CN102181008A - Water absorption resin for well repair and leaking stoppage and synthesis method thereof - Google Patents
Water absorption resin for well repair and leaking stoppage and synthesis method thereof Download PDFInfo
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Abstract
The invention relates to water absorption resin for well repair and leaking stoppage. The water absorption resin is prepared by the following synthesis steps of: a, mixing 10 to 15 percent of 2-acrylamide-2-methylpropanesulfonic acid, 30 to 45 percent of acrylamide, 0.2 to 0.5 percent of N,N-methylenebisacrylamide and deionized water in a weight ratio with stirring to form a mixture, wherein the stirring time is 5 to 10 minutes and the stirring temperature is 30 to 50 DEG C; b, putting the prepared mixture into a polymerization reaction kettle, stirring the mixture, introducing nitrogen for 30 minutes to displace air in the polymerization reaction kettle, simultaneously heating the polymerization reaction kettle to the temperature of between 40 and 50 DEG C, then adding 0.03 to 0.08 weight percent of persulfate initiator into the mixture, performing polymerization reaction on the mixture to generate the water absorption resin, and preserving heat for at least 6 hours after the polymerization reaction starts; and c, drying the prepared water absorption resin at the temperature of not more than 120 DEG C for 24 hours till complete drying, and crushing the dried water absorption resin into granules with a diameter of 0.5 to 40 millimeters to obtain the water absorption resin for well repair and leaking stoppage.
Description
Invention field
The present invention relates to a kind of water-absorbing resin, particularly a kind of well workover leak stopping water-absorbing resin the invention still further relates to the synthetic method of described well workover leak stopping with water-absorbing resin.
Background technology
The oil field is in recovery process, because the effect that waterflood flush or resident fluid wash away, the formation cementation thing is damaged easily, and zone permeability and pore throat radius are further increased, form " macropore " and the high infiltration band on stratum, the workover fluid leakage phenomena often takes place in workover treatment.The leakage of workover fluid has not only increased the consumption of workover fluid, cause workover treatment normally to carry out, but also can cause such as clay swelling in the reservoir, it is quick and fine migration takes place that speed appears in the sandstone reservoir of poor diagenetic grade, non-cementing properties and weak cementing properties, and formation contaminant such as reservoir rock wettability modification, influence the oil offtake after the workover treatment.
In order to overcome the above problems, in workover treatment, can adopt patching materials to prevent the leakage of workover fluid usually.Shutoff after the water-absorbent that water-absorbing resin had, snappiness and the extruding makes it to become the appropriate materials of well workover leak stopping.Present existing acrylic acid or the like water-absorbing resin heat and salinity tolerance performance, chemical stability and ageing resistance under the reservoir condition of oil field is all relatively poor, can't satisfy the needs of existing oil field reservoir condition.
Therefore, be necessary to provide a kind of new well workover leak stopping water-absorbing resin and synthetic method thereof.
Summary of the invention
The purpose of this invention is to provide a kind of well workover leak stopping water-absorbing resin.
Another object of the present invention provides the synthetic method of a kind of well workover leak stopping with water-absorbing resin.
The present invention relates to a kind of well workover leak stopping water-absorbing resin, it is that each component by following weight proportion makes through following synthesis step:
Described synthesis step is as follows:
A. take by weighing 2-acrylamido-2-methyl propane sulfonic acid, acrylamide, N respectively by described weight proportion, N-methylene-bisacrylamide and deionized water, described each component is mixed to form mixture, and churning time is 5-10 minute, and whipping temp is 30-50 ℃;
B. the described mixture that makes among the step a is put into polymerization reaction kettle, stir described mixture and feed nitrogen so that described polymerization reaction kettle is carried out air displacement, the logical nitrogen time is 30 minutes, simultaneously described polymerization reaction kettle is heated to 40-50 ℃, the persulfuric acid salt initiator that adds described weight proportion then in described mixture makes described mixture carry out polyreaction to generate water-absorbing resin, after described polyreaction begins, be incubated at least 6 hours;
C. with the described water-absorbing resin oven dry that makes among the step b, bake out temperature is no more than 120 ℃, drying time be 24 hours until oven dry, the described water-absorbing resin after will drying then is ground into the 0.5-40mm size particles, promptly gets described well workover leak stopping water-absorbing resin.
Described well workover leak stopping with the preferred weight proportion of each component of water-absorbing resin is:
Described persulfuric acid salt initiator is Sodium Persulfate, Potassium Persulphate or ammonium persulphate, preferred Sodium Persulfate.
The invention still further relates to the synthetic method of above-mentioned well workover leak stopping with water-absorbing resin, it may further comprise the steps:
A. take by weighing 2-acrylamido-2-methyl propane sulfonic acid, acrylamide, N respectively by described weight proportion, N-methylene-bisacrylamide and deionized water, described each component is mixed to form mixture, and churning time is 5-10 minute, and whipping temp is 30-50 ℃;
B. the described mixture that makes among the step a is put into polymerization reaction kettle, stir described mixture and feed nitrogen so that described polymerization reaction kettle is carried out air displacement, the logical nitrogen time is 30 minutes, simultaneously described polymerization reaction kettle is heated to 40-50 ℃, the persulfuric acid salt initiator that adds described weight proportion then in described mixture makes described mixture carry out polyreaction to generate water-absorbing resin, after described polyreaction begins, be incubated at least 6 hours;
C. with the described water-absorbing resin oven dry that makes among the step b, bake out temperature is no more than 120 ℃, drying time be 24 hours until oven dry, the described water-absorbing resin after will drying then is ground into the 0.5-40mm size particles, promptly gets described well workover leak stopping water-absorbing resin.
Well workover leak stopping of the present invention is as follows with each component role of water-absorbing resin:
2-acrylamido-2-methyl propane sulfonic acid: it has good hydratability and low to cationic susceptibility, thereby can guarantee that polymkeric substance still has good water-absorbing-retaining ability under high temperature, high salt and highly compressed condition.
Acrylamide: its good water solubility, polymerization activity are good, thereby are easy to control the desired molecular weight of the water-absorbing resin that can obtain to suit, and acrylamide also has extensive, the moderate advantage of raw material sources.
N, the N-methylene-bisacrylamide: it mainly acts on is as linking agent in polyreaction, when its content is lower than 0.2% weight percent, be difficult to make water-absorbing resin to form crosslinked body, and content make water-absorbing resin become fragile when being higher than 0.5% weight percent easily and cause intensity to reduce.
Persulfuric acid salt initiator: its mainly act on be in polyreaction as initiator, when its content is higher than 0.08% weight percent, cause water-absorbing resin poly-cruelly easily, then be difficult to make the water-absorbing resin polymerization when content is lower than 0.03% weight percent.
Deionized water: its content is generally the weight proportion of 40-60%.The main effect of deionized water is to provide solvent as dissolved monomer for the polyreaction of water-absorbing resin.
Well workover leak stopping of the present invention is effective with the water-swelling of water-absorbing resin, heat and salinity tolerance and compressive property are strong.Not only shutoff stratum leak path promptly prevents the leakage of workover fluid, and can degrade voluntarily, and zone permeability is recovered again, and the stratum is not had injury.In addition, well workover leak stopping of the present invention is simple, workable, easy to use with the synthetic method of water-absorbing resin.
Performance evaluation:
The well workover leak stopping that following embodiment of the present invention is made is carried out performance evaluation with water-absorbing resin below, and evaluation content is as follows:
(1) heat and salinity tolerance and compressive property evaluation.The water-absorbing resin that following embodiment is made is configured to the dry water-absorbing resin of certain order number, and it is joined in the water sucting medium that salinity (in sodium-chlor) is 30000mg/L (is the dosing basis with the seawater), take out after 72 hours 120 ℃ of following water-swellings, the resin after will absorbing water then is used for leakage-stop liquid and carry out casting bed test.Under 120 ℃ condition, test the leak stopping performance of water-absorbing resin respectively.If plugging effect is better under the certain pressure condition, the pressure 0.5Mpa that then at every turn raises by this testing method, the pressure that constantly raises, measures the maximum compressive property of water-absorbing resin.
With existing acrylic acid or the like water-absorbing resin as a comparison case, the heat and salinity tolerance of the water-absorbing resin that makes of the following embodiment 1-4 of the present invention and the test result of compressive property are asked for an interview table 1.
Table 1
| Performance | Comparative Examples | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Heat-resisting property | 100℃ | 120℃ | 120℃ | 120℃ | 120℃ |
| Anti-salt property (in sodium-chlor) | 30000mg/L | 30000mg/L | 30000mg/L | 30000mg/L | 30000mg/L |
| Ageing resistance | 12h | 20h | 19h | 22h | 24h |
| Compressive property (casting bed pressure-bearing) | 3MPa | 4.5MPa | 5MPa | 5.5MPa | 5MPa |
Test result shows, the water-absorbing resin that the present invention makes is with respect to existing acrylic acid or the like water-absorbing resin, heat-resisting property, ageing resistance and compressive property all are improved, heat-resisting property has improved 20 ℃, the anti-aging time can prolong one times, and compressive property is can reach 5.5MPa under the condition of 30000mg/L 120 ℃ * 72 hours and salinity (in sodium-chlor).Therefore, the better effects if of water-absorbing resin shutoff of the present invention stratum seepage is more suitable for satisfying the needs of existing oil field reservoir condition.And the water-absorbing resin that the present invention makes is after workover treatment is finished, and the de-plugging of can wearing out voluntarily recovers zone permeability automatically, thereby can not damage the stratum.In addition, water-absorbing resin synthetic method of the present invention is simple, workable, and the water-absorbing resin particle size distribution range after oven dry is pulverized is wider, and can obtain the water-absorbing resin that specific dimensions distributes by the parameter of adjusting pulverizer, thereby realize effect the specific specific shutoff of stratum leak path.
Embodiment
Embodiment 1
(1) material choice.The well workover leak stopping of present embodiment is selected following raw material for use with water-absorbing resin:
2-acrylamido-2-methyl propane sulfonic acid: 30g, raw material sources are Japanese import, and purity is 99%, and type of service is a white crystalline powder;
Acrylamide: 80g, raw material sources are produced by Beijing chemical reagents corporation, and purity is 98%, and type of service is the white crystals body;
N,N methylene bis acrylamide: 1g, raw material sources are produced by Beijing chemical reagents corporation, and purity is 98%, and type of service is a white crystalline powder;
Sodium Persulfate: 0.1g, raw material sources are produced by chemical reagent company limited of Tianjin Jin Hui the Pacific-Asian, and purity is 99%, and type of service is the white crystals body;
Deionized water: 88.9g, raw material sources are self-control.
(2) raw material stirring.2-acrylamido-2-methyl propane sulfonic acid, acrylamide and N with above-mentioned weight proportion, the N-methylene-bisacrylamide mixes in uncovered agitator, add the deionized water of above-mentioned weight proportion then and mix to form mixture, churning time is 10 minutes, and whipping temp is 40 ℃.
(3) polyreaction.The mixture that mixing stirs is put into polymerization reaction kettle, open agitating function, and feed nitrogen so that polymerization reaction kettle is carried out air displacement, the logical nitrogen time is 30 minutes, polymerization reaction kettle is heated to 45 ℃ simultaneously, the Sodium Persulfate that adds above-mentioned weight proportion then in mixture generates water-absorbing resin with initiated polymerization, after polyreaction begins, is incubated at least 6 hours.
(4) oven dry is pulverized.The water-absorbing resin that polyreaction is generated takes out from polymerization reaction kettle, it is cut into suitable shape so that oven dry, water-absorbing resin after shearing is put into baking oven dries, bake out temperature is 120 ℃, drying time is 24 hours, use the water-absorbing resin after pulverizer will be dried to be ground into water absorbing resin particle then, grain diameter is between 0.5-40mm.
(5) packing.Water absorbing resin particle after pulverizing is sieved according to different-grain diameter, and use the water absorbing resin particle packing of damp proof material each particle diameter grade.
Embodiment 2-4
The well workover leak stopping of embodiment of the invention 2-4 is identical with embodiment 1 with the preparation method of water-absorbing resin, and its each component concentration is asked for an interview table 2.
Table 2
| Raw material | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| 2-acrylamido-2-methyl propane sulfonic acid | 10g | 12g | 15g |
| Acrylamide | 35g | 40g | 45g |
| N,N methylene bis acrylamide | 0.3g | 0.4g | 0.5g |
| Persulfuric acid salt initiator | Sodium Persulfate, 0.05g | Potassium Persulphate, 0.03g | Ammonium persulphate, 0.08g |
| Deionized water | 54.65g | 47.57g | 39.42g |
Claims (5)
1. well workover leak stopping water-absorbing resin, its each component by following weight proportion makes through following synthesis step:
Described synthesis step is as follows:
A. take by weighing 2-acrylamido-2-methyl propane sulfonic acid, acrylamide, N respectively by described weight proportion, N-methylene-bisacrylamide and deionized water, described each component is mixed to form mixture, and churning time is 5-10 minute, and whipping temp is 30-50 ℃;
B. the described mixture that makes among the step a is put into polymerization reaction kettle, stir described mixture and feed nitrogen so that described polymerization reaction kettle is carried out air displacement, the logical nitrogen time is 30 minutes, simultaneously described polymerization reaction kettle is heated to 40-50 ℃, the persulfuric acid salt initiator that adds described weight proportion then in described mixture makes described mixture carry out polyreaction to generate water-absorbing resin, after described polyreaction begins, be incubated at least 6 hours;
C. with the described water-absorbing resin oven dry that makes among the step b, bake out temperature is no more than 120 ℃, drying time be 24 hours until oven dry, the described water-absorbing resin after will drying then is ground into the 0.5-40mm size particles, promptly gets described well workover leak stopping water-absorbing resin.
2. well workover leak stopping water-absorbing resin as claimed in claim 1, wherein the weight proportion of each component is:
3. well workover leak stopping water-absorbing resin as claimed in claim 1, wherein said persulfuric acid salt initiator is Sodium Persulfate, Potassium Persulphate or ammonium persulphate.
4. well workover leak stopping water-absorbing resin as claimed in claim 3, wherein said persulfuric acid salt initiator is a Sodium Persulfate.
5. each described well workover leak stopping is with the method for water-absorbing resin among the synthetic claim 1-4, and it may further comprise the steps:
A. take by weighing 2-acrylamido-2-methyl propane sulfonic acid, acrylamide, N respectively by described weight proportion, N-methylene-bisacrylamide and deionized water, described each component is mixed to form mixture, and churning time is 5-10 minute, and whipping temp is 30-50 ℃;
B. the described mixture that makes among the step a is put into polymerization reaction kettle, stir described mixture and feed nitrogen so that described polymerization reaction kettle is carried out air displacement, the logical nitrogen time is 30 minutes, simultaneously described polymerization reaction kettle is heated to 40-50 ℃, the persulfuric acid salt initiator that adds described weight proportion then in described mixture makes described mixture carry out polyreaction to generate water-absorbing resin, after described polyreaction begins, be incubated at least 6 hours;
C. with the described water-absorbing resin oven dry that makes among the step b, bake out temperature is no more than 120 ℃, drying time be 24 hours until oven dry, the described water-absorbing resin after will drying then is ground into the 0.5-40mm size particles, promptly gets described well workover leak stopping water-absorbing resin.
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| CN 201110072410 CN102181008B (en) | 2011-03-24 | 2011-03-24 | Water absorption resin for well repair and leaking stoppage and synthesis method thereof |
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| CN 201110072410 CN102181008B (en) | 2011-03-24 | 2011-03-24 | Water absorption resin for well repair and leaking stoppage and synthesis method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073679A (en) * | 2012-12-25 | 2013-05-01 | 北京希涛技术开发有限公司 | Method for producing polyacrylamide microsphere water shutoff agent |
| CN104449613A (en) * | 2014-10-31 | 2015-03-25 | 中国石油化工集团公司 | Water-absorbent resin temporary plugging agent and preparation method thereof |
| CN104531099A (en) * | 2014-12-29 | 2015-04-22 | 河北光大石化有限公司 | Salt-resistant filtrate-loss reducer for drilling fluid and preparation method of salt-resistant filtrate-loss reducer |
| CN109666467A (en) * | 2017-10-13 | 2019-04-23 | 中国石油化工股份有限公司 | Controllable time delay expands sealing agent and preparation method thereof |
| CN110387133A (en) * | 2019-06-12 | 2019-10-29 | 施祖新 | A kind of preparation method of fiber duct modified water absorbent resin |
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| CN101619188A (en) * | 2009-07-16 | 2010-01-06 | 青岛红树林投资有限公司 | Underwater high-strength epoxy anchor adhesive and preparation method thereof |
| CN101864032A (en) * | 2010-05-14 | 2010-10-20 | 中国石油大学(华东) | Micro emulsion polymer for displacement control of oil deposit deep part with high temperature and mineralization and preparation method |
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2011
- 2011-03-24 CN CN 201110072410 patent/CN102181008B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101619188A (en) * | 2009-07-16 | 2010-01-06 | 青岛红树林投资有限公司 | Underwater high-strength epoxy anchor adhesive and preparation method thereof |
| CN101864032A (en) * | 2010-05-14 | 2010-10-20 | 中国石油大学(华东) | Micro emulsion polymer for displacement control of oil deposit deep part with high temperature and mineralization and preparation method |
Non-Patent Citations (1)
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| 《中国优秀博硕士学位论文全文数据库（硕士）工程科技I辑》 20040915 刘洋 聚丙烯酰胺系高吸水性树脂研究 第1章至第3章 1－5 , * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073679A (en) * | 2012-12-25 | 2013-05-01 | 北京希涛技术开发有限公司 | Method for producing polyacrylamide microsphere water shutoff agent |
| CN103073679B (en) * | 2012-12-25 | 2015-04-15 | 北京希涛技术开发有限公司 | Method for producing polyacrylamide microsphere water shutoff agent |
| CN104449613A (en) * | 2014-10-31 | 2015-03-25 | 中国石油化工集团公司 | Water-absorbent resin temporary plugging agent and preparation method thereof |
| CN104531099A (en) * | 2014-12-29 | 2015-04-22 | 河北光大石化有限公司 | Salt-resistant filtrate-loss reducer for drilling fluid and preparation method of salt-resistant filtrate-loss reducer |
| CN109666467A (en) * | 2017-10-13 | 2019-04-23 | 中国石油化工股份有限公司 | Controllable time delay expands sealing agent and preparation method thereof |
| CN110387133A (en) * | 2019-06-12 | 2019-10-29 | 施祖新 | A kind of preparation method of fiber duct modified water absorbent resin |
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| CN102181008B (en) | 2013-07-10 |
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Address after: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee after: China Oilfield Services Limited Patentee after: China Offshore Oil Group Co., Ltd. Address before: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee before: China Oilfield Services Limited Patentee before: China National Offshore Oil Corporation |
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