CN101376723A - Preparation of reduction complexing type polymer chromium cross linker - Google Patents
Preparation of reduction complexing type polymer chromium cross linker Download PDFInfo
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- CN101376723A CN101376723A CNA2007101207748A CN200710120774A CN101376723A CN 101376723 A CN101376723 A CN 101376723A CN A2007101207748 A CNA2007101207748 A CN A2007101207748A CN 200710120774 A CN200710120774 A CN 200710120774A CN 101376723 A CN101376723 A CN 101376723A
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- oxalic acid
- gelatinizing
- water
- preparation
- sodium
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Abstract
The invention relates to a preparation method of a cross linker of reducing-complex polymer chrome. (1), water and sodium acid chromate are added into a reactor; (2), oxalic acid is added in batches under stirring; (3), the temperature is raised between 60 and 80 DEG C and then a stirring reaction with a constant temperature is carried out for 1 to 2 hours; (4) aqueous alkali is slowly added under stirring and reacted for 1 hour; the mol ratio of Cr(III) to the oxalic acid is 1:7 to 9; the mass ratio of the sodium acid chromate to water is 1:2 to 4.8; the aqueous alkali is the water liquor of sodium hydroxide or potassium hydroxide with a concentration of 10 to 50 percent and the dosage of the aqueous alkali is 2.2 to 11.3 percent of the mass of the oxalic acid; the material varieties are less; the preparation process is simply operated; the cross linker has no pungent smells and has the advantages of gelatinizing performance delaying, adjustable gelatinizing time, large scale of the gelatinizing concentration, low using amount and low polymer consumption; the lowest gelatinizing concentration of HPAM can achieve 600mg/L; a formed gelatinizing system is stable in performance which can be stable for more than 60 days under the oxygen exposure condition of 60 DEG C.
Description
Technical field
The present invention relates to a kind of oil field that is used for and improve the preparation method of the polymer gel of recovery ratio with chromium cross linker.
Background technology
High-valency metal chromium is one of linking agent of being used always of field polymers gel technique, and the product of application mainly contains redox system chromium and organic complex chromium.Redox system is mainly the mixture of dichromate and reductive agent, and the shortcoming of this system is: do not have the delayed cross-linking feature, redox reaction can affect to polymkeric substance, and sexavalent chrome has hypertoxicity.Organic complex chromium is mainly the complexing trivalent chromium of acetic acid (salt), propionic acid (salt), lactic acid (salt) etc.Patent CN200410023616.7 provides the preparation method of a kind of polyacrylamide gel with the retarded crosslinking agent, it is that raw material adopts reduction method to make a kind of compound organic complex chromium with sodium dichromate 99, the vitriol oil, S-WAT, humic acids, acetic acid, citric acid, 40% sodium hydroxide, water, but its raw material type is various, preparation process complexity, product have the irritating smell of acetic acid.People such as bibliographical information: Tian Yuqin, Zheng Yancheng, Wang Mount Lushan, Duan Hongdong adopt dichromate and reductive agent reaction to generate trivalent chromium respectively, the method of carrying out complexing with organic acid has prepared linking agent again, this method exists preparation process complicated, hexavalent chrome reduction is incomplete, uses Sodium Nitrite can produce shortcomings such as nitrogen peroxide toxic gas as reductive agent.As linking agent, but it uses inconvenience, cost high to people such as Ye Bo, Gan Xuhong with the organic acid of mol ratio 5:1 and chromium trichloride.
People such as Li Yongtai, Peng Zhigang has prepared a kind of organic chromium complex compound crystal linking agent, but complicated process of preparation, and working substance content is low.
Summary of the invention
The purpose of this invention is to provide a kind of with oxalic acid and sodium dichromate 99 as raw material, reduction by oxalic acid and complex reaction prepare the oil field and improve recovery ratio with the preparation method of polyacrylamide gel with polymer chromium cross linker.
Starting material required for the present invention are sodium dichromate 99, oxalic acid, alkaline solution, water.Concrete grammar is:
1. in reactor, add entry and sodium dichromate 99;
2. under agitation add oxalic acid in batches;
3. be warming up to 60～80 ℃ of constant temperature stirring reactions 1 hour～2 hours;
4. under agitation slowly add alkaline solution, continue reaction 1 hour.
The Cr that sodium dichromate 99 provided (III) is 1:7～9 with the mol ratio of oxalic acid.
The mass ratio of sodium dichromate 99 and water is 1:2～4.8.
Used alkaline solution is 10～50% sodium hydroxide or potassium hydroxide aqueous solution.The consumption of sodium hydroxide or potassium hydroxide is 2.2～11.3% of an oxalic acid quality.
The effective chromium ion concentration of prepared cross-linking agent is 4.0%.
Oxalic acid belongs to diprotic acid, has both had stronger complex ability, has reductibility again, can oxidized production carbonic acid gas and water.The present invention utilizes the Cr of the reductibility of oxalic acid with sodium dichromate 99
6+Be reduced into Cr
3+, again by Cr
3+With the oxalic acid complexing, generate the polymer chromium cross linker of complex state.
The effect of invention
The present invention has following characteristics:
1. preparation technology is simple.The raw material type that the present invention uses is few, and preparation process is simple to operate.
2. linking agent has no irritating odor.The present invention uses the complexing agent of oxalic acid as chromium ion, has no irritating odor, and has brought convenience for production and use.
3. have the gel-forming property of delaying, gelation time is adjustable.Linking agent of the present invention and HPAM gelation time can be controlled at random time in the several hrs to 15 day by additive.
4. linking agent becomes the gum concentration wide ranges, and usage quantity is low.When the HPAM working concentration is 1000mg/L, HPAM/Cr
3+Mass ratio all can form the stable gel system in 5～50 scopes.
5. polymer loading is low.Use linking agent of the present invention, the minimum one-tenth gum concentration of HPAM can reach 600mg/L.
6. the gelling system stable performance of Xing Chenging.The formed gelling system of linking agent of the present invention and HPAM can be stablized more than 60 days under 60 ℃, sudden and violent oxygen condition.
Embodiment
Embodiment 1:
Prepare raw material: sodium dichromate 99, oxalic acid, sodium hydroxide, water.
Place the magnetic agitation control-temperature electric heating to put the 250mL there-necked flask that magnetic agitation, reflux exchanger, thermometer are housed, in adding flask, add 11.92g sodium dichromate 99 and 34.72g deionized water, divide adding 45.36g oxalic acid 7 times after stirring 10min, continue to stir and be warming up to 70 ℃, the sodium hydroxide solution 12.0g of slow adding 20% behind the isothermal reaction 2h, continuation is at 70 ℃ of isothermal reaction 1h, and cooling promptly obtains 104.0g linking agent, Cr
3+Content 4.0%.
Embodiment 2:
Prepare raw material: sodium dichromate 99, oxalic acid, potassium hydroxide, water.
Place the magnetic agitation control-temperature electric heating to put the 250mL there-necked flask that magnetic agitation, reflux exchanger, thermometer are housed, in adding flask, add 11.92g sodium dichromate 99 and 44.8g deionized water, divide adding 35.28g oxalic acid 5 times after stirring 10min, continue to stir and be warming up to 60 ℃, the potassium hydroxide solution 12.0g of slow adding 20% behind the isothermal reaction 2h, continuation is at 60 ℃ of isothermal reaction 1h, and cooling promptly obtains 104.0g linking agent, Cr
3+Content 4.0%.
Claims (1)
1. the preparation method of a reduction complexing type polymer chromium cross linker is a raw material with sodium dichromate 99, oxalic acid, alkaline solution, water, it is characterized in that:
1. in reactor, add entry and sodium dichromate 99;
2. under agitation add oxalic acid in batches;
3. be warming up to 60 ℃～80 ℃ constant temperature stirring reactions 1 hour～2 hours;
4. under agitation slowly add alkaline solution, continue reaction 1 hour;
The Cr that sodium dichromate 99 provided (III) is 1:7～9 with the mol ratio of oxalic acid;
The mass ratio of sodium dichromate 99 and water is 1:2～4.8;
Used alkaline solution is 10～50% sodium hydroxide or potassium hydroxide aqueous solution; The consumption of sodium hydroxide or potassium hydroxide is 2.2～11.3% of an oxalic acid quality.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101207748A CN101376723A (en) | 2007-08-27 | 2007-08-27 | Preparation of reduction complexing type polymer chromium cross linker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101207748A CN101376723A (en) | 2007-08-27 | 2007-08-27 | Preparation of reduction complexing type polymer chromium cross linker |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101376723A true CN101376723A (en) | 2009-03-04 |
Family
ID=40420465
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101207748A Pending CN101376723A (en) | 2007-08-27 | 2007-08-27 | Preparation of reduction complexing type polymer chromium cross linker |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101376723A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353569B (en) * | 2008-09-17 | 2011-06-29 | 西南石油大学 | Controllable cross linked gel water blockage plugging material |
| CN103666422A (en) * | 2013-12-04 | 2014-03-26 | 天津大港油田滨港集团博弘石油化工有限公司 | High-strength dilatation-retarding particle deep fluid diverting agent |
-
2007
- 2007-08-27 CN CNA2007101207748A patent/CN101376723A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353569B (en) * | 2008-09-17 | 2011-06-29 | 西南石油大学 | Controllable cross linked gel water blockage plugging material |
| CN103666422A (en) * | 2013-12-04 | 2014-03-26 | 天津大港油田滨港集团博弘石油化工有限公司 | High-strength dilatation-retarding particle deep fluid diverting agent |
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| PB01 | Publication | ||
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Open date: 20090304 |