CN106675547A - Method for preparing gel breaker by utilizing modified carbon nano tube immobilized compound enzyme - Google Patents
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- CN106675547A CN106675547A CN201611135251.6A CN201611135251A CN106675547A CN 106675547 A CN106675547 A CN 106675547A CN 201611135251 A CN201611135251 A CN 201611135251A CN 106675547 A CN106675547 A CN 106675547A
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
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Abstract
The invention relates to a method for preparing a gel breaker by utilizing a modified carbon nano tube immobilized compound enzyme and belongs to the technical field of gel breaker preparation. The method comprises the following steps: firstly, utilizing concentrated nitric acid and concentrated sulfuric acid to oxidize and modify the carbon nano tube, thereby acquiring a modified carbon nano tube used as an immobilized enzyme carrier; respectively immobilizing the compound enzyme of beta-mannase, cellulase and protease onto the carbon nano tube, thereby acquiring a modified carbon nano tube immobilized compound enzyme; utilizing a chitosan solution and an Arabic gum solution to prepare a viscous fluid; and wrapping the viscous fluid on the surface of the modified carbon nano tube immobilized compound enzyme and then drying, thereby acquiring the gel breaker. A protecting film is arranged on the gel breaker prepared according to the invention; if the gel breaker is added into a fracturing fluid, the viscosity can be prevented from being lost in advance; the retention rate for the viscosity of the fracturing fluid before gel breaking reaches up to 100%; the lasting gel breaking capacity is above 98h; the flow-back fracturing fluid does not need to be treated and can meet the flow-back requirement; the gel breaker has a considerable economic benefit and can reduce the damage to the stratum; the rock core damage rate is below 15%; and the well yield is increased.
Description
Technical field
The present invention relates to a kind of method that utilization modified carbon nano-tube immobilization compound enzyme prepares gel breaker, belongs to gel breaker
Preparing technical field.
Background technology
In oilfield development process, hydraulic fracturing is the effective ways for improving oil well production efficiency.Its principle is to utilize water-setting
Glue transmits high pressure, and crack is formed in rock stratum, and enters crack using hydrogel carrying proppant.Then, it is broken using gel breaker
The prop-carrying capacity of bad hydrogel, makes proppant be deposited in crack, so that crack can not close, increase crude oil is in oil well
Infiltration rate.
Conventional gel breaker is Ammonium persulfate., but gel breaker addition can be such that fracturing fluid viscosity damages in advance too early or excessively
Lose, affect the width generation capacity of fracturing fluid in work progress, or even cause sand fallout in advance, cause construction failure;And the mistake for adding
It is few, glue can be made brokenly not thorough again, residue and fluid retention injury are caused to oil reservoir, flow conductivity is reduced, affect fracturing effect.It is general
Logical gel breaker dissolves in a liquid, and with fluid loss, in stratum, the gel breaker of dissolving will not be polymerized leak-off with filter cake
The concentration of thing and concentrate, it is impossible to effectively make filter cake break glue, therefore possible permanent damage can be caused to stratum.Another has the disadvantage brokenly
Glue speed is too fast and should not control, and causes fracturing fluid viscosity premature loss in construction.
The content of the invention
The technical problem to be solved:For traditional gel breaker in construction fracturing fluid viscosity premature loss,
And the problem of broken glue inefficiency, it is of the invention first oxidation modification to be carried out to CNT with concentrated nitric acid and concentrated sulphuric acid, obtain carbon modified
Nanotube is used as fixed zymophore, then respectively the compound enzyme of 'beta '-mannase, cellulase and protease is fixed on into carbon and receives
On mitron, modified carbon nano-tube immobilization compound enzyme is obtained, recycle chitosan solution and Arabic glue to be prepared into viscous solution, will
It is coated on modified carbon nano-tube immobilization compound enzyme surface, and gel breaker is obtained after being dried, and it is broken that the present invention is prepared
Colloid, because surface has protecting film, being added in fracturing fluid can prevent viscosity from losing in advance, and enzyme is fixed on into carbon modified
On nanotube, the activity of enzyme can be greatly improved, so as to improve brokenly glue efficiency, reduce the injury to stratum, improve oil well output,
With considerable economic benefit.
To solve above-mentioned technical problem, the technical solution used in the present invention is:
(1)A diameter of 50~the 70nm of 3~5g are weighed, length is 10~20 μm of CNT, in putting it into flask, and respectively
The salpeter solution of 100~150mL of addition mass fractions 65% and the sulfuric acid solution of 120~150mL mass fractions 95%, ultrasonic disperse 5~
10min, is put in oil bath pan after dispersion and is heated to 120~130 DEG C, 10~12h of condensing reflux, backflow be evaporated under reduced pressure after terminating to
It is dry, solid is collected, solid deionized water is cleaned by ultrasonic 2~4 times, 3~5min is washed every time, vacuum drying is put into after washing
Case, is dried 10~20h at a temperature of 90~100 DEG C, collects dried object, obtains modified carbon nano-tube;
(2)1~3g 'beta '-mannases, 1~5g cellulase, 1~5g protease are weighed respectively is added to 150~200mLpH
For in 6.0 disodium hydrogen phosphates and sodium dihydrogen phosphate buffer, stirring 15~20min of mixing obtains complex enzyme liquid, weighs 2~3g
Above-mentioned modified carbon nano-tube is added in complex enzyme liquid, in being put into constant-temperature table, temperature be 4 DEG C, rotating speed be 80~100r/
Carry out under conditions of min after 4~5h of vibration, in being put into refrigerator, 15~20h is fixed under the conditions of 3~5 DEG C, filter after fixing, obtain
Filtering residue, respectively with the disodium hydrogen phosphate and sodium dihydrogen phosphate buffer of pH6.0 and deionized water rinsing 2~3 times, puts after flushing
In entering baking oven, 8~10h is dried at a temperature of 80~100 DEG C, modified carbon nano-tube immobilization compound enzyme is obtained after being dried, it is standby;
(3)Weigh 3~5g shitosans to be added in the acetic acid solution of 300~500g mass fractions 1%, stirring mixes molten to shitosan
Solution, obtains chitosan solution, weighs 8~10g arabic gum powder and is added in 150~200g deionized waters, is heated to 50~60
DEG C, stir to the dissolving of arabic gum powder, Arabic glue is obtained, the chitosan solution of Arabic glue and 160~200g is mixed
Close, stir to obtain viscous solution;
(4)The above-mentioned viscous solution of 250~300g is weighed, 2~3g steps are added in viscous solution(2)Standby modified carbon nano-tube is consolidated
Surely compound enzyme is changed, in being put into ice-water bath, 1~2h of stirring mixing at a temperature of 0~5 DEG C, sucking filtration after stirring obtains filtering residue, is put into baking
In case, 12~15h is dried at a temperature of 70~80 DEG C, gel breaker is obtained after being dried.
The application process of the present invention:Gel breaker prepared by the present invention is added into fracturing fluid, the amount of addition is fracturing fluid
The 1~2% of quality, is stirred after mix homogeneously to it, the fracturing fluid containing gel breaker, then according to a conventional method, is thrown in oil
In well.After testing, viscosity conservation rate reaches 100% before fracturing liquid rubber-breaking, and after breaking gel viscosity is down to 3.6~4.3mPas,
Persistently gel breaking capacity is higher than 98h, and returns discharge fracturing fluid and need not be processed, and reaches the row of returning and requires.
Compared with additive method, Advantageous Effects are the present invention:
(1)Gel breaker surface prepared by the present invention has protecting film, and being added in fracturing fluid can prevent viscosity from losing in advance, pressure
Split viscosity conservation rate before the broken glue of liquid and reach 100%;
(2)The lasting gel breaking capacity of gel breaker prepared by the present invention is higher than 98h, and returns discharge fracturing fluid and need not be processed, and reaches and returns
Row requires, with considerable economic benefit;
(3)Gel breaker prepared by the present invention reduces the injury to stratum, and core damage rate is less than 15%, improves oil well output.
Specific embodiment
A diameter of 50~the 70nm of 3~5g are weighed first, and length is 10~20 μm of CNT, in putting it into flask,
And the salpeter solution of 100~150mL mass fractions 65% and the sulfuric acid solution of 120~150mL mass fractions 95% are separately added into, ultrasound is divided
5~10min is dissipated, is put into after dispersion in oil bath pan and is heated to 120~130 DEG C, 10~12h of condensing reflux, backflow is reduced pressure after terminating
It is evaporated to dryness, collects solid, solid deionized water is cleaned by ultrasonic 2~4 times, 3~5min is washed every time, is put into after washing true
Empty drying baker, is dried 10~20h at a temperature of 90~100 DEG C, collects dried object, obtains modified carbon nano-tube;1~3g is weighed respectively
'beta '-mannase, 1~5g cellulase, 1~5g protease are added to 150~200mLpH for 6.0 disodium hydrogen phosphates and phosphoric acid
In sodium dihydrogen buffer solution, stirring 15~20min of mixing obtains complex enzyme liquid, weighs the above-mentioned modified carbon nano-tubes of 2~3g and is added to
In complex enzyme liquid, in being put into constant-temperature table, temperature be 4 DEG C, rotating speed be 80~100r/min under conditions of carry out 4~5h of vibration
Afterwards, it is put in refrigerator, 15~20h is fixed under the conditions of 3~5 DEG C, filter after fixing, filtering residue is obtained, respectively with the phosphoric acid hydrogen of pH6.0
Disodium and sodium dihydrogen phosphate buffer and deionized water rinsing 2~3 times, are put in baking oven, in 80~100 DEG C of temperature after flushing
8~10h of lower drying, obtains modified carbon nano-tube immobilization compound enzyme after being dried, standby;3~5g shitosans are weighed again is added to 300
In the acetic acid solution of~500g mass fractions 1%, stirring mixes to shitosan dissolving, obtains chitosan solution, weighs 8~10g Arabic
Rubber powder end is added in 150~200g deionized waters, is heated to 50~60 DEG C, is stirred to the dissolving of arabic gum powder, obtains me
Primary glue, the chitosan solution of Arabic glue and 160~200g is mixed, and stir to obtain viscous solution;Finally weigh 250~
The above-mentioned viscous solution of 300g, the standby modified carbon nano-tube immobilization compound enzymes of 2~3g are added in viscous solution, are put into ice-water bath
In, 1~2h of stirring mixing at a temperature of 0~5 DEG C, sucking filtration after stirring obtains filtering residue, in being put into baking oven, at a temperature of 70~80 DEG C
12~15h is dried, gel breaker is obtained after being dried.
Example 1
The a diameter of 70nm of 5g are weighed first, length is 20 μm of CNT, in putting it into flask, and be separately added into 150mL
The salpeter solution of mass fraction 65% and the sulfuric acid solution of 150mL mass fractions 95%, ultrasonic disperse 10min, are put into oil bath pan after dispersion
In be heated to 130 DEG C, condensing reflux 12h, backflow is evaporated to dryness under reduced pressure after terminating, and collects solid, and solid deionized water is surpassed
Sound is cleaned 4 times, and 5min is washed every time, and vacuum drying oven is put into after washing, and 20h is dried at a temperature of 100 DEG C, collects dried object,
Obtain modified carbon nano-tube;3g 'beta '-mannases, 5g cellulase, 5g protease are weighed respectively is added to 200mLpH for 6.0 phosphorus
In sour disodium hydrogen and sodium dihydrogen phosphate buffer, stirring mixing 20min obtains complex enzyme liquid, weighs the above-mentioned modified carbon nano tubes of 3g
Pipe is added in complex enzyme liquid, in being put into constant-temperature table, temperature be 4 DEG C, rotating speed be 100r/min under conditions of vibrated
After 5h, in being put into refrigerator, 20h is fixed under the conditions of 5 DEG C, filtered after fixing, filtering residue is obtained, respectively with the disodium hydrogen phosphate of pH6.0
With sodium dihydrogen phosphate buffer and deionized water rinsing 3 times, it is put into after flushing in baking oven, at a temperature of 100 DEG C 10h is dried,
Modified carbon nano-tube immobilization compound enzyme is obtained after drying, it is standby;5g shitosans are weighed again is added to the acetic acid of 500g mass fractions 1%
In solution, stirring mixes to shitosan dissolving, obtains chitosan solution, weighs 10g arabic gum powder and is added to 200g deionizations
In water, 60 DEG C are heated to, are stirred to the dissolving of arabic gum powder, obtain Arabic glue, the shell of Arabic glue and 200g is gathered
Sugar juice mixes, and stir to obtain viscous solution;The above-mentioned viscous solution of 300g is finally weighed, addition 3g is standby in viscous solution is modified
CNT immobilization compound enzyme, in being put into ice-water bath, the stirring mixing 2h at a temperature of 5 DEG C, sucking filtration after stirring obtains filtering residue, puts
In entering baking oven, 15h is dried at a temperature of 80 DEG C, gel breaker is obtained after being dried.
Gel breaker prepared by the present invention is added into fracturing fluid, the amount of addition is the 2% of fracturing fluid quality, and it is carried out
After being uniformly mixed, the fracturing fluid containing gel breaker, then according to a conventional method, thrown in oil well.After testing, pressure break
Viscosity conservation rate reaches 100% before the broken glue of liquid, and after breaking gel viscosity is down to 4.3mPas, and lasting gel breaking capacity is 99h, and returns row pressure
Splitting liquid need not be processed, and reach the row's of returning requirement.
Example 2
The a diameter of 50nm of 3g are weighed first, length is 10 μm of CNT, in putting it into flask, and be separately added into 100mL
The salpeter solution of mass fraction 65% and the sulfuric acid solution of 120mL mass fractions 95%, ultrasonic disperse 5min, are put in oil bath pan after dispersion
120 DEG C are heated to, condensing reflux 10h, backflow is evaporated to dryness under reduced pressure after terminating, collect solid, by solid deionized water ultrasound
Cleaning 2 times, washs every time 3min, and vacuum drying oven is put into after washing, and 15h is dried at a temperature of 90 DEG C, collects dried object, must change
Property CNT;1g 'beta '-mannases, 1g cellulase, 1g protease are weighed respectively is added to 150mLpH for 6.0 phosphoric acid hydrogen
In disodium and sodium dihydrogen phosphate buffer, stirring mixing 15min obtains complex enzyme liquid, weighs the above-mentioned modified carbon nano-tubes of 2g and adds
Enter in complex enzyme liquid, in being put into constant-temperature table, temperature be 4 DEG C, rotating speed be 80r/min under conditions of carry out vibration 4h after,
In being put into refrigerator, 15h is fixed under the conditions of 3 DEG C, filtered after fixing, filtering residue is obtained, respectively with the disodium hydrogen phosphate and phosphoric acid of pH6.0
Sodium dihydrogen buffer solution and deionized water rinsing 2 times, are put in baking oven after flushing, and 8h is dried at a temperature of 80 DEG C, after being dried
Modified carbon nano-tube immobilization compound enzyme, it is standby;3g shitosans are weighed again to be added in the acetic acid solution of 300g mass fractions 1%, are stirred
Mix and mix to shitosan dissolving, obtain chitosan solution, weigh 8g arabic gum powder and be added in 150g deionized waters, be heated to
50 DEG C, stir to the dissolving of arabic gum powder, obtain Arabic glue, the chitosan solution of Arabic glue and 160g is mixed,
Stir to obtain viscous solution;The above-mentioned viscous solution of 250g is finally weighed, adds the standby modified carbon nano-tubes of 2g to consolidate in viscous solution
Surely compound enzyme is changed, in being put into ice-water bath, the stirring mixing 1h at a temperature of 0 DEG C, sucking filtration after stirring obtains filtering residue, in being put into baking oven,
12h is dried at a temperature of 70 DEG C, gel breaker is obtained after being dried.
Gel breaker prepared by the present invention is added into fracturing fluid, the amount of addition is the 1% of fracturing fluid quality, and it is carried out
After being uniformly mixed, the fracturing fluid containing gel breaker, then according to a conventional method, thrown in oil well.After testing, pressure break
Viscosity conservation rate reaches 100% before the broken glue of liquid, and after breaking gel viscosity is down to 3.8mPas, and lasting gel breaking capacity is 100h, and the row of returning
Fracturing fluid need not be processed, and reach the row's of returning requirement.
Example 3
The a diameter of 60nm of 4g are weighed first, length is 15 μm of CNT, in putting it into flask, and be separately added into 120mL
The salpeter solution of mass fraction 65% and the sulfuric acid solution of 130mL mass fractions 95%, ultrasonic disperse 8min, are put in oil bath pan after dispersion
125 DEG C are heated to, condensing reflux 11h, backflow is evaporated to dryness under reduced pressure after terminating, collect solid, by solid deionized water ultrasound
Cleaning 3 times, washs every time 4min, and vacuum drying oven is put into after washing, and 15h is dried at a temperature of 95 DEG C, collects dried object, must change
Property CNT;2g 'beta '-mannases, 4g cellulase, 4g protease are weighed respectively is added to 170mLpH for 6.0 phosphoric acid hydrogen
In disodium and sodium dihydrogen phosphate buffer, stirring mixing 17min obtains complex enzyme liquid, weighs the above-mentioned modified carbon nano-tubes of 2g and adds
Enter in complex enzyme liquid, in being put into constant-temperature table, temperature be 4 DEG C, rotating speed be 90r/min under conditions of carry out vibration 5h after,
In being put into refrigerator, 17h is fixed under the conditions of 4 DEG C, filtered after fixing, filtering residue is obtained, respectively with the disodium hydrogen phosphate and phosphoric acid of pH6.0
Sodium dihydrogen buffer solution and deionized water rinsing 2 times, are put in baking oven after flushing, and 9h is dried at a temperature of 90 DEG C, after being dried
Modified carbon nano-tube immobilization compound enzyme, it is standby;4g shitosans are weighed again to be added in the acetic acid solution of 400g mass fractions 1%, are stirred
Mix and mix to shitosan dissolving, obtain chitosan solution, weigh 9g arabic gum powder and be added in 170g deionized waters, be heated to
55 DEG C, stir to the dissolving of arabic gum powder, obtain Arabic glue, the chitosan solution of Arabic glue and 180g is mixed,
Stir to obtain viscous solution;The above-mentioned viscous solution of 270g is finally weighed, adds the standby modified carbon nano-tubes of 2g to consolidate in viscous solution
Surely compound enzyme is changed, in being put into ice-water bath, the stirring mixing 1h at a temperature of 3 DEG C, sucking filtration after stirring obtains filtering residue, in being put into baking oven,
14h is dried at a temperature of 75 DEG C, gel breaker is obtained after being dried.
Gel breaker prepared by the present invention is added into fracturing fluid, the amount of addition is the 2% of fracturing fluid quality, and it is carried out
After being uniformly mixed, the fracturing fluid containing gel breaker, then according to a conventional method, thrown in oil well.After testing, pressure break
Viscosity conservation rate reaches 100% before the broken glue of liquid, and after breaking gel viscosity is down to 4.1mPas, and lasting gel breaking capacity is 99h, and returns row pressure
Splitting liquid need not be processed, and reach the row's of returning requirement.
Claims (1)
1. a kind of method that utilization modified carbon nano-tube immobilization compound enzyme prepares gel breaker, it is characterised in that concrete preparation process
For:
(1)A diameter of 50~the 70nm of 3~5g are weighed, length is 10~20 μm of CNT, in putting it into flask, and respectively
The salpeter solution of 100~150mL of addition mass fractions 65% and the sulfuric acid solution of 120~150mL mass fractions 95%, ultrasonic disperse 5~
10min, is put in oil bath pan after dispersion and is heated to 120~130 DEG C, 10~12h of condensing reflux, backflow be evaporated under reduced pressure after terminating to
It is dry, solid is collected, solid deionized water is cleaned by ultrasonic 2~4 times, 3~5min is washed every time, vacuum drying is put into after washing
Case, is dried 10~20h at a temperature of 90~100 DEG C, collects dried object, obtains modified carbon nano-tube;
(2)1~3g 'beta '-mannases, 1~5g cellulase, 1~5g protease are weighed respectively is added to 150~200mLpH
For in 6.0 disodium hydrogen phosphates and sodium dihydrogen phosphate buffer, stirring 15~20min of mixing obtains complex enzyme liquid, weighs 2~3g
Above-mentioned modified carbon nano-tube is added in complex enzyme liquid, in being put into constant-temperature table, temperature be 4 DEG C, rotating speed be 80~100r/
Carry out under conditions of min after 4~5h of vibration, in being put into refrigerator, 15~20h is fixed under the conditions of 3~5 DEG C, filter after fixing, obtain
Filtering residue, respectively with the disodium hydrogen phosphate and sodium dihydrogen phosphate buffer of pH6.0 and deionized water rinsing 2~3 times, puts after flushing
In entering baking oven, 8~10h is dried at a temperature of 80~100 DEG C, modified carbon nano-tube immobilization compound enzyme is obtained after being dried, it is standby;
(3)Weigh 3~5g shitosans to be added in the acetic acid solution of 300~500g mass fractions 1%, stirring mixes molten to shitosan
Solution, obtains chitosan solution, weighs 8~10g arabic gum powder and is added in 150~200g deionized waters, is heated to 50~60
DEG C, stir to the dissolving of arabic gum powder, Arabic glue is obtained, the chitosan solution of Arabic glue and 160~200g is mixed
Close, stir to obtain viscous solution;
(4)The above-mentioned viscous solution of 250~300g is weighed, 2~3g steps are added in viscous solution(2)Standby modified carbon nano-tube is consolidated
Surely compound enzyme is changed, in being put into ice-water bath, 1~2h of stirring mixing at a temperature of 0~5 DEG C, sucking filtration after stirring obtains filtering residue, is put into baking
In case, 12~15h is dried at a temperature of 70~80 DEG C, gel breaker is obtained after being dried.
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Cited By (1)
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CN111187608A (en) * | 2020-01-13 | 2020-05-22 | 西安石油大学 | Enzyme seepage agent for improving guar gum fracturing fluid performance and application thereof |
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CN111187608A (en) * | 2020-01-13 | 2020-05-22 | 西安石油大学 | Enzyme seepage agent for improving guar gum fracturing fluid performance and application thereof |
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Application publication date: 20170517 |