CN104231156A - Clean fracturing fluid thickening agent and preparation method thereof - Google Patents
Clean fracturing fluid thickening agent and preparation method thereof Download PDFInfo
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- CN104231156A CN104231156A CN201410482758.3A CN201410482758A CN104231156A CN 104231156 A CN104231156 A CN 104231156A CN 201410482758 A CN201410482758 A CN 201410482758A CN 104231156 A CN104231156 A CN 104231156A
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Abstract
The invention discloses a clean fracturing fluid thickening agent and a preparation method thereof. The thickening agent is prepared by mixing methacrylamide, 2-acrylamide-2-methyl-1-moropholino ethanesulfonic acid salt, styrene, acryloyloxyethyl trimethyl ammonium chloride, sodium p-styrenesulfonate and N-vinyl-pyrrolidone in solvent water, adjusting the pH value of mixed reaction liquid to be 8-9, adding an initiator for initiating a free radical under the protection of nitrogen and then performing polymerization according to a microwave method. The clean fracturing fluid thickening agent has the advantages of high shearing resistance, high viscosity, high carrying property and the like; furthermore, the clean fracturing fluid thickening agent is short in liquid mixing time, high in dispersion property and high in swelling speed, and can realize simultaneously liquid mixing and construction.
Description
Technical field
The invention belongs to conventional gas and oil to hide and unconventionaloil pool Tibetan fracturing technique field, particularly a kind of clean fracturing fluid thickener and preparation method thereof.
Background technology
Fracturing yield increasing technology is one of the most effective well stimulation technology in hydrocarbon-bearing pool recovery process, thickening material mainly vegetable jelly and the derivative thereof that current pressure break uses, exists that dissolving speed is slow, insolubles content is high, residue is many and have the problems such as injury to reservoir after broken glue.In addition, traditional fracturing technology also exists the problems such as setup time length, residual liquid discharge contaminate environment, and especially preparation is successively carried out in two steps with construction, can not realize the two real-time matching, often causes passive and fracturing liquid waste of constructing.
At present, studies in China Low Damage polymer fracturing fluid system starts to walk, but not yet finds and a kind ofly have high shearing, strong inhibition, high viscosity, the good feature of environmental protection polymer viscosifier taken without advantages such as residues after grittiness, broken glue.Make thickening material thermostability poor, can not clay stabilization be kept, make the crack of producing can not reach required width and the degree of depth.
Summary of the invention
The object of the present invention is to provide thickening material of a kind of clean fracturing fluid and preparation method thereof, shear resistant is good, viscosity is high, take the advantages such as grittiness is good to adopt the clean fracturing fluid thickener prepared by the method to have, and this clean fracturing fluid thickener liquid preparation time is short, thickening material good dispersity, swelling rate are fast, can realize the construction of dosing limit, limit.
To achieve these goals, clean fracturing fluid thickener of the present invention, be made up of the raw material of following weight percent:
The preparation method of this clean fracturing fluid thickener comprises following key step:
(1) configuring mixed reaction solution: mixed by the raw material of above-mentioned weight percent, wherein, water is solvent, through stirring, other each component being dissolved in the water completely;
(2) adjust the pH value of solution to pH=8-9, solution temperature controls at 10-15 DEG C, adds initiator and cause generation free radical under nitrogen protection;
(3) temperature is increased to room temperature, within 2-3 minute, is mixed, then take out with microwave method 500W heating, under air-tight state (i.e. isolated air), be warming up to 60 DEG C, and be incubated 4 hours, resulting polymers is that gel is block;
(4) polymkeric substance obtained in step (3) carried out purify, dry, granulation, pulverize, namely obtain clean fracturing fluid thickener.
Preferably, mixed reaction solution pH=8-9 (namely mixed reaction solution is weakly alkaline) is regulated with sodium hydroxide solution in described step (2).
Preferably, the middle nitrogen protection of described step (2) is for passing into nitrogen 30min.
Preferably, in described step (2), initiator causes the time is 15-20min.
In the course of the polymerization process, described initiator comprises azo and oxidation-reduction system two class initiator.Wherein, azo-initiator selects at least one in azo diisobutyl amidine hydrochloride, Diisopropyl azodicarboxylate; In oxidation-reduction system, at least one in ammonium persulphate, Potassium Persulphate selected by oxygenant, and at least one in sodium formaldehyde sulphoxylate, sodium bisulfite then selected by reductive agent.
Described initiator amount adds 0.1-0.3g initiator in often liter of mixed reaction solution.
In the elicitation procedure of step (2), after adding initiator 15-20min, if see that temperature raises, then illustrate and cause successfully, create free radical, the reaction of step (3) can be continued, otherwise need to add initiator and again cause.
The clean fracturing fluid thickener of above-mentioned preparation is raw materials used, comprising: Methacrylamide (AAM), 2-acrylamide-2-methyl isophthalic acid-propane sulfonate (AMPS), vinylbenzene (ST), acrylyl oxy-ethyl-trimethyl salmiac (DAC), Sodium styrene sulfonate (BNS) and-vinyl-pyrrolidone (NVP).
Relevant monomer structure is as follows:
The clean fracturing fluid thickener that preparation method of the present invention obtains is white powder.
When the mass concentration of described thickening material in clean fracturing fluid is 0.3%-1%, waterfrac treatment effect is best, can be used as fracturing liquid core additive and uses, not only can improve output, cost-saving, and the construction requirement of on-the-spot mixture continuously can be met, reach volume increase object.
Evaluation at present to fracturing liquid technology, whether its visco-elasticity of primary evaluation meets pressing crack construction needs.In general, when clean fracturing fluid hang the viscosity after sand reach 25mPas time, be and there is excellent suspension and prop-carrying capacity.And this clean fracturing fluid thickener is when in fracturing liquid, mass concentration is 0.5%, viscosity at ambient temperature is 10-20mPas; After high-speed stirring (5000 revs/min) 120min, viscosity at ambient temperature 33-36mPas; When temperature more than 100 DEG C, when shearing 120min, product viscosity is 50-70mPas.
Therefore, compared with prior art, this clean fracturing fluid thickener has that shear resistant is good, viscosity is high, take the good advantage of grittiness, and this clean fracturing fluid thickener liquid preparation time is short, and thickening material good dispersity, swelling rate are fast, can realize the construction of dosing limit, limit.
Embodiment
Below in conjunction with embodiment, foregoing invention content of the present invention is described in further detail.But this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and customary means, make various replacement and change, all should comprise within the scope of the invention.
The technical scheme that the present invention specifically implements is:
Embodiment 1
In reaction solution, the weight percent of each monomer and water is: AAM:AMPS:ST:DAC:BNS:NVP: water=10:3:10:15:1:5:56.
(1) mixed reaction solution is prepared: in 3000mL beaker, add distilled water 560g, add monomer A AM100g, monomer A MPS 30g, monomer ST 100g, monomer DAC 150g, monomers B NS 10g, monomer NVP 50g, be stirred to and dissolve completely;
(2) regulate mixed reaction solution pH value to pH=8 with sodium hydroxide, and solution temperature is maintained 15 DEG C.Top blast nitrogen deoxygenation in 30 minutes, adds initiator (adding Potassium Persulphate 0.05g, sodium bisulfite 0.06g, Diisopropyl azodicarboxylate 0.06g, sodium formaldehyde sulphoxylate 0.05g in often liter of mixed reaction solution), causes and produces free radical in 20 minutes;
(3) temperature is elevated to room temperature, heats with microwave method moderate heat (500W) and mixed for 2 minutes, heat up under then taking out air tight condition, be incubated 4 hours;
(4) obtained colloid carried out purify, dry, granulation, be crushed to 50 orders, obtain product clean fracturing fluid thickener.
This product appearance is white powder, and when in clean fracturing fluid, mass concentration is 0.5%, viscosity at ambient temperature 16mPas, under normal temperature after outstanding sand 120min, viscosity is 33mPas.
Embodiment 2
In reaction solution, the weight percent of each monomer and water is: AAM:AMPS:ST:DAC:BNS:NVP: water=15:1:15:10:2:3:54.
(1) mixed reaction solution is prepared: in 3000mL beaker, add distilled water 540g, add monomer A AM150g, monomer A MPS 10g, monomer ST 150g, monomer DAC 100g, monomers B NS 20g, monomer NVP 30g, be stirred to and dissolve completely;
(2) regulate mixed reaction solution pH value to pH=9 with sodium hydroxide, and solution temperature is maintained 15 DEG C.Top blast nitrogen deoxygenation in 30 minutes, add initiator (adding ammonium sulfate 0.03g, azo diisobutyl amidine hydrochloride 0.08g, Diisopropyl azodicarboxylate 0.03g, sodium formaldehyde sulphoxylate 0.08g in often liter of mixed reaction solution), cause and produce free radical in 20 minutes;
(3) temperature is elevated to room temperature, heats with microwave method moderate heat (500W) and mixed for 3 minutes, heat up under then taking out air tight condition, be incubated 4 hours;
(4) obtained colloid carried out purify, dry, granulation, be crushed to 50 orders, obtain product clean fracturing fluid thickener.
This product appearance is white powder, and when in clean fracturing fluid, mass concentration is 0.5%, viscosity at ambient temperature 19mPas, under normal temperature after outstanding sand 120min, viscosity is 36mPas.
Embodiment 3
In reaction solution, the weight percent of each monomer and water is: AAM:AMPS:ST:DAC:BNS:NVP: water=5:5:10:20:1:4:55.
(1) mixed reaction solution is prepared: in 3000mL beaker, add distilled water 550g, add monomer A AM50g, monomer A MPS 50g, monomer ST 100g, monomer DAC 200g, monomers B NS 10g, monomer NVP40g, be stirred to and dissolve completely;
(2) regulate mixed reaction solution pH value to pH=8 with sodium hydroxide, and solution temperature is maintained 15 DEG C.Top blast nitrogen deoxygenation in 30 minutes, add initiator (adding ammonium sulfate 0.07g, azo diisobutyl amidine hydrochloride 0.04g, Diisopropyl azodicarboxylate 0.07g, sodium formaldehyde sulphoxylate 0.04g in often liter of mixed reaction solution), cause and produce free radical in 18 minutes;
(3) temperature is elevated to room temperature, heats with microwave method moderate heat (500W) and mixed for 2 minutes, heat up under then taking out air tight condition, be incubated 4 hours;
(4) obtained colloid carried out purify, dry, granulation, be crushed to 50 orders, obtain product clean fracturing fluid thickener.
This product appearance is white powder, and when in clean fracturing fluid, mass concentration is 0.5%, viscosity at ambient temperature 15mPa.s, under normal temperature after outstanding sand 120min, viscosity is 33mPas.
Embodiment 4
In reaction solution, the weight percent of each monomer and water is: AAM:AMPS:ST:DAC:BNS:NVP: water=10:5:15:10:2:2:56.
(1) mixed reaction solution is prepared: in 3000mL beaker, add distilled water 560g, add monomer A AM100g, monomer A MPS 50g, monomer ST 150g, monomer DAC 100g, monomers B NS 20g, monomer NVP 20g, be stirred to and dissolve completely;
(2) regulate mixed reaction solution pH value to pH=9 with sodium hydroxide, and solution temperature is maintained 15 DEG C.Top blast nitrogen deoxygenation in 30 minutes, add initiator (adding Potassium Persulphate 0.06g, azo diisobutyl amidine hydrochloride 0.08g, sodium bisulfite 0.06g, sodium formaldehyde sulphoxylate 0.08g in often liter of mixed reaction solution), cause and produce free radical in 15 minutes;
(3) temperature is elevated to room temperature, heats with microwave method moderate heat (500W) and mixed for 2.5 minutes, heat up under then taking out air tight condition, be incubated 4 hours;
(4) obtained colloid carried out purify, dry, granulation, be crushed to 50 orders, obtain product clean fracturing fluid thickener.
This product appearance is white powder, and when in clean fracturing fluid, mass concentration is 0.5%, viscosity at ambient temperature 18mPas, under normal temperature after outstanding sand 120min, viscosity is 36mPas.
This clean fracturing fluid thickener adds in fracturing liquid when carrying out dosing, and its liquid preparation time is short, and good dispersity, swelling rate are fast, occurs without water-insoluble residue, can meet the requirement constructed in dosing limit, limit.
When thickening material prepared by the present invention mass concentration in clean fracturing fluid is 0.3%-1%, waterfrac treatment effect is best.In practice of construction, from the viewpoint of its performance and cost two, the add-on of general thickening material in fracturing liquid is 0.5% (mass concentration).When adding in clean fracturing fluid; Thickening material is when in fracturing liquid, mass concentration is 0.5%, and viscosity at ambient temperature is 15-19mPas, after high-speed stirring (5000 revs/min) 120min, viscosity at ambient temperature 33-36mPas, visible, can stable viscosity be kept in certain hour, can hang sand under normal temperature, effect is better than guanidine rubber cement liquid; When temperature more than 100 DEG C, when shearing 120min, product viscosity is 50-70mPas, as seen under the high temperature conditions, still has good anti-shear performance.
Claims (6)
1. a clean fracturing fluid thickener, is characterized in that, is made up of the raw material of following weight percent:
2. a preparation method for clean fracturing fluid thickener described in claim 1, is characterized in that, comprises the steps:
(1) configuring mixed reaction solution: mixed by the raw material of above-mentioned weight percent, wherein, water is solvent, through stirring, other each component being dissolved in the water completely;
(2) adjust the pH value of solution to 8-9, solution temperature controls at 10-15 DEG C, adds multiple initiator and cause generation free radical under nitrogen protection;
(3) temperature is increased to room temperature, within 2-3 minute, is mixed with microwave method 500W heating, then take out, under sealed state, be warming up to 60 DEG C, and be incubated 4 hours, obtain gel piece shaped polymer;
(4) polymkeric substance obtained in step (3) carried out purify, dry, granulation, pulverize, namely obtain clean fracturing fluid thickener.
3. the preparation method of clean fracturing fluid thickener according to claim 2, is characterized in that, in described step (2), nitrogen protection is for passing into nitrogen 30min.
4. the preparation method of clean fracturing fluid thickener according to claim 2, is characterized in that, in described step (2), initiator causes the time is 15-20min.
5. the preparation method of clean fracturing fluid thickener according to claim 2, it is characterized in that, described initiator comprises azo-initiator and oxidation-reducting system initiator.
6. the preparation method of clean fracturing fluid thickener according to claim 2, is characterized in that, the total consumption of described initiator is for adding 0.1-0.3g initiator in often liter of mixed reaction solution and described multiple initiator adds with arbitrary proportion.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105837720A (en) * | 2016-04-01 | 2016-08-10 | 孙安顺 | Resin filler for fracturing and its preparation method |
| CN107759738A (en) * | 2016-08-17 | 2018-03-06 | 中国石油化工股份有限公司 | A kind of water-soluble hot increasing stick copolymer, preparation method and application |
| US9932517B1 (en) * | 2017-04-06 | 2018-04-03 | China University Of Petroleum (East China) | Polymer and preparation method thereof, and viscosified acid fluid |
| CN111607032A (en) * | 2019-02-25 | 2020-09-01 | 中国石油天然气股份有限公司 | Thickening agent, preparation method and application thereof |
| CN114057933A (en) * | 2020-07-30 | 2022-02-18 | 中石化石油工程技术服务有限公司 | Temperature-resistant and salt-resistant flow type regulator and solid-free anti-pollution drilling fluid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1995270A (en) * | 2006-11-15 | 2007-07-11 | 北京希涛技术开发有限公司 | Densifier for aqueous breakdown fluid and its production method |
-
2014
- 2014-09-19 CN CN201410482758.3A patent/CN104231156A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1995270A (en) * | 2006-11-15 | 2007-07-11 | 北京希涛技术开发有限公司 | Densifier for aqueous breakdown fluid and its production method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105837720A (en) * | 2016-04-01 | 2016-08-10 | 孙安顺 | Resin filler for fracturing and its preparation method |
| CN107759738A (en) * | 2016-08-17 | 2018-03-06 | 中国石油化工股份有限公司 | A kind of water-soluble hot increasing stick copolymer, preparation method and application |
| US9932517B1 (en) * | 2017-04-06 | 2018-04-03 | China University Of Petroleum (East China) | Polymer and preparation method thereof, and viscosified acid fluid |
| CN111607032A (en) * | 2019-02-25 | 2020-09-01 | 中国石油天然气股份有限公司 | Thickening agent, preparation method and application thereof |
| CN111607032B (en) * | 2019-02-25 | 2022-08-05 | 中国石油天然气股份有限公司 | Thickening agent, preparation method and application thereof |
| CN114057933A (en) * | 2020-07-30 | 2022-02-18 | 中石化石油工程技术服务有限公司 | Temperature-resistant and salt-resistant flow type regulator and solid-free anti-pollution drilling fluid |
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Application publication date: 20141224 |