CN101813635A - Method for detecting content of nitrogenous polymer gel micro-sphere - Google Patents
Method for detecting content of nitrogenous polymer gel micro-sphere Download PDFInfo
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- CN101813635A CN101813635A CN 201010145008 CN201010145008A CN101813635A CN 101813635 A CN101813635 A CN 101813635A CN 201010145008 CN201010145008 CN 201010145008 CN 201010145008 A CN201010145008 A CN 201010145008A CN 101813635 A CN101813635 A CN 101813635A
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Abstract
The invention relates to a method for detecting the content of nitrogenous polymer gel micro-sphere, which provides scientific evidence for improving a synthesis technique, controlling the quality of products and summarizing rules of applications of micro-spheres in oil fields. The method for detecting the content of nitrogen contained polymer gel micro-sphere is characterized in that bluestone, lemery and selenium powder or sodium selenate are taken as a catalyst, and sulphuric acid is used as a digestion sample so that organic nitrogen in nitrogen contained polymer gel micro-sphere is decomposed to ammonia; the ammonia and the sulphuric acid are compounded into ammonium sulphate, and the ammonia is basified and distilled from ammonium sulphate; standard acid is used for titration after the absorption with acid; and the nitrogen content of the sample is calculated, the nitrogen content is multiplied by a reduction factor of the nitrogen-containing polymer, and the gel micro-sphere content of the nitrogen-containing polymer can be obtained.
Description
Technical field
This method relates to the profile control that is widely used in the oil-field development field, the polymer with nitrogen microspheres product of water-plugging technology detects the method for polymer with nitrogen gel micro-sphere content.
Prior art
Profile control and water plugging technology is the important method that improves oil recovery rate by water filling.Wherein the polymer with nitrogen microballoon is the novel blocking agent that profile control and water plugging uses.Though the polymer with nitrogen microballoon is applied, still there is not this microballoon content detecting method of analysis at present.
Goal of the invention
The objective of the invention is by polymer with nitrogen microballoon content detecting method, for improving synthetic technology, control product quality and summary microballoon provide scientific basis in the rule of field use.
Summary of the invention
Polymer with nitrogen microballoon content detecting method of the present invention is to be catalyzer with copper sulphate, glazier's salt and selenium powder or sodium selenate, make the digestion sample with sulfuric acid, make the organic nitrogen in the polymer with nitrogen gel micro-sphere be decomposed into ammonia, these ammonia and sulphation are combined into ammonium sulfate, alkalization distills out ammonia then, again with the standard acidometric titration, obtains the nitrogen content in the sample after absorbing with acid, multiply by the reduction coefficient of polymer with nitrogen, can try to achieve polymer with nitrogen gel micro-sphere content.
The concrete steps that detect:
1) takes by weighing 0.2～2.0g polymer with nitrogen gel micro-sphere product as sample 1 or draw 10～20mL and inject produced liquid in oil well behind the microballoon as sample 2, move in the dry digestion bottle respectively, add 0.3～0.5g copper sulphate, 0.5～1.0g glazier's salt, 0.05～0.1g selenium powder and 10～30mL sulfuric acid, to digest bottle and tilt to prop up slowly heating on well heater, treat the whole charings of content, after foam stops fully, Fast Heating, and keep that liquid is little in the bottle boils, be the blue-green clear to liquid after, take off and be cooled to room temperature, it is standby as liquid to be measured 1 to add 20mL water mixing.
2) will digest bottle one side ports and connect water vapor generation bottle, the opposite side port arrives receiving bottle after connecting condenser, Centronics port connects tap funnel, dress water 400mL in the bottle takes place in water vapour, add 0.1～0.3mL methyl red indicator solution and 1～3mL sulfuric acid, be acid with the pH value that keeps water less than 5, the water in the bottle takes place in the heated and boiled water vapour; In receiving bottle, add sour absorption liquid and 0.05～0.2mL mixing indicator solution of 10～20mL mass concentration 1%, and the lower end of condenser is inserted under the receiving bottle liquid level; With mass concentration is that 40% sodium hydroxide solution is poured in the tap funnel, opens piston, treats that water vapour takes place to begin distillation after the water boiling in the bottle, and steam feeds and is equipped with in the digestion bottle of liquid 1 to be measured, and ammonia is absorbed to receiving bottle by condenser zone; The inclination receiving bottle makes the condenser lower end leave liquid level, and redistillation 1min collects the condensed fluid in the condenser, washes outside, condenser lower end then, makes liquid 2 to be measured all enter receiving bottle; Taking off receiving bottle, is terminal point with standard salt acidometric titration indicator to grey or bluish violet, the volume V1 of record quota of expenditure hydrochloric acid.
3) take by weighing and abovementioned steps 1) in copper sulphate, glazier's salt, selenium powder and the sulfuric acid of equal in quality, add in the digestion bottle, do not add sample, respectively set by step 1) and step 2) do blank test, measure under the blank condition volume V of titration quota of expenditure hydrochloric acid
2
4) result treatment
1) nitrogen content in the polymer with nitrogen gel micro-sphere sample calculates
Be calculated as follows:
X
1＝【(V
1-V
2)×c×0.014】/m×100％ (1)
X
2＝【(V
1-V
2)×c×0.014】/V×10
6 (2)
In the formula, X
1--the mass percentage content of nitrogen in the sample 1 polymer with nitrogen gel micro-sphere;
X
2--the content of nitrogen in the sample 2 polymer with nitrogen gel micro-spheres;
V
1--the volume of sample titration quota of expenditure hydrochloric acid;
V
2--the volume of blank titration quota of expenditure hydrochloric acid;
0.014--1mL standard hydrochloric acid the suitable gram number of nitrogen;
The concentration of the accurate solution of c--acidity scale;
M--takes by weighing the quality of sample 1;
V--draws the volume of sample 2;
(3) microballoon content in the calculation sample
Be calculated as follows:
Y
1＝F×X
1 (3)
Y
2＝F×X
2 (4)
Y in the formula
1--microballoon content (%) in the sample 1;
Y
2--microballoon content (mg/L) in the sample 2;
The F--nitrogen content is scaled the coefficient of microsphere polymer gel micro-sphere content;
Analysis result should be accurate to 0.01%.
Described mixing indicator solution is by the 0.1% methyl red ethanolic solution and 1 parts by volume moral, the 0.1% methylene blue ethanolic solution of 2 parts by volume or be that 0.1% methyl red ethanolic solution of 2 parts by volume and 0.1% bromcresol green ethanolic solution of 1 parts by volume are made into.
Adopt method of the present invention to be used to detect the content of polymer with nitrogen gel micro-sphere,, also obtain good effect at aspects such as improving oil recovery factor for the improvement and the field use of this product synthetic technology provides foundation.
Description of drawings
Accompanying drawing 1 is the structural representation of slaking apparatus; 1 is adjustable electric furnace among the figure, the 2nd, and digestion bottle, the 3rd, retort stand, the 4th, surge flask, the 5th, one-level absorption bottle, the 6th, secondary absorption bottle.
Accompanying drawing 2 is distillation absorption plant structural representations; Among the figure, the 7th, electric jacket, the 8th, steam generator, the 2nd, digestion bottle, the 9th, a platform, the 10th, tap funnel, the 11st, ground bend pipe, the 12nd, condenser, the 13rd, bend pipe, the 14th, receiving bottle.
Embodiment
Application example 1, the detection of polymer with nitrogen gel micro-sphere product content:
With reference to attached Fig. 1 and 2, take by weighing 0.2000g polymer with nitrogen gel micro-sphere product liquid and 0.5g copper sulphate, 1.0g glazier's salt is put into the digestion bottle of Fig. 1 slaking apparatus after 0.1g selenium powder and 30mL sulfuric acid mix, with the digestion bottle with 45 tiltedly on the asbestos gauge of adjustable electric furnace, careful heating, treat the whole charings of content, after foam stops fully, strengthen firepower, and keep that liquid is little in the bottle boils, after being the blue-green clear to liquid, taking off to put and be chilled to room temperature, carefully add 20mL water.Put cold after, mixing is standby.Get and handle copper sulphate, glazier's salt, selenium powder and the sulfuric acid of sample same amount and do blank test, after distillation absorption plant alkalization distillation shown in Figure 2 absorbs,, consume hydrochloric acid 4mL with 0.0665mol/L salt acidometric titration by Same Way.Can calculate microballoon content with above-mentioned data:
1) by the nitrogen content in formula (1) the calculating polymer with nitrogen gel micro-sphere:
X
1＝【(V
1-V
2)×c×0.014】/m×100％
＝[(4-0)×0.0665×0.014]/0.2000×100％
＝1.862％
2) calculate polymer gel micro-sphere content by formula (2):
Y
1＝F×X
1
＝5.07×1.862％
＝9.44％
Application example 2, the detection of polymer gel micro-sphere content in the produced liquid in oil well:
With reference to attached Fig. 1 and 2, draw the 15mL produced liquid in oil well of oil removing after filtration, put into the digestion bottle of Fig. 1 slaking apparatus after 0.3g copper sulphate, 0.5g glazier's salt, 0.05g selenium powder and 20mL sulfuric acid mix, the digestion bottle is tiltedly propped up on the asbestos gauge of adjustable electric furnace with 45, careful heating, treat the whole charings of content, after foam stops fully, strengthen firepower, and keep that liquid is little in the bottle boils, after being the blue-green clear to liquid, taking off to put and be chilled to room temperature, carefully add 20mL water.Put cold after, mixing is standby.Get and handle copper sulphate, glazier's salt, selenium powder and the sulfuric acid of sample same amount and do blank test, after distillation absorption plant alkalization distillation shown in Figure 2 absorbs,, consume hydrochloric acid 0.35mL with 0.0665mol/L salt acidometric titration by Same Way.Can calculate microballoon content with above-mentioned data:
(1) by the content of nitrogen in formula (two) calculation sample
X
2＝[(V
1-V
2)×c×0.014]/V×10
6
＝[(0.35-0)×0.0665×0.014]/15×10
6
＝2.17mg/L
(2) by polymer gel micro-sphere content in formula (four) calculation sample
Y
2＝F×X
2
＝5.07×2.17
＝11.00mg/L
Show by example: this method can detect the content and the concentration of product in oilfield produced fluid of polymer with nitrogen gel micro-sphere.For improving polymer with nitrogen gel micro-sphere synthetic technology, the control product quality is for oil-field development provides foundation.
The present invention has provided two typical embodiment, and with reference to summary of the invention of the present invention, the conversion relevant parameter all can be realized the purpose that detects.
Claims (3)
1. polymer with nitrogen gel micro-sphere content detecting method, it is characterized in that: with copper sulphate, glazier's salt and selenium powder or sodium selenate is catalyzer, make the digestion sample with sulfuric acid, make the organic nitrogen in the polymer with nitrogen gel micro-sphere be decomposed into ammonia, these ammonia and sulphation are combined into ammonium sulfate, and alkalization distills out ammonia then, after absorbing with acid again with the standard acidometric titration, obtain the nitrogen content in the sample, multiply by the reduction coefficient of polymer with nitrogen, can try to achieve polymer with nitrogen gel micro-sphere content.
2. polymer with nitrogen gel micro-sphere content detecting method according to claim 1 is characterized in that the concrete steps that detect:
1) takes by weighing 0.2～2.0g polymer with nitrogen gel micro-sphere product as sample 1 or draw 10～20mL and inject produced liquid in oil well behind the microballoon as sample 2, move in the dry digestion bottle respectively, add 0.3～0.5g copper sulphate, 0.5～1.0g glazier's salt, 0.05～0.1g selenium powder and 10～30mL sulfuric acid, to digest bottle and tilt to prop up slowly heating on well heater, treat the whole charings of content, after foam stops fully, Fast Heating, and keep that liquid is little in the bottle boils, be the blue-green clear to liquid after, take off and be cooled to room temperature, it is standby as liquid to be measured 1 to add 20mL water mixing;
2) will digest bottle one side ports and connect water vapor generation bottle, the opposite side port arrives receiving bottle after connecting condenser, Centronics port connects tap funnel, dress water 400mL in the bottle takes place in water vapour, add 0.1～0.3mL methyl red indicator solution and 1～3mL sulfuric acid, be acid with the pH value that keeps water less than 5, the water in the bottle takes place in the heated and boiled water vapour; In receiving bottle, add sour absorption liquid and 0.05～0.2mL mixing indicator solution of 10～20mL mass concentration 1%, and the lower end of condenser is inserted under the receiving bottle liquid level; With mass concentration is that 40% sodium hydroxide solution is poured in the tap funnel, opens piston, treats that water vapour takes place to begin distillation after the water boiling in the bottle, and steam feeds and is equipped with in the digestion bottle of liquid 1 to be measured, and ammonia is absorbed to receiving bottle by condenser zone; The inclination receiving bottle makes the condenser lower end leave liquid level, and redistillation 1min collects the condensed fluid in the condenser, washes outside, condenser lower end then, makes liquid 2 to be measured all enter receiving bottle; Taking off receiving bottle, is terminal point with standard salt acidometric titration indicator to grey or bluish violet, the volume V of record quota of expenditure hydrochloric acid
1
3) take by weighing and abovementioned steps 1) in copper sulphate, glazier's salt, selenium powder and the sulfuric acid of equal in quality, add in the digestion bottle, do not add sample, respectively set by step 1) and step 2) do blank test, measure under the blank condition volume V of titration quota of expenditure hydrochloric acid
2
4) result treatment
1) nitrogen content in the polymer with nitrogen gel micro-sphere sample calculates
Be calculated as follows:
X
1＝【(V
1-V
2)×c×0.014】/m×100％ (1)
X
2＝【(V
1-V
2)×c×0.014】/V×10
6 (2)
In the formula, X
1---the mass percentage content of nitrogen in the sample 1 polymer with nitrogen gel micro-sphere;
X
2---the content of nitrogen in the sample 2 polymer with nitrogen gel micro-spheres;
V
1---the volume of sample titration quota of expenditure hydrochloric acid;
V
2---the volume of blank titration quota of expenditure hydrochloric acid;
0.014---1mL standard hydrochloric acid the suitable gram number of nitrogen;
C---the concentration of the accurate solution of acidity scale;
M---take by weighing the quality of sample 1;
V---draw the volume of sample 2;
(2) microballoon content in the calculation sample
Be calculated as follows:
Y
1＝F×X
1 (3)
Y
2＝F×X
2 (4)
Y in the formula
1---microballoon content (%) in the sample 1;
Y
2---microballoon content (mg/L) in the sample 2;
F---nitrogen content is scaled the coefficient of microsphere polymer gel micro-sphere content;
Analysis result should be accurate to 0.01%.
3. polymer with nitrogen gel micro-sphere content detecting method according to claim 2, it is characterized in that described mixing indicator solution is by the 0.1% methyl red ethanolic solution and 1 parts by volume moral, the 0.1% methylene blue ethanolic solution of 2 parts by volume or be that 0.1% methyl red ethanolic solution of 2 parts by volume and 0.1% bromcresol green ethanolic solution of 1 parts by volume are made into.
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|---|---|---|---|
| CN 201010145008 CN101813635A (en) | 2010-04-08 | 2010-04-08 | Method for detecting content of nitrogenous polymer gel micro-sphere |
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|---|---|---|---|
| CN 201010145008 CN101813635A (en) | 2010-04-08 | 2010-04-08 | Method for detecting content of nitrogenous polymer gel micro-sphere |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103994915A (en) * | 2013-02-17 | 2014-08-20 | 张琤 | Minisize microwave quick-acting distillation device |
| CN104155232A (en) * | 2014-07-31 | 2014-11-19 | 中国石油大学(北京) | Device for evaluating sulfur resistance of gel used in well completion process of unbalanced drill |
| CN104374868A (en) * | 2014-11-27 | 2015-02-25 | 中国石油天然气股份有限公司 | Method for detecting content of microsphere mobile gel in produced liquid and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415961A (en) * | 2002-12-05 | 2003-05-07 | 大庆油田有限责任公司 | Method for measuring carboxylates din ternary combination flooding injection grout and consistency of polymer |
| CN201051096Y (en) * | 2007-06-14 | 2008-04-23 | 南开大学 | A novel Kjeldahl nitrogen measurement device |
-
2010
- 2010-04-08 CN CN 201010145008 patent/CN101813635A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415961A (en) * | 2002-12-05 | 2003-05-07 | 大庆油田有限责任公司 | Method for measuring carboxylates din ternary combination flooding injection grout and consistency of polymer |
| CN201051096Y (en) * | 2007-06-14 | 2008-04-23 | 南开大学 | A novel Kjeldahl nitrogen measurement device |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103994915A (en) * | 2013-02-17 | 2014-08-20 | 张琤 | Minisize microwave quick-acting distillation device |
| CN104155232A (en) * | 2014-07-31 | 2014-11-19 | 中国石油大学(北京) | Device for evaluating sulfur resistance of gel used in well completion process of unbalanced drill |
| CN104155232B (en) * | 2014-07-31 | 2017-01-18 | 中国石油大学(北京) | Device for evaluating sulfur resistance of gel used in well completion process of unbalanced drill |
| CN104374868A (en) * | 2014-11-27 | 2015-02-25 | 中国石油天然气股份有限公司 | Method for detecting content of microsphere mobile gel in produced liquid and application thereof |
| CN104374868B (en) * | 2014-11-27 | 2016-04-06 | 中国石油天然气股份有限公司 | Method for detecting content of microsphere mobile gel in produced liquid and application thereof |
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Open date: 20100825 |