost without chlorine residue, wherein containing cl concn
Less than 10 mgL-1.So, it is believed that when the oxidation-reduction potential of solution is down to 10mV or less, it is believed that chlorine residue quilt substantially
Except complete, meet requirement of experiment is less than 10mgL-1, it is seen that Fig. 8.
Operating procedure is as follows: (1) using purification brine as solvent, be configured to 0.2 gL-1Ammonium chloride solution 50mL, i.e., often
50mL refines the ammonium chloride for containing 0.0100 g in brine.(2) under stirring conditions, it is to about 1.6~2.0 mL concentration of addition
7.944 g·L-1Platinum electrode and saturated calomel electrode are placed in solution by liquor natrii hypochloritis after reacting half an hour, are observed molten
The variation of oxidation reduction potential.(3) after reacting half an hour, from 20mL solution is pipetted in beaker in small beaker, pH is adjusted
Greater than 10, the amount of chlorine residue in chlorine residue test paper detection solution is used.(4) Asia of 0.1 mol/L is added into remaining 30mL solution
Sodium bisulfate is added 100 μ L solution of sodium bisulfite every time using liquid-transfering gun, observes the variation of oxidation-reduction potential.(5) again
After 1.0mL sodium hydrogensulfite is added, the content of chlorine residue in solution at this time is surveyed using chlorine residue test paper, and observes oxidation-reduction potential
Variation.(6) solution of sodium bisulfite is continuously added to 1.6mL, detects the contents of residual chlorine of solution, and the oxidation of recording solution at this time
Reduction potential.With the addition of sodium hydrogensulfite, oxidation-reduction potential is gradually decreased in solution, corresponding residual chlorine amount, using remaining
The detection of chlorine test paper, residual chlorine amount is also gradually decreasing, and when sodium hydrogensulfite reaches appropriate, the amount of chlorine residue also meets and wants in solution
It asks.
Three, chlorine residue effect is removed with what oxidation-reduction potential evaluated sodium sulfite and sodium hydrogensulfite:
Evaluate principle: sodium hydrogensulfite or sodium sulfite are added in the solution containing certain chlorine residue, and the oxidation of solution is also
Former current potential can reduce, and be believed that the amount of chlorine residue has reached requirement when potential drop is down to 10mV.It is evaluated with oxidation-reduction potential
Sodium sulfite and sodium hydrogensulfite remove chlorine residue effect, the speed changed by solution oxide reduction potential, it can be seen that the two is removed
The difference of chlorine residue effect.
Operating method: (1) solution of sodium bisulfite and mass fraction that preparation mass fraction is 5% and 15% respectively are 5% He
15% sodium sulfite solution.(2) certain density (0.0100 g/50 mL) ammonium chloride solution 500 is prepared with exquisite brine
mL.(3) take 50 mL ammonium chloride solutions in beaker with pipette, addition 2mL concentration is 7.944 gL-1Sodium hypochlorite it is molten
Liquid reacts half an hour under appropriate stirring.(4) after complete reaction, the pH of solution at this time is detected using pH meter, and more than use
Chlorine test paper detects the amount of chlorine residue in solution at this time.(5) platinum electrode and saturated calomel electrode are connected with electrochemical workstation, and will
Electrode is placed in solution, detects the oxidation-reduction potential of solution at this time.(6) step 1 is slowly added in Xiang Shangshu solution to be prepared
Drug, pay attention to required time when recording solution oxidation-reduction potential is down to 10 mV or less.(7) it is computed, mass fraction
All it is 600 μ L for 5% sodium hydrogensulfite and the Optimum of sodium sulfite solution, can similarly obtains the sulfurous that mass fraction is 15%
The Optimum of sour hydrogen sodium and sodium sulfite solution.The pH value of solution reduces about 0.05, can almost ignore the variation of pH.It uses
Chlorine residue test paper detection, the residual chlorine amount before the non-dosing of solution are 100 ~ 200 mg/L.Experimental result is shown in Table 1, it is known that, sodium sulfite and
Sodium hydrogensulfite removes chlorine residue effect relatively.But the sodium hydrogensulfite that mass fraction is 5% or mass fraction is 15% is except remaining
Chlorine effect is all better than the sodium sulfite that mass fraction is 5% or mass fraction is 15%.And the sodium hydrogensulfite that mass fraction is 15%
It is fastest except chlorine residue effect is best.
The amount that chlorine residue after different drugs is added in table 1 reaches the time used in requirement
Claims (1)
1. except the method that ammonia removes chlorine residue effect in a kind of evaluating oilfield brine, it is characterised in that: use hypochlorous acid in brine of oil field
Sodium solution is carried out except during ammonia, by platinum plate electrode and saturated calomel electrode be placed in temperature be 30 DEG C, pH value be 10~12 into
It went except the oxidation reduction potential value of brine of oil field being measured using open circuit potential, when what is measured in the brine of oil field of ammonia treatment
When the oxidation reduction potential value of brine of oil field is 510~530mV, i.e., the ammonia content in brine of oil field is then less than 1 mgL-1, so
Afterwards brine of oil field handle except chlorine residue using sodium hydrogensulfite or sodium sulfite solution, be carried out in brine of oil field except chlorine residue
Platinum plate electrode and saturated calomel electrode same as described above, are placed in that temperature is 30 DEG C, pH value is 10~12 to carry out by Cheng Zhong
In the brine of oil field handled except chlorine residue, the oxidation reduction potential value of brine of oil field is measured using open circuit potential, when the oil measured
When oxidation reduction potential value≤10mV of field brine, i.e., the chlorinity in brine of oil field is then less than 10 mgL-1, then brine of oil field
It has had reached except ammonia is except chlorine residue effect.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2485657Y (en) * | 2001-05-28 | 2002-04-10 | 刘秀宁 | Automatic inspector for amonia and nitrogen contents in sewage |
| JP2005181279A (en) * | 2003-11-27 | 2005-07-07 | Iwaki Co Ltd | Apparatus for measuring residual chlorine, and electrode unit |
| WO2006112521A1 (en) * | 2005-04-15 | 2006-10-26 | Mitsubishi Heavy Industries, Ltd. | Method of electrolyzing wastewater containing ammonia nitrogen and apparatus therefor |
| US20110297539A1 (en) * | 2003-11-14 | 2011-12-08 | Fis Inc. | Water quality analyzer |
| CN104215679A (en) * | 2014-09-30 | 2014-12-17 | 国家电网公司 | Electrochemical method for measuring free residual chlorine in water |
-
2016
- 2016-04-25 CN CN201610259093.9A patent/CN105929006B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2485657Y (en) * | 2001-05-28 | 2002-04-10 | 刘秀宁 | Automatic inspector for amonia and nitrogen contents in sewage |
| US20110297539A1 (en) * | 2003-11-14 | 2011-12-08 | Fis Inc. | Water quality analyzer |
| JP2005181279A (en) * | 2003-11-27 | 2005-07-07 | Iwaki Co Ltd | Apparatus for measuring residual chlorine, and electrode unit |
| WO2006112521A1 (en) * | 2005-04-15 | 2006-10-26 | Mitsubishi Heavy Industries, Ltd. | Method of electrolyzing wastewater containing ammonia nitrogen and apparatus therefor |
| CN104215679A (en) * | 2014-09-30 | 2014-12-17 | 国家电网公司 | Electrochemical method for measuring free residual chlorine in water |
Non-Patent Citations (1)
| Title |
|---|
| 盐卤水中的氨（铵）含量的电位法快速测定;陈敬平 等;《化学传感器》;20150930;第35卷(第3期);第54-58页 * |
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