CN104374868A - Detection method of movable microsphere gel content in produced fluid and application thereof - Google Patents

Detection method of movable microsphere gel content in produced fluid and application thereof Download PDF

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Publication number
CN104374868A
CN104374868A CN201410705366.9A CN201410705366A CN104374868A CN 104374868 A CN104374868 A CN 104374868A CN 201410705366 A CN201410705366 A CN 201410705366A CN 104374868 A CN104374868 A CN 104374868A
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microballoon
ammonium sulfate
concentration
iron ammonium
shake gels
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CN201410705366.9A
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CN104374868B (en
Inventor
张俊
任从军
王俊良
聂凤云
刘丽华
刘武友
谢冰晰
蒋伟
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China Petroleum and Natural Gas Co Ltd
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China Petroleum and Natural Gas Co Ltd
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Abstract

The invention provides a detection method of movable microsphere gel content in produced fluid and application thereof. The method includes: preparing movable microsphere gel solution with known movable microsphere gel concentration, adding the movable microsphere gel solution to a container, adding potassium dichromate solution and silver sulfate-sulfuric acid solution, performing heating to allow reaction, performing titrating with ammonium ferrous sulfate after reaction is over, and drawing a linear regression equation between the movable microsphere gel concentration and mass of the ammonium ferrous sulfate which is converted from microsphere-consumed potassium dichromate; experimenting a sample according to the steps above, and calculating the soft movable micro-gel content in the produced liquid according to the consumed mass of the ammonium ferrous sulfate by means of the linear regression equation. The method helps measure the movable microsphere gel in the produced liquid, the influence of oil content, inorganic ions and chromaticity of the produced liquid during measuring is eliminated, and accurate measurement of the concentration of the movable microsphere gel in the produced liquid is achieved.

Description

A kind of Produced Liquid microballoon shake gels detection method of content and application thereof
Technical field
The invention belongs to petroleum production engineering field, be specifically related to a kind of Produced Liquid microballoon shake gels detection method of content and application thereof, reach the object understanding combination of zones situation.
Background technology
Microballoon shake gels is a kind of novel deep profile correction chemical agent, oil field that is serious for major reservoir water logging, remaining oil distribution high degree of dispersion has good transfer drive effect, this transfer drive technology can directly adjust the uneven situation of reservoir deep water drive effectively, improves sweep efficiency.
Microballoon shake gels is a kind of polyacrylamide polymers W/O emulsion fluid microballoon, existing detection method is by the impact of the factors such as oil content, inorganic ions and the colourity of Produced Liquid own in temperature, Produced Liquid, cause the mass concentration deviation that measures comparatively large or exceed measurement range, cannot the content of Measurement accuracy microballoon shake gels in Produced Liquid.At present, Kjeldahl's method is only had to measure this Realization of Product accurate quantitative analysis in document.
Summary of the invention
One object of the present invention is to provide a kind of Produced Liquid microballoon shake gels detection method of content; The method consumes the quality of iron ammonium sulfate by back titration, eliminates metallic ion, disturbing factor that nitrogen-containing group (Kjeldahl's method) produces, improves the accuracy of testing result.
Another object of the present invention is to provide the application of the inventive method in Produced Liquid microballoon shake gels content detection.
For reaching above-mentioned purpose, on the one hand, the invention provides a kind of Produced Liquid microballoon shake gels detection method of content, described method comprises:
(1) equation of linear regression is drawn: the microballoon shake gels aqueous solution that preparation microballoon shake gels concentration is known, get microballoon shake gels aqueous solution noted earlier to be added to respectively in container, add potassium bichromate solution and silver sulfate-sulfuric acid solution respectively, add thermal response, reaction terminates rear iron ammonium sulfate titration, and the potassium dichromate drawing the concentration-microballoon consumption of microballoon shake gels is converted into the equation of linear regression of the quality of iron ammonium sulfate;
(2) cubage: materials and test as stated above, according to the quality of the iron ammonium sulfate consumed, calculates the content of microballoon shake gels in Produced Liquid by equation of linear regression.
According to method of the present invention, described method comprises:
(1) equation of linear regression is drawn: the microballoon shake gels aqueous solution that preparation microballoon shake gels concentration is known, get microballoon shake gels aqueous solution noted earlier to be added to respectively in container, add potassium bichromate solution and silver sulfate-sulfuric acid solution respectively, add thermal response, reaction terminates rear iron ammonium sulfate titration, the volume of the consumption of record iron ammonium sulfate, blank assay is done with Produced Liquid before noting microballoon, calculate the volume that iron ammonium sulfate consumes, the potassium dichromate drawing the concentration-microballoon consumption of microballoon shake gels is converted into the equation of linear regression of the quality of iron ammonium sulfate:
y=5.907x+0.212 (R 2=0.999)
The potassium dichromate of microballoon consumption is converted into the computing method of iron ammonium sulfate quality:
M=C (V blank-V) × 392
The quality that m---iron ammonium sulfate consumes, g;
The concentration of c---iron ammonium sulfate, mol/L;
V is blank---and blank assay consumes the volume of iron ammonium sulfate;
V---sample consumes the volume of iron ammonium sulfate;
(2) cubage: get 20mL sample and test as stated above, according to the quality of the iron ammonium sulfate consumed, calculates the content of microballoon shake gels in Produced Liquid by the equation of linear regression described in step (1).
According to method of the present invention, it is characterized in that the concentration of the microballoon shake gels aqueous solution of the concentration known described in step (1) is respectively 10mg/L, 20mg/L, 50mg/L, 100mg/L, 150mg/L, 200mg/L, 250mg/L and 300mg/L.
According to method of the present invention, be get each 20mL of described microballoon shake gels aqueous solution to be added to respectively in container in step (1), add potassium bichromate solution and 30mL silver sulfate-sulfuric acid solution that 5mL concentration is 1.5mol/L respectively.
According to method of the present invention, add thermal response described in step (1) for backflow 2h.
According to method of the present invention, add examination iron after step (1) reaction terminates and try clever indicator, then use ferrous sulphate titration.
According to method of the present invention, in step (1), ferroin indicator consumption is that 2-6 drips; Be preferably 4.
According to method of the present invention, in step (1), ferrous ammonium sulfate concentration is 0.1mol/L.
According to method of the present invention, reaction is indicator with ferroin after terminating in step (1), and with the titration of 0.1mol/L iron ammonium sulfate, solution has yellow to become blue-green to bronzing, is terminal.
Method according to claim 1 and 2, in step (1), described microballoon shake gels aqueous solution is added to after in container respectively, first add potassium bichromate solution and anti-bumping beaded glass respectively, connect reflux condensing tube, add silver sulfate-sulfuric acid solution from condenser pipe top again, add thermal response; Wherein preferably add 3 anti-bumping beaded glasses.
According to method of the present invention, in described Produced Liquid, microballoon shake gels content is 10mg/L ~ 500mg/L.
On the other hand, present invention also offers the application of the inventive method in Produced Liquid microballoon shake gels content detection.
According to application of the present invention, in described Produced Liquid, microballoon shake gels content is 10mg/L ~ 300mg/L.
In sum, the invention provides a kind of Produced Liquid microballoon shake gels detection method of content and application thereof.Method tool of the present invention has the following advantages:
(1) concentration range 10mg/L ~ 300mg/L is measured,
(2)R 2=0.999,
(3) detection limit 10mg/L,
(4) a large amount of metal ion disturbance is got rid of.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 checkout equipment figure, and wherein drawing reference numeral is: 1, condenser pipe 2, conical flask 3, heating jacket.
Embodiment
Describe the beneficial effect of implementation process of the present invention and generation below by way of specific embodiment in detail, be intended to help reader to understand essence of the present invention and feature better, not as can the restriction of practical range to this case.
1, the drafting of microballoon shake gels typical curve
Preparation microballoon shake gels concentration known is 10mg/L, 20mg/L, 50mg/L, 100mg/L, 150mg/L, 200mg/L, 250mg/L, (application block generally microballoon shake gels is same manufacturer production to the microballoon shake gels aqueous solution of 300mg/L, as manufacturer changes or production specifications change, new standard solution need be prepared), as shown in Figure 1, getting standard solution 20mL is added in 250mL ground conical flask, (adding 5mL concentration is 1.5mol/L potassium bichromate solution (concentration of the Produced Liquid potassium dichromate of variable concentrations is all consistent with consumption) and 3 anti-bumping beaded glasses, connect reflux condensing tube, 30mL silver sulfate-sulfuric acid solution is added from condenser pipe top, heating, timing is started from solution boiling, backflow 2h, be indicator with ferroin after reaction terminates, with the titration of 0.1mol/L iron ammonium sulfate, solution has yellow to become blue-green to bronzing, be terminal, the volume of the consumption of record iron ammonium sulfate, blank assay is done with Produced Liquid before noting microballoon, calculate the volume that iron ammonium sulfate consumes, the potassium dichromate drawing the concentration-microballoon consumption of microballoon shake gels is converted into the equation of linear regression of the quality of iron ammonium sulfate:
y=5.907x+0.212 (R 2=0.999)
The potassium dichromate of microballoon consumption is converted into the computing method of iron ammonium sulfate quality:
M=C (V blank-V) × 392
The quality that m---iron ammonium sulfate consumes, g;
The concentration of c---iron ammonium sulfate, mol/L;
V is blank---and blank assay consumes the volume of iron ammonium sulfate;
V---sample consumes the volume of iron ammonium sulfate.
392---the relative molecular mass of six ferrous sulfate hydrate ammoniums.
2, the pre-treatment of Produced Liquid
Measure Produced Liquid 100mL, use quantitative filter paper filters out Residual oil and impurity is for subsequent use.
3, measure 20mL Produced Liquid to measure by method described in 1, the quality of the iron ammonium sulfate that record consumes, calculates the mass concentration of microballoon.(because the concentration of microballoon in Produced Liquid is unknown, when measurement result is greater than 300mg/L, answering the solution after dilution process to redeterminate)
This detection method adds up detection 22 well at the displacement of reservoir oil block 9 of Jilin Oil Field microballoon shake gels, block 11, block 12.
Remarks: testing result is greater than 300mg/L are converted by dilution Produced Liquid to obtain.
4, preparing mass concentration with distilled water and on-the-spot water is the microballoon shake gels 500mL being respectively 100mg/L, measure the concentration of microballoon shake gels in known solution according to 5.3 starch iodide methods in this method and SY/T 6576-2003 respectively, measurement result is as follows:
Conclusion:
1, carry out mensuration by this method and standard method to the microballoon shake gels solution that the concentration that distilled water is prepared is 100mg/L to draw: use the microballoon shake gels solution concentration measurement result of distilled water preparation close to true value, relative deviation is less, and two kinds of method measurement result relative deviations are respectively 3.5% and 3.3%.
2, carry out mensuration by this method and standard method to the microballoon shake gels solution that the concentration that on-the-spot water is prepared is 100mg/L to draw: the obvious deviation true value of standard method measurement result, and our rule is close to true value 100mg/L, standard deviation is respectively 4.75% and 10.00%.
3, describe according to standard, starch iodide method can not eliminate the interference of oil, amine goods and materials, iodate ion and dark matter in solution, and therefore starch iodide method measurement result deviation true value is comparatively large, and these materials then affect less on this method measurement result.

Claims (10)

1. a Produced Liquid microballoon shake gels detection method of content, is characterized in that, described method comprises:
(1) equation of linear regression is drawn: the microballoon shake gels aqueous solution that preparation microballoon shake gels concentration is known, get microballoon shake gels aqueous solution noted earlier to be added to respectively in container, add potassium bichromate solution and silver sulfate-sulfuric acid solution respectively, add thermal response, reaction terminates rear iron ammonium sulfate titration, and the potassium dichromate drawing the concentration-microballoon consumption of microballoon shake gels is converted into the equation of linear regression of the quality of iron ammonium sulfate;
(2) cubage: materials and test as stated above, according to the quality of the iron ammonium sulfate consumed, calculates the content of microballoon shake gels in Produced Liquid by equation of linear regression.
2. method according to claim 1, is characterized in that, described method comprises:
(1) equation of linear regression is drawn: the microballoon shake gels aqueous solution that preparation microballoon shake gels concentration is known, get microballoon shake gels aqueous solution noted earlier to be added to respectively in container, add potassium bichromate solution and silver sulfate-sulfuric acid solution respectively, add thermal response, reaction terminates rear iron ammonium sulfate titration, the volume of the consumption of record iron ammonium sulfate, blank assay is done with Produced Liquid before noting microballoon, calculate the volume that iron ammonium sulfate consumes, the potassium dichromate drawing the concentration-microballoon consumption of microballoon shake gels is converted into the equation of linear regression of the quality of iron ammonium sulfate:
y=5.907x+0.212(R 2=0.999)
The potassium dichromate of microballoon consumption is converted into the computing method of iron ammonium sulfate quality:
M=C (V blank-V) × 392
The quality that m---iron ammonium sulfate consumes, g;
The concentration of c---iron ammonium sulfate, mol/L;
V is blank---and blank assay consumes the volume of iron ammonium sulfate;
V---sample consumes the volume of iron ammonium sulfate;
(2) cubage: get 20mL sample and test as stated above, according to the quality of the iron ammonium sulfate consumed, calculates the content of microballoon shake gels in Produced Liquid by the equation of linear regression described in step (1).
3. method according to claim 1 and 2, is characterized in that the concentration of the microballoon shake gels aqueous solution of the concentration known described in step (1) is respectively 10mg/L, 20mg/L, 50mg/L, 100mg/L, 150mg/L, 200mg/L, 250mg/L and 300mg/L.
4. method according to claim 1 and 2, it is characterized in that, be get each 20mL of described microballoon shake gels aqueous solution to be added to respectively in container in step (1), add silver sulfate-sulfuric acid solution that potassium bichromate solution that 5mL concentration is 1.5mol/L and 30mL mass concentration are 0.5% respectively.
5. method according to claim 1 and 2, is characterized in that, adds thermal response for backflow 2h described in step (1).
6. method according to claim 1 and 2, is characterized in that, adds examination iron and tries clever indicator, then use ferrous sulphate titration after step (1) reaction terminates; Wherein preferably ferroin indicator consumption is that 2-6 drips; Be more preferably 4; Wherein going back preferably sulfuric acid ferrous ammonium concentration is 0.1mol/L.
7. method according to claim 1 and 2, is characterized in that, reaction is indicator with ferroin after terminating in step (1), and with the titration of 0.1mol/L iron ammonium sulfate, solution has yellow to become blue-green to bronzing, is terminal.
8. method according to claim 1 and 2, it is characterized in that, in step (1), described microballoon shake gels aqueous solution is added to after in container respectively, first add potassium bichromate solution and anti-bumping beaded glass respectively, connect reflux condensing tube, add silver sulfate-sulfuric acid solution from condenser pipe top again, add thermal response; Wherein preferably add 3 anti-bumping beaded glasses.
9. method according to claim 1 and 2, is characterized in that, in described Produced Liquid, microballoon shake gels content is 10mg/L ~ 500mg/L.
10. the application of claim 1 ~ 9 any one method in Produced Liquid microballoon shake gels content detection; Wherein in preferred described Produced Liquid, microballoon shake gels content is 10mg/L ~ 300mg/L.
CN201410705366.9A 2014-11-27 2014-11-27 A kind of Produced Liquid microballoon shake gels detection method of content and application thereof Active CN104374868B (en)

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