CN104558404B - Hydrophobically associating polymer for shale gas exploitation - Google Patents
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Abstract
The invention relates to a hydrophobically associating polymer for shale gas exploitation and a preparation method thereof and an application of the hydrophobically associating polymer as a drag reducer in shale gas exploitation and is mainly used for solving the problem of low drag reduction rate of the polymers in the prior art. The hydrophobically associating polymer for shale gas exploitation is prepared from the following mixtures in parts by mass through free radical polymerization: a) 100 parts of acrylamide; b) 0-60 parts of free radical polymerization anion monomer; c) 0.1-60 parts of free radical polymerization hydrophobic monomer; and d) 200-2,000 parts of water; and the technical problem is solved relatively well by the technical scheme, and the hydrophobically associating polymer can be used as a drag reducer in shale gas exploitation.
Description
Technical field
The present invention relates to for the hydrophobic associated polymer of shale gas exploitation, its preparation method, and described hydrophobic association
Polymer application as drag reducer in shale gas exploitation.
Background technology
Increasingly in short supply with petroleum resources, energy security problem becomes increasingly conspicuous, and shale gas resource has become countries in the world energy
Source circle falls over each other the focus studied.At present, Chinese shale gas resources exploration is still in the exploration starting stage, and exploitation protects this
A little resources are the important topics that China's energy industry faces.Shale gas exploitation at present is usually used hydraulic fracturing technology, due to page
When rock air pressure splits, liquid displacement is very big, needs to add a certain amount of drag reducer such as hydroxypropyl guar gum, polyacrylamide in clear water
Amine etc., for reducing frictional resistance in pipeline for the liquid, improves construction effect.But the polymer matrix pressure break system of routine is due to containing
There are water-insoluble and colloid residue, easily cause shale reservoir grievous injury, fracturing fluid is unfavorable for after being cross-linked to form frozen glue stitching net
Formed, and the frictional resistance in pipeline can be increased, therefore restriction is brought to construction equipment.Abroad shale oil and gas reservoir is changed at present
Make, mainly adopt smooth aqueous systems.In order to increase dissolubility and dispersive property, it is outer for generally drag reducer being fabricated to mineral oil
The suspension of phase, the use of mineral oil considerably increases the difficulty returning discharge opeing process.Conventional hydroxypropyl guar gum is a kind of gala
Mannan, is easily degraded by microorganisms, and generally also needs to add a certain amount of antibacterial therefore in slippery water.The making of antibacterial
With bringing more serious environmental problem, making the process returning discharge opeing more complicated.Accordingly, it would be desirable to it is high to develop a kind of environmental protection
The again economic drag reducer of effect, thus reducing operation pressure, improves construction technology success rate and economic benefit.
Also in starting stage, Southwest Petrol University in terms of the domestic development in shale gas drag reducer, petrochina is natural
Gas limited company, petroleum works Institute for Research and Technology of petrochina Henan Oil Field branch company, petrochina northwest oilfield branch work
Journey Institute for Research and Technology, extends the mechanisms such as oil and has all carried out research work in terms of shale gas drag reducer, achieve certain
Progress.
A kind of preparation method of shale gas drag reducer of the patent report of Publication No. cn102977877a, by normal
The method introducing function monomer on the polyacrylamide of rule, improves the anti-shear performance of drag reducer, resistance-reducing yield can reach
70%；The patent of Publication No. cn102516975, cn103045226a and cn103010488a all reports smooth water type drag reduction
The preparation method of agent, but such drag reducer resistance-reducing yield is all than relatively low.
Content of the invention
One of the technical problem to be solved is the low problem of polymer resistance-reducing yield of prior art, provides one kind
For the hydrophobic associated polymer of shale gas exploitation, this hydrophobic associated polymer has the advantages that resistance-reducing yield is high.
The two of the technical problem to be solved are the systems of the described hydrophobic associated polymer of one of above-mentioned technical problem
Preparation Method.
The three of the technical problem to be solved are that the hydrophobic associated polymer described in one of above-mentioned technical problem exists
As the application of drag reducer in shale gas exploitation.
In order to solve one of above-mentioned technical problem, technical scheme is as follows: hydrophobic for shale gas exploitation is formed
Close polymer, obtained through radical polymerization by the mixture that following masses part represents:
A) 100 parts of acrylamide；
B) 0～60 part of radical polymerization anionic monomer；
C) 0.1～60 part of radical polymerization hydrophobic monomer；
D) 200～2000 parts of water.
In technique scheme, described radical polymerization anionic monomer preferably is selected from 2- acrylamido -2- methyl-prop sulphur
Acid, acrylic acid, methacrylic acid, vinylbenzenesulfonic acid, at least one in vinyl sulfonic acid.
In technique scheme, described radical polymerization hydrophobic monomer preferably is selected from anion hydrophobic monomer or cation hydrophobic
One of monomer；Described anion hydrophobic monomer has the (i) shown formula of formula；Described cation hydrophobic monomer has formula
(ii) shown formula；r1It is c4~c16Alkyl, m be selected from nh4Or any one in alkali metal；r3And r4It is independently selected from c1~c4
Alkyl, r2For c12~c22Alkyl, x be halogen, x more preferably chlorine；
(i)；(ii).
As most preferred technical scheme, described hydrophobic associated polymer, the mixture being represented by following masses part is through certainly
Obtained by base polymerization:
A) 100 parts of acrylamide；
B) 50～60 parts of 2- acrylamide-2-methylpro panesulfonic acid；
C) the (i) shown anion hydrophobic monomer of 0.1～2 part of formula, wherein r1For c8~c12Alkyl, m be selected from nh4Or alkali
Any one in metal；
D) 500～700 parts of water.
In above-mentioned most preferred technical scheme, the most preferably r1For c10Alkyl.
For solving the two of above-mentioned technical problem, technical scheme is as follows: the technical side of one of above-mentioned technical problem
The preparation method of the hydrophobic associated polymer described in case, includes following step successively:
A () adds water, acrylamide, radical polymerization anionic monomer, the hydrophobic list of radical polymerization in polymeric kettle
Body, stir formation solution；
B () adjusts the ph value of solution to 7 ~ 10, add radical polymerization initiator, cause 0.5 ~ 1 in 10 ~ 30 DEG C of temperature
Hour；
C () is polymerized 2 ~ 8 hours at a temperature of 40 ~ 60 DEG C, obtain aqueous gel hydrophobic associated polymer.
In technique scheme, described radical initiator is preferably redox initiator.
In technique scheme, described radical initiator consumption preferably accounts for the 0.003～0.5% of described total weight of monomer.
In technique scheme, described radical initiator preferably by Ammonium persulfate. or alkali metal persulphate extremely
Few a kind of oxidant and in alkali metal sulfite, alkali metal bisulfite or alkali metal thiosulfate at least one
Plant reducing agent composition.
In technique scheme, preferably also comprise the steps: after described step (c)
D () is dried, obtain the hydrophobic associated polymer of dry state.
In technique scheme, the temperature that described step (d) is dried is preferably 80～95 DEG C.
For solving the three of above-mentioned technical problem, technical scheme is as follows: dredging described in one of above-mentioned technical problem
The application as drag reducer in shale gas exploitation of water association polymer.
The drag reduction that described hydrophobic associated polymer is preferably made into 0.005 ~ 0.2wt% by the method for for example described application is water-soluble
Liquid huge discharge is rapidly injected bottom, can effectively reduce the circulation friction pressure in operation.
The key problem in technology of the present invention is to employ hydrophobic monomer in acrylamide copolymer, and drag reduction agent concentration of the present invention is
During 0.005 ~ 0.2wt%, resistance-reducing yield can reach more than 76%, and the acrylamide copolymer resistance-reducing yield being provided without hydrophobic monomer is only
60%, achieve preferable technique effect.
Specific embodiment
[embodiment 1]
1st, the synthesis of polymer
It is initially charged 650g deionized water in polymeric kettle, add 100g acrylamide (am), 54g 2- acrylamido -2-
Methyl propane sulfonic acid (amps), 1.5g 2- acrylamido dodecyl sodium sulfate (naamc12S), stir to being completely dissolved, use
It is 9 that naoh adjusts ph value, and starts to be passed through high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then sequentially adds
The persulfate aqueous solution 15.5g of the aqueous solution of sodium bisulfite 15.5g of 0.1wt% and 0. 1wt%, as initiator, continues logical
Seal after nitrogen 30min.After 1 hour, reaction temperature is gradually increased to 45 DEG C, reaction obtains aqueous gel polymerization after 3 hours
Product, cuts after glue forced air drying 1.5h under 90 c, being smashed with pulverizer sieves obtains the hydrophobic associated polymer of dry state.
2nd, the preparation of drag reducer
In 10l water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical agitation 200rpm, obtain
Drag reduction agent solution to 0.01wt%.
3rd, the performance test of drag reducer
In addition to drag reduction agent solution flows through 1/2 inch of pipe with 10l/min flow, other is according to sy/t 6376-2008
In fracturing fluid general technical specifications, the method for 7.13.1 carries out friction-reducing agent of fracturing fluid interior resistance-reducing performance evaluation.Clear water is loaded many
Function flow circuits instrument, measures clear water and passes through stable pressure reduction δ during pipelinep 1；Measure above-mentioned fracturing fluid after the same method
Friction reducer flows through stable pressure reduction δ during pipelinep 2, by formula (1) calculating resistance-reducing yield η:
(1)
Result sees attached list 1.
Inventors herein have recognized that, when described hydrophobic associated polymer, the mixture being represented by following masses part is through certainly
When being obtained by base polymerization, resistance reducing effect is best: a) 100 parts of acrylamide；B) 50～60 parts of 2- acrylamido -2- methyl
Propane sulfonic acid；C) the (i) shown anion hydrophobic monomer of 0.1～2 part of formula, wherein r1For c8~c12Alkyl, m be selected from nh4Or alkali
Any one in metal；D) 500～700 parts of water.This also can from embodiment 1 and other embodiments and comparative example on year-on-year basis
Intuitively find out.
[embodiment 2]
1st, the synthesis of polymer
It is initially charged 650g deionized water in a kettle., add 100g acrylamide (am), 60g2- acrylamido -2-
Methyl propane sulfonic acid (amps), 15g 2- acrylamido dodecyl sodium sulfate (naamc12S), stir to being completely dissolved, use
It is 9 that naoh adjusts ph value, and starts to be passed through high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then sequentially adds 0.
Persulfate aqueous solution 17.5 g of the aqueous solution of sodium bisulfite 17.5g of 1wt% and 0. 1wt%, as initiator, continues logical nitrogen
Seal after gas 30min.After 1 hour, reaction temperature is gradually increased to 45 DEG C, reaction obtained gel polymerizate after 3 hours, cut
After glue under 90 c forced air drying 1.5h, smash to sieve with pulverizer and obtain hydrophobically associating polymers.
2nd, the preparation of drag reducer
In 10l water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical agitation 200rpm, obtain
Drag reduction agent solution to 0.01wt%.
3rd, the performance test of drag reducer
Method of testing is same as Example 1, and result sees attached list 1.
[embodiment 3]
1st, the synthesis of polymer
It is initially charged 650g deionized water in a kettle., add 100g acrylamide (am), 55.5g2- acrylamido ten
Dialkyl sulfonates (naamc12S), stir to being completely dissolved, adjusting ph value with naoh is 9, and starts to be passed through high pure nitrogen,
After 30min, temperature in the kettle is down to 15 DEG C, then sequentially adds the aqueous solution of sodium bisulfite 10g and 0. 1wt% of 0.1wt%
Persulfate aqueous solution 10g, as initiator, seals after continuing logical nitrogen 30min.After 1 hour, reaction temperature is gradually increased to 45
DEG C, reaction obtained gel polymerizate after 3 hours, cuts after glue forced air drying 1.5h under 90 c, is smashed with pulverizer and sieve
Obtain hydrophobic associated polymer.
2nd, the preparation of drag reducer
In 10l water, add 1g hydrophobically associating polymers, under the speed of mechanical agitation 200rpm, stir 20 points
Clock, obtains the drag reduction agent solution of 0.01wt%.
3rd, the performance test of drag reducer
Method of testing is same as Example 1, and result sees attached list 1.
[embodiment 4]
1st, the synthesis of polymer
Be initially charged 650g deionized water in a kettle., add 100g acrylamide (am), 40g methacrylic acid (maa),
12g solution property (c18Dmaa), stir to being completely dissolved, adjusting ph value with naoh is 9, and starts
It is passed through high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then sequentially add the aqueous solution of sodium bisulfite of 0.1wt%
The persulfate aqueous solution 15.2g of 15.2g and 0.1wt%, as initiator, seals after continuing logical nitrogen 30min.Will after 1 hour
Reaction temperature is gradually increased to 45 DEG C, and reaction obtained gel polymerizate after 3 hours, cut forced air drying under 90 c after glue
1.5h, smashes to sieve with pulverizer and obtains hydrophobic associated polymer.
2nd, the preparation of drag reducer
In 10l water, add 1g hydrophobically associating polymers, under the speed of mechanical agitation 200rpm, stir 20 points
Clock, obtains the drag reduction agent solution of 0.01wt%.
3rd, the performance test of drag reducer
Method of testing is same as Example 1, and result sees attached list 1.
[embodiment 5]
1st, the synthesis of polymer
It is initially charged 650g deionized water in a kettle., add 100g acrylamide (am), 30g acrylic acid (aa), 9g ten
Six alkyl dimethyl allyl ammonium chloride (c16Dmaa), stir to being completely dissolved, adjusting ph value with naoh is 9, and starts to be passed through
Temperature in the kettle is down to 15 DEG C after 30min by high pure nitrogen, then sequentially adds the aqueous solution of sodium bisulfite 13.9g of 0.1wt%
With the persulfate aqueous solution 13.9g of 0.1wt% as initiator, seal after continuing logical nitrogen 30min.Temperature will be reacted after 1 hour
Degree is gradually increased to 45 DEG C, and reaction obtained gel polymerizate after 3 hours, cuts after glue forced air drying 1.5h under 90 c, uses powder
Broken machine is smashed to sieve and is obtained hydrophobic associated polymer.
2nd, the preparation of drag reducer
In 10l water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical agitation 200rpm, obtain
Drag reduction agent solution to 0.01wt%.
3rd, the performance test of drag reducer
Method of testing is same as Example 1, and result sees attached list 1.
[embodiment 6]
1st, the synthesis of polymer
It is initially charged 650g deionized water in a kettle., add 100g acrylamide (am), 20g vinylbenzenesulfonic acid
(vbs), 6g2- acrylamido myristyl sodium sulfonate (naamc14S) stir to being completely dissolved, adjusting ph value with naoh is 9,
And start to be passed through high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then sequentially adds the sodium sulfite water of 0.1wt%
The persulfate aqueous solution 12.3g of solution 12.3g and 0.1wt%, as initiator, seals after continuing logical nitrogen 30min.1 hour
Afterwards reaction temperature is gradually increased to 45 DEG C, reaction obtained gel polymerizate after 3 hours, after cutting glue, air blast is done under 90 c
Dry 1.5h, smashes to sieve with pulverizer and obtains hydrophobic associated polymer.
2nd, the preparation of drag reducer
In 10l water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical agitation 200rpm, obtain
Drag reduction agent solution to 0.01wt%.
3rd, the performance test of drag reducer
Method of testing is same as Example 1, and result sees attached list 1.
[embodiment 7]
1st, the synthesis of polymer
It is initially charged 650g deionized water in a kettle., add 100g acrylamide (am), 10g acrylic acid (aa), 3g 2-
Acrylamido ten sodium alkyl sulfonate (naamc10S), stir to being completely dissolved, adjusting ph value with naoh is 9, and starts to be passed through height
Temperature in the kettle is down to 15 DEG C after 30min by pure nitrogen gas, then sequentially add 0.1wt% aqueous solution of sodium bisulfite 11.3g and
The persulfate aqueous solution 11.3g of 0.1wt%, as initiator, seals after continuing logical nitrogen 30min.By reaction temperature after 1 hour
It is gradually increased to 45 DEG C, reaction obtained gel polymerizate after 3 hours, cut after glue forced air drying 1.5h under 90 c, with pulverizing
Machine is smashed to sieve and is obtained hydrophobic associated polymer.
2nd, the preparation of drag reducer
In 10l water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical agitation 200rpm, obtain
Drag reduction agent solution to 0.01wt%.
3rd, the performance test of drag reducer
Method of testing is same as Example 1, and result sees attached list 1.
[embodiment 8]
1st, the synthesis of polymer
It is initially charged 650g deionized water in a kettle., add 100g acrylamide (am), 5g2- acrylamido -2- first
Base propane sulfonic acid (amps), 1g 2- acrylamido octyl sodium sulfonate (naamc8S), stir to being completely dissolved, adjusted with naoh
Ph value is 9, and starts to be passed through high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then sequentially adds the sulfurous of 0.1wt%
The persulfate aqueous solution 10.6g of sour hydrogen sodium water solution 10.6g and 0.1wt%, as initiator, seals after continuing logical nitrogen 30min
Mouthful.After 1 hour, reaction temperature is gradually increased to 45 DEG C, reaction obtained gel polymerizate after 3 hours, cuts after glue in 90 c
Lower forced air drying 1.5h, smashes to sieve with pulverizer and obtains hydrophobic associated polymer.
2nd, the preparation of drag reducer
In 10l water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical agitation 200rpm, obtain
Drag reduction agent solution to 0.01wt%.
3rd, the performance test of drag reducer
Method of testing is same as Example 1, and result sees attached list 1.
[comparative example]
1st, the synthesis of polymer
Be initially charged 650g deionized water in a kettle., add 100g acrylamide (am), 55.5g 2- acrylamido-
2- methyl propane sulfonic acid (amps), stirs to being completely dissolved, adjusting ph value with naoh is 9, and starts to be passed through high pure nitrogen, 30min
Afterwards temperature in the kettle is down to 15 DEG C, then sequentially adds the over cure of aqueous solution of sodium bisulfite 15.4g and 0.1wt% of 0.1wt%
Sour aqueous solutions of potassium 15.4g, as initiator, seals after continuing logical nitrogen 30min.After 1 hour, reaction temperature is gradually increased to 45
DEG C, reaction obtained gel polymerizate after 3 hours, cuts after glue forced air drying 1.5h under 90 c, is smashed with pulverizer and sieve
Obtain acrylamide copolymerized polymer.
2nd, the preparation of drag reducer
In 10l water, add 1g acrylamide copolymerized polymer, under the speed of mechanical agitation 200rpm, stir 20 points
Clock, obtains the drag reduction agent solution of 0.01wt%.
3rd, the performance test of drag reducer
Method of testing is same as Example 1, and result sees attached list 1.
Inventors herein have recognized that, in terms of improving resistance-reducing yield, amps and the (i) shown anion hydrophobic monomer of formula
(wherein r1For c8~c12Alkyl, m be selected from nh4Or any one in alkali metal) there is synergism.From comparative example, embodiment
1 and embodiment 3 on year-on-year basis in can also intuitively find out.
Table 1 embodiment and comparative example resistance-reducing yield result
Claims (8)
1. it is used for the hydrophobic associated polymer of shale gas exploitation, the mixture being represented by following masses part is through radical polymerization
:
A) 100 parts of acrylamide；
B) 50～60 parts of 2- acrylamide-2-methylpro panesulfonic acid；
C) the anion hydrophobic monomer shown in 0.1～2 part of formula (i), wherein r1For c8～c12Alkyl, m be selected from nh4Or alkali gold
Any one in genus；
D) 500～700 parts of water.
2. the preparation method of the hydrophobic associated polymer described in claim 1, includes following step successively:
A () adds the anion shown in water, acrylamide, 2- acrylamide-2-methylpro panesulfonic acid, formula (i) in polymeric kettle
Hydrophobic monomer, stir formation solution；
B () adjusts the ph value of solution to 7～10, add radical initiator, cause 0.5～1 hour in 10～30 DEG C of temperature；
C () is polymerized 2～8 hours at a temperature of 40～60 DEG C, obtain aqueous gel hydrophobic associated polymer.
3. the preparation method of hydrophobic associated polymer according to claim 2, is characterized in that described radical initiator is
Redox initiator.
4. the preparation method of hydrophobic associated polymer according to claim 2, is characterized in that described radical initiator is used
Measure for account for polymerized monomer gross weight 0.003～0.5%.
5. the preparation method of hydrophobic associated polymer according to claim 3, it is characterized in that described radical initiator by
Selected from least one of Ammonium persulfate. or alkali metal persulphate oxidant with selected from alkali metal sulfite, alkali metal sulfurous acid
At least one reducing agent composition in hydrogen salt or alkali metal thiosulfate.
6. the preparation method of hydrophobic associated polymer according to claim 2, it is characterized in that also including after step (c) as
Lower step:
D () is dried, obtain the hydrophobic associated polymer of dry state.
7. the preparation method of hydrophobic associated polymer according to claim 6, is characterized in that the temperature that step (d) is dried is
80～95 DEG C.
8. the application as drag reducer in shale gas exploitation of the hydrophobic associated polymer described in claim 1.
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| CN108250357A (en) * | 2018-01-26 | 2018-07-06 | 重庆科技学院 | A kind of method that no soap method prepares cation-type hydrophobic association type polyacrylamide |
| CN109135714A (en) * | 2018-09-17 | 2019-01-04 | 佛山市禅城区诺高环保科技有限公司 | A kind of preparation method of long-acting antiseptic resistance-reducing agent |
| CN112778455A (en) * | 2020-12-30 | 2021-05-11 | 宁波锋成先进能源材料研究院有限公司 | Temperature-resistant salt-resistant hydrophobic association polymer and preparation method and application thereof |
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| CN102977877B (en) * | 2012-12-04 | 2014-08-06 | 西南石油大学 | Drag reducer for shale gas fracture and preparation method of drag reducer |
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