CN105733550B - A kind of recyclable fracturing fluid gelatinizer of amino acids and preparation method thereof - Google Patents
A kind of recyclable fracturing fluid gelatinizer of amino acids and preparation method thereof Download PDFInfo
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- CN105733550B CN105733550B CN201610187780.4A CN201610187780A CN105733550B CN 105733550 B CN105733550 B CN 105733550B CN 201610187780 A CN201610187780 A CN 201610187780A CN 105733550 B CN105733550 B CN 105733550B
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- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
Abstract
The present invention relates to recyclable fracturing fluid gelatinizer of a kind of amino acids and preparation method thereof, which be formulated by following components：Modified xantham gum 7 10%, gellan gum 5 7%, clay stabilizer 0.5 1%, conditioning agent 0.6 1%, protective agent 0.3 0.7%, polyethylene glycol 10%, dispersant 1~2%, surplus is water；Above-mentioned percentage is mass percent.The thickening agent has good compatibility, can increase viscosity, and frictional resistance is low, and solid-carrying performance is good, and residue is few, small to formation damage, and anti-salt property is high, the features such as having higher instant capacity, can be used for high temperature deep well.The thickening agent is when configuring fracturing fluid without many additives, realize that conventional fracturing fluid (or acidizing and fracturing fluid) Infinite Cyclic utilizes, make fracturing fluid possess formula be simple and convenient to operate, be of low cost, using water wisely, continuous mixture, clean manufacturing the characteristics of.
Description
Technical field
The present invention relates to recyclable fracturing fluid gelatinizer of a kind of amino acids and preparation method thereof, belong to fracturing fluid technology,
The problem of main fracturing fluid in the prior art that solves is difficult to meet environmental requirement, reuse.
Background technology
Oil-gas field development effect depends on fracturing technology and fracturing fluid, and conventional fracturing fluid (or acidizing and fracturing fluid) is mainly planted
Thing glue (guanidine glue etc.) thickening agent (or acid solution) and clay stabilizer, cleanup additive, preservative, fungicide, pH value conditioning agent etc. add
The mixing liquid that agent forms by a certain percentage, belongs to disposable recyclable fracturing fluid, with degree of thickening is good, glue joins, it is wide etc. to be applicable in
Feature, therefore be widely used in the exploitation of oil gas field.But conventional fracturing fluid (or acidizing and fracturing fluid) water consumption is big, no
It can reuse, it is poor to environmental suitability.And also there are anti-salt property is poor, viscosity is small for thickening agent, it is impossible to be used in high temperature deep well,
And the continuous mixture of fracturing fluid prepared in construction is can not achieve, the problems such as instant capacity is poor.
It is new in order to adapt to《Law on Environmental Protection》Requirement, realize fracturing fluid and it is other enter well return discharge opeing and recycle and do not land
Purpose.Need to study a kind of thickening agent while overcome disadvantages mentioned above, to substitute conventional fracturing fluid (or acidizing and fracturing fluid)
Many additives, realize that conventional fracturing fluid (or acidizing and fracturing fluid) Infinite Cyclic utilizes, are provided simultaneously with supporting simple, operation side
Just the characteristics of, of low cost, using water wisely, continuous mixture, clean manufacturing.
The content of the invention
To solve the above-mentioned problems, the purpose of the present invention is a kind of recyclable fracturing fluid gelatinizer of amino acids and its preparation
Method, the thickening agent have good compatibility, can increase viscosity, and frictional resistance is low, and solid-carrying performance is good, and residue is few, and stratum is hindered
Evil is small, and anti-salt property is high, the features such as having higher instant capacity, can be used for high temperature deep well.The thickening agent when configuring fracturing fluid without
Must many additives, realize that conventional fracturing fluid (or acidizing and fracturing fluid) Infinite Cyclic utilizes, possessing fracturing fluid, formula is simple, behaviour
The characteristics of making convenient, of low cost, using water wisely, continuous mixture, clean manufacturing.
The purpose of the present invention is what is realized by following technical proposal, a kind of recyclable fracturing fluid gelatinizer of amino acids,
It is characterized in that：It is formulated by following components：Modified xantham gum 7-10%, gellan gum 5-7%, clay stabilizer 0.5-1%,
Conditioning agent 0.6-1%, protective agent 0.3-0.7%, polyethylene glycol 10%, dispersant 1~2%, surplus are water；Above-mentioned percentage is matter
Measure percentage.
The modified xantham gum, its preparation method are：By weight, by 20 parts of xanthans, 270 parts of solvent, catalysis
7 parts of agent is added in three mouthfuls of reaction bulbs equipped with reflux condensate device, be stirred at room temperature swelling 24 it is small when, then heat to 50
DEG C, 5 parts of modifying agent is slowly added to, when reaction 24 is small；By reaction product acetone precipitation, washing, unreacted modifying agent is removed
And catalyst, filtering；When drying 8 is small in vacuum drying oven under temperature 50 C, modified xantham gum is obtained；Wherein xanthans is flat
Average molecular weight is 500 × 104；Modifying agent is benzyl chloride；Catalyst is sodium hydroxide；Solvent is ethanol.
The gellan gum, its preparation method comprise the following steps：By her eastern algae pseudomonad through eggplant bottle strain access three
Angle bottle culture is concentrated, shaking table culture 18h at 28 DEG C, is then accessed 300L seed tank cultures and is concentrated, 18 are cultivated at 28~30 DEG C
~20h, then force feed cultivate 72h into 3000L fermentation tanks at identical temperature, be finally sent at the identical temperature of 50t fermentation tanks and maintain
72h, obtains gellan gum liquid；The fermentation medium is that mass ratio is 2% soybean slag, 2% sucrose and 96% water composition.
The clay stabilizer is potassium chloride；The conditioning agent is petroleum sodium sulfonate；The protective agent is 10
Number white oil；Dispersant is micron or nanometer grade silica.
The molecular weight of the polyethylene glycol is 12,000,000.
A kind of preparation method of the recyclable fracturing fluid gelatinizer of amino acids, it is characterized in that：Specifically include as follows
Step：
1）In the water that the polyethylene glycol of formula ratio and dispersant are sequentially added to formula ratio, 300r/min is at the uniform velocity stirred
5min, makes it be uniformly dispersed, and it is spare to obtain mixed liquor；
2）The powder of the modified xantham gum of formula ratio and gellan gum is crossed and obtains uniform powder with the sieving of 120 mesh respectively,
3）Modified xantham gum after sieving and gellan gum powder are added into step 1）Mixed liquor in, 500r/min is at the uniform velocity stirred
Mixing 0.5h makes it be uniformly dispersed；
4）The clay stabilizer of formula ratio is added into step 3）Mixed liquor in allocate uniform, then add the tune of formula ratio
Section agent and protective agent stir evenly.
The present invention has following technique effect compared with prior art：1）Swelling time is fast, and the dissolution time of thickening agent is
No more than 5min, and the dissolution time of scene routine is again smaller than 9min；2）With heat safe effect, the thickening agent of 4% present invention
Temperature resistant capability reaches 140-145 DEG C；3）The amino acids thickening agent viscosity is existing 2 times of thickening agent viscosity；4）Improving can
Recycle salt resistance and the anti-aging property of fracturing fluid；5）The existing thickening agent dosage of modified xantham gum and gellan gum amount ratio of the present invention
It is low；6）The thickening agent, without many additives, realizes that conventional fracturing fluid (or acidizing and fracturing fluid) is infinitely followed when configuring fracturing fluid
Ring utilize, make fracturing fluid possess formula be simple and convenient to operate, be of low cost, using water wisely, continuous mixture, the spy of clean manufacturing
Point；Through field application, the continuous pressing crack construction of five collecting well groups, than conventional pressure break using water wisely more than 50%, returns discharge opeing utilization with water
Rate 100%.
The present invention is described in further detail with reference to embodiment and embodiment attached drawing, but not as to the present invention's
Limit.
Brief description of the drawings
Fig. 1 is the solution heat resistance figure that concentration of the present invention is the recyclable fracturing fluid gelatinizer of 4% amino acids.
Embodiment
A kind of recyclable fracturing fluid gelatinizer of amino acids, it is formulated by following components：Modified xantham gum 7-
10%th, gellan gum 5-7%, clay stabilizer 0.5-1%, conditioning agent 0.6-1%, protective agent 0.3-0.7%, polyethylene glycol 10%, scattered
Agent 1~2%, surplus are water；Above-mentioned percentage is mass percent.
A kind of preparation method of the recyclable fracturing fluid gelatinizer of amino acids, specifically comprises the following steps：
1）In the water that the polyethylene glycol of formula ratio and dispersant are sequentially added to formula ratio, 300r/min is at the uniform velocity stirred
5min, makes it be uniformly dispersed, and it is spare to obtain mixed liquor；
2）The powder of the modified xantham gum of formula ratio and gellan gum is crossed and obtains uniform powder with the sieving of 120 mesh respectively,
3）Modified xantham gum after sieving and gellan gum powder are added into step 1）Mixed liquor in, 500r/min is at the uniform velocity stirred
Mixing 0.5h makes it be uniformly dispersed；
4）The clay stabilizer of formula ratio is added into step 3）Mixed liquor in allocate uniform, then add the tune of formula ratio
Section agent and protective agent stir evenly.
Embodiment 1
A kind of preparation method of the recyclable fracturing fluid gelatinizer of amino acids, specifically comprises the following steps：
1）The polyethylene glycol of 10kg and the dispersant of 1kg is taken to sequentially add in the water of 75.6kg, 300r/min is at the uniform velocity stirred
5min, makes it be uniformly dispersed, and it is spare to obtain mixed liquor；
2）The powder of the modified xantham gum of 7kg and the gellan gum of 5kg is crossed and obtains uniform powder with the sieving of 120 mesh respectively
End,
3）The modified xantham gum of 7kg after sieving and 5kg gellan gums powder are added into step 1）Mixed liquor in, 500r/
Min, which at the uniform velocity stirs 0.5h, makes it be uniformly dispersed；
4）The clay stabilizer of 0.5kg is added into step 3）Mixed liquor in allocate uniform, then add the adjusting of 0.6kg
Agent and 0.3kg protective agents stir evenly.
The modified xantham gum, its preparation method are：By weight, by 20 parts of xanthans, 270 parts of solvent, catalysis
7 parts of agent is added in three mouthfuls of reaction bulbs equipped with reflux condensate device, be stirred at room temperature swelling 24 it is small when, then heat to 50
DEG C, 5 parts of modifying agent is slowly added to, when reaction 24 is small；By reaction product acetone precipitation, washing, unreacted modifying agent is removed
And catalyst, filtering；When drying 8 is small in vacuum drying oven under temperature 50 C, modified xantham gum is obtained；Wherein xanthans is flat
Average molecular weight is 500 × 104；Modifying agent is benzyl chloride；Catalyst is sodium hydroxide；Solvent is ethanol.
The gellan gum, its preparation method comprise the following steps：By her eastern algae pseudomonad (Pseudomonas elodea) concentrated through eggplant bottle strain access triangular flask culture, shaking table culture 18h at 28 DEG C, then accesses 300L seed tank cultures
Concentrate, 18~20h is cultivated at 28~30 DEG C, then force feed is cultivated 72h, be finally sent into 3000L fermentation tanks at identical temperature
72h is maintained at the identical temperature of 50t fermentation tanks, obtains gellan gum liquid；The fermentation medium is that mass ratio is 2% soybean slag, 2%
Sucrose and 96% water composition.The gellan gum can also directly be bought from market.
The clay stabilizer is potassium chloride；The conditioning agent is petroleum sodium sulfonate；The protective agent is No. 10
White oil；Dispersant is micron or nanometer grade silica, makes it easier to dissolve.The molecular weight of the polyethylene glycol is 1200
Ten thousand.
By the recyclable fracturing fluid gelatinizer of above-mentioned amino acids, it is used for Sulige gas field pressure break of reviving, dissolving by 4% and water proportioning
Time only needs 4min, and recovery of core permeability shears one up to 95%, using six fast viscosity apparatus with the shear rate of 170-1
Hour, viscosity was 50mPas, and residue tends to 0 after breaking gel, injury rate of the recyclable fracturing fluid which configures to permeability
Less than 2%, the recyclable fracturing fluid gelatinizer system temperature resistant capability of amino acids is up to 140 DEG C（Such as Fig. 1）.The common thickening in scene
System dissolution time is not more than 9min.
Through field application, the continuous pressing crack construction of five collecting well groups, than conventional pressure break using water wisely more than 50%, returns discharge opeing with water
Utilization rate 100%.
Embodiment 2
A kind of preparation method of the recyclable fracturing fluid gelatinizer of amino acids, specifically comprises the following steps：
1）The polyethylene glycol of 10kg and the dispersant of 1.5kg is taken to sequentially add in the water of 72.5kg, 300r/min is at the uniform velocity stirred
5min is mixed, it is uniformly dispersed, it is spare to obtain mixed liquor；
2）The powder of the modified xantham gum of 8kg and the gellan gum of 6kg is crossed and obtains uniform powder with the sieving of 120 mesh respectively
End,
3）The modified xantham gum of 8kg after sieving and 6kg gellan gums powder are added into step 1）Mixed liquor in, 500r/
Min, which at the uniform velocity stirs 0.5h, makes it be uniformly dispersed；
4）The clay stabilizer of 0.7kg is added into step 3）Mixed liquor in allocate uniform, then add the adjusting of 0.8kg
Agent and 0.5kg protective agents stir evenly.
The gellan gum, its preparation method comprise the following steps：By her eastern algae pseudomonad (Pseudomonas elodea) concentrated through eggplant bottle strain access triangular flask culture, shaking table culture 18h at 28 DEG C, then accesses 300L seed tank cultures
Concentrate, 18~20h is cultivated at 28~30 DEG C, then force feed is cultivated 72h, be finally sent into 3000L fermentation tanks at identical temperature
72h is maintained at the identical temperature of 50t fermentation tanks, obtains gellan gum liquid；The fermentation medium is that mass ratio is 2% soybean slag, 2%
Sucrose and 96% water composition.The gellan gum can also directly be bought from market.
The clay stabilizer is potassium chloride；The conditioning agent is petroleum sodium sulfonate；The protective agent is 10
Number white oil；Dispersant is micron or nanometer grade silica.The molecular weight of the polyethylene glycol is 12,000,000.
By the recyclable fracturing fluid gelatinizer of above-mentioned amino acids, it is used for Sulige gas field pressure break of reviving, dissolving by 4% and water proportioning
Time only needs 4min, and recovery of core permeability shears one up to 96%, using six fast viscosity apparatus with the shear rate of 170-1
Hour, viscosity was 51mPas, and residue tends to 0 after breaking gel, injury rate of the recyclable fracturing fluid which configures to permeability
Less than 2%, the recyclable fracturing fluid gelatinizer system temperature resistant capability of amino acids is up to 142 DEG C.The common thickening system dissolving in scene
Time is not more than 9min.
Through field application, the continuous pressing crack construction of five collecting well groups, than conventional pressure break using water wisely more than 50%, returns discharge opeing with water
Utilization rate 100%.
Embodiment 3
A kind of preparation method of the recyclable fracturing fluid gelatinizer of amino acids, specifically comprises the following steps：
1）The polyethylene glycol of 10kg and the dispersant of 2kg is taken to sequentially add in the water of 68.3kg, 300r/min is at the uniform velocity stirred
5min, makes it be uniformly dispersed, and it is spare to obtain mixed liquor；
2）The powder of the modified xantham gum of 10kg and the gellan gum of 7kg is crossed and obtains uniform powder with the sieving of 120 mesh respectively
End,
3）The modified xantham gum of 10kg after sieving and 7kg gellan gums powder are added into step 1）Mixed liquor in, 500r/
Min, which at the uniform velocity stirs 0.5h, makes it be uniformly dispersed；
4）The clay stabilizer of 1kg is added into step 3）Mixed liquor in allocate it is uniform, then add 1kg conditioning agent and
0.7kg protective agents stir evenly.
The gellan gum, its preparation method comprise the following steps：By her eastern algae pseudomonad (Pseudomonas elodea) concentrated through eggplant bottle strain access triangular flask culture, shaking table culture 18h at 28 DEG C, then accesses 300L seed tank cultures
Concentrate, 18~20h is cultivated at 28~30 DEG C, then force feed is cultivated 72h, be finally sent into 3000L fermentation tanks at identical temperature
72h is maintained at the identical temperature of 50t fermentation tanks, obtains gellan gum liquid；The fermentation medium is that mass ratio is 2% soybean slag, 2%
Sucrose and 96% water composition.The gellan gum can also directly be bought from market.
The clay stabilizer is potassium chloride；The conditioning agent is petroleum sodium sulfonate；The protective agent is 10
Number white oil；Dispersant is micron or nanometer grade silica.The molecular weight of the polyethylene glycol is 12,000,000.
By the recyclable fracturing fluid gelatinizer of above-mentioned amino acids, it is used for Sulige gas field pressure break of reviving, dissolving by 4% and water proportioning
Time only needs 4.5min, and recovery of core permeability is sheared up to 96% using six fast viscosity apparatus with the shear rate of 170-1
One hour viscosity is 52mPas, and residue tends to 0 after breaking gel, injury of the recyclable fracturing fluid which configures to permeability
Rate is less than 3%, and the recyclable fracturing fluid gelatinizer system temperature resistant capability of amino acids is up to 145 DEG C.The common thickening system in scene is molten
The solution time is not more than 9min.
Through field application, the continuous pressing crack construction of five collecting well groups, than conventional pressure break using water wisely more than 50%, returns discharge opeing with water
Utilization rate 100%.
Embodiment 4
Here is the comparative illustration on additive of the present invention ratio：
1#-3# is the number of thickening agent host agent, thickening agent assistant agent and dispersant in inventive formulation scope of the present invention in table 1
It is worth the additive prepared, 4# is same formula using the present invention, but thickening agent host agent, the ratio of thickening agent assistant agent be not in this hair
The additive situation of the preparation of bright formula rate scope：
System heat resistance and dissolution time when 1 formula using the present invention of table and ratio
It can be drawn from table 1, when formula using the present invention and ratio, its heat resistance and than not using this formula
It is high.
The relation of 2 thickener concentration of table and solution apparent viscosity, test condition are 30 DEG C, 7.34s-1.
The result shows that compared with unmodified xanthans, modified xantham gum has more preferable tackifying ability, the salt of its low concentration
Aqueous solution also has the apparent viscosity of higher.
Influence of 3 sodium chloride concentration of table to apparent viscosity
The result shows that compared with unmodified xanthans, modified xantham gum solutions display thickens behavior for obvious salt, has
More preferable anti-salt property, the thickening agent solution of high salt concentration (6.0g/dL) still have higher viscosity number.
The part that the present embodiment does not describe in detail belongs to the common knowledge of the industry, may search on the net, here not
Describe one by one.
Claims (4)
1. a kind of recyclable fracturing fluid gelatinizer of amino acids, it is characterized in that：It is formulated by following components：Modified xanthan
Glue 7-10%, gellan gum 5-7%, clay stabilizer 0.5-1%, conditioning agent 0.6-1%, protective agent 0.3-0.7%, polyethylene glycol 10%,
Dispersant 1~2%, surplus are water；Above-mentioned percentage is mass percent；
The modified xantham gum, its preparation method are：By weight, by 20 parts of xanthans, 270 parts of solvent, 7 parts of catalyst
Add equipped with reflux condensate device three mouthfuls of reaction bulbs in, be stirred at room temperature swelling 24 it is small when, then heat to 50 DEG C, delay
It is slow to add 5 parts of modifying agent, when reaction 24 is small；By reaction product acetone precipitation, washing, remove unreacted modifying agent and urge
Agent, filtering；When drying 8 is small in vacuum drying oven under temperature 50 C, modified xantham gum is obtained；The wherein average mark of xanthans
Son amount is 500 × 104；Modifying agent is benzyl chloride；Catalyst is sodium hydroxide；Solvent is ethanol；
The clay stabilizer is potassium chloride；The conditioning agent is petroleum sodium sulfonate；The protective agent is white for No. 10
Oil；Dispersant is micron or nanometer grade silica.
2. the recyclable fracturing fluid gelatinizer of a kind of amino acids according to claim 1, it is characterized in that：The knot is cold
Glue, its preparation method comprise the following steps：Her eastern algae pseudomonad is accessed triangular flask culture through eggplant bottle strain to concentrate, at 28 DEG C
Shaking table culture 18h, then accesses 300L seed tank cultures and concentrates, and cultivates 18~20h at 28~30 DEG C, then force feed is to 3000L
In fermentation tank, 72h is cultivated at identical temperature, is finally sent at the identical temperature of 50t fermentation tanks and maintains 72h, obtain gellan gum liquid；Institute
The fermentation medium stated is that mass ratio is 2% soybean slag, 2% sucrose and 96% water composition.
3. the recyclable fracturing fluid gelatinizer of a kind of amino acids according to claim 1, it is characterized in that：The poly- second two
The molecular weight of alcohol is 12,000,000.
4. a kind of preparation method of the recyclable fracturing fluid gelatinizer of amino acids according to claim 1, it is characterized in that：Tool
Body includes the following steps：
1）In the water that the polyethylene glycol of formula ratio and dispersant are sequentially added to formula ratio, 300r/min at the uniform velocity stirs 5min, makes
It is uniformly dispersed, and it is spare to obtain mixed liquor；
2）The powder of the modified xantham gum of formula ratio and gellan gum is obtained into uniform powder with the sieving of 120 mesh respectively；
3）Modified xantham gum after sieving and gellan gum powder are added into step 1）Mixed liquor in, 500r/min is at the uniform velocity stirred
0.5h makes it be uniformly dispersed；
4）The clay stabilizer of formula ratio is added into step 3）Mixed liquor in allocate uniform, then add the conditioning agent of formula ratio
Stirred evenly with protective agent.
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| CN104974738A (en) * | 2014-04-10 | 2015-10-14 | 中国石油化工股份有限公司 | Water-based gel fracturing fluid and application thereof |
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| CN102134283A (en) * | 2010-12-20 | 2011-07-27 | 成都理工大学 | Preparation method of associated modified xanthan gum |
| CN104508239A (en) * | 2012-06-29 | 2015-04-08 | 贝克休斯公司 | Fracturing fluids and methods for treating hydrocarbon-bearing formations |
| WO2015086808A1 (en) * | 2013-12-12 | 2015-06-18 | Omya International Ag | Improved gel stability |
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