CN102757779A - Preparation method of acidic crosslinking agent applied to carboxymethyl guar gum - Google Patents
Preparation method of acidic crosslinking agent applied to carboxymethyl guar gum Download PDFInfo
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- CN102757779A CN102757779A CN2012102371825A CN201210237182A CN102757779A CN 102757779 A CN102757779 A CN 102757779A CN 2012102371825 A CN2012102371825 A CN 2012102371825A CN 201210237182 A CN201210237182 A CN 201210237182A CN 102757779 A CN102757779 A CN 102757779A
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Abstract
The invention relates to a preparation method of an acidic crosslinking agent applied to carboxymethyl guar gum. An acid technology is usually carried out in a hydraulic fracturing process, which causes secondary damage to a reservoir stratum. The preparation method comprises the following steps of: uniformly mixing 3 parts by weight of citric acid, 57-82 parts by weight of water and 10-20 parts by weight of micromolecular polyhydroxy compound and heating, after the temperature reaches 50 DEG C, slowly adding 5-20 parts by weight of zirconium oxychloride; and keeping the temperature to be 50-55 DEG C, reacting for 3-4 hours, cooling a product to reach room temperature to obtain the acidic crosslinking agent. The cidic crosslinking agent provided by the invention is suitable for an acidic system, and jelly formed by crosslinking is higher in temperature tolerance and is well in sand carrying property, and can be applied to an alkaline-sensitive stratum; a small quantity of citric acid is added in a synthesis process, so that the pH of the whole reaction system is kept constant, the operation step during production is simplified; and the consumption of the organic zirconium crosslinking agent is 0.8 percent, the concentration of a carboxymethyl guar gum water solution is 0.4 percent, and the quantity of residue after crosslinking gelout is 160mg/L.
Description
Technical field
The present invention relates to the linking agent of a kind of oil field carboxymethyl guar glue pressure break system, be specifically related to a kind of preparation method who is applied to the acidic crosslinking agent of carboxymethyl guar glue.
Background technology
Pressure break is the important method of oilfield stimulation, along with the development of stimulation technology, uses waterfrac treatment can not fully satisfy field requirement separately.In the waterfrac treatment process,, can bring the secondary injury to reservoir often with the carrying out of acidification technique.Under sour environment, can suppress effectively to migrate because of the expansion that the surperficial negative typical case of clay causes, strengthen the molecular force of each interlayer, thereby stablize clay layer.On the other hand, fracturing liquid presents acidity, can play plugging removal effect, improves the effect of reservoir permeability.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who is applied to the acidic crosslinking agent of carboxymethyl guar glue, be used for overcoming the inapplicable secondary injury problem with alkali quick property bottom and acidification technology of oil well of fracturing liquid in the prior art.
The technical scheme that the present invention adopted is:
Be applied to the preparation method of the acidic crosslinking agent of carboxymethyl guar glue, it is characterized in that:
Realize by following steps:
Step 1: 3 weight part Hydrocerol As, 57-82 weight parts water and 10-20 weight part small molecules polyol are mixed and heat, treat temperature to 50 ℃ after, slowly add 5 ~ 20 weight part zirconium oxychlorides;
Step 2: maintain the temperature at 50-55 ℃, reaction 3-4h, product is cooled to room temperature, obtains acidic crosslinking agent.
Described small molecules polyol is selected from glucose, fructose, sucrose, sorbyl alcohol, glucono-and sodium salt thereof.
The present invention has the following advantages:
1, is fit to acid system
The present invention is fit to acid system, crosslinkedly becomes the frozen glue tolerable temperature higher, and taking grittiness can be good, can be applied to the quick property of alkali stratum, has expanded the crosslinked range of application of carboxymethyl guar fracturing fluid.
2, synthesis technique is easier
Add a small amount of Hydrocerol A in the synthesis technique, make whole reaction system pH keep constant, simplify the operation steps in producing.
3, level of residue is few
The organic zirconium dosage of crosslinking agent is 0.8%, and carboxymethyl guar glue solution concentration is 0.4%, and level of residue is 160mg/L behind the crosslinked broken glue.
4, small molecules polyol
The small molecules polyol is as part in the organic zirconium linking agent, its excess molecular be wrapped in colloidal solid (inorganic zirconium) around, can play the effect of shielding to the zirconates ion, thereby prolong the crosslinking time of linking agent and improve the heat resistance of frozen glue.
Embodiment
Below in conjunction with embodiment the present invention is carried out detailed explanation.
To achieve these goals, the technical scheme of the present invention's employing is:
A kind of acidic crosslinking agent of using carboxymethyl guar glue and preparation method thereof, its special character is: the raw material and the weight proportion of said linking agent are following:
3 parts of Hydrocerol As
5 ~ 20 parts of zirconium oxychlorides
57 ~ 82 parts in water
10 ~ 20 parts of small molecules polyols
Wherein: the small molecules polyol comprises: glucose, fructose, sucrose, sorbyl alcohol, glucono-and sodium salt thereof etc.
Embodiment 1
With the Hydrocerol A of 3 weight parts, the water of 57 weight parts, the sucrose of 20 weight parts mixes; When treating that system temperature rises to 50 ℃, add the zirconium oxychloride of 20 weight parts, holding temperature is at 55 ℃; Reaction 3h, the transparent homogeneous liquid that obtains is acid organic zirconium linking agent.
Embodiment 2
With the Hydrocerol A of 3 weight parts, the water of 77 weight parts, 1; The glucose of 5 weight parts mixes, and when treating that system temperature rises to 50 ℃, adds the zirconium oxychloride of 5 weight parts; Holding temperature is reacted 3.5h at 50 ℃, and the transparent homogeneous liquid that obtains is acid organic zirconium linking agent.
Embodiment 3
With the Hydrocerol A of 3 weight parts, the water of 77 weight parts, the sorbyl alcohol of 10 weight parts mixes, and when treating that system temperature rises to 50 ℃, adds the zirconium oxychloride of 10 weight parts, and holding temperature is reacted 4h at 50 ℃.The transparent homogeneous liquid that obtains is acid organic zirconium linking agent.
Embodiment 4
With the Hydrocerol A of 3 weight parts, the water of 82 weight parts, the fructose of 10 weight parts mixes, and when treating that system temperature rises to 50 ℃, adds the zirconium oxychloride of 5 weight parts, and holding temperature is reacted 3h at 55 ℃, and the transparent homogeneous liquid that obtains is acid organic zirconium linking agent.
Embodiment 5
With the Hydrocerol A of 3 weight parts, the water of 72 weight parts, the glucono-of 10 weight parts mixes; When treating that system temperature rises to 50 ℃, add the zirconium oxychloride of 15 weight parts, holding temperature is at 50 ℃; Reaction 3.5h, the transparent homogeneous liquid that obtains is acid organic zirconium linking agent.
Embodiment 6
With the Hydrocerol A of 3 weight parts, the water of 72 weight parts, the Sunmorl N 60S of 10 weight parts mixes; When treating that system temperature rises to 50 ℃, add the zirconium oxychloride of 15 weight parts, holding temperature is at 50 ℃; Reaction 3.5h, the transparent homogeneous liquid that obtains is acid organic zirconium linking agent.
With crosslinked according to 0.4:100 of the linking agent that obtains and ethyloic base guar gum, be stirred to the frozen glue that can hang, and write down the used time, and detect the tolerable temperature of frozen glue than mixing.Crosslinking time and tolerable temperature are all carried out by oil and gas industry standard SY/T5107-2005 standard.
Detected result is as shown in the table:
Learnt that by above result linking agent provided by the invention can form frozen glue under acidic conditions, broken glueization under alkaline condition can not produce phenomenons such as sand plug in carrying of the fracturing fluid process, meet to acid cross-linked the purpose on the quick property of alkali stratum.
It is cited that content of the present invention is not limited to embodiment, and the conversion of any equivalence that those of ordinary skills take technical scheme of the present invention through reading specification sheets of the present invention is claim of the present invention and contains.
Claims (2)
1. be applied to the preparation method of the acidic crosslinking agent of carboxymethyl guar glue, it is characterized in that:
Realize by following steps:
Step 1: 3 weight part Hydrocerol As, 57-82 weight parts water and 10-20 weight part small molecules polyol are mixed and heat, treat temperature to 50 ℃ after, slowly add 5-20 weight part zirconium oxychloride;
Step 2: maintain the temperature at 50-55 ℃, reaction 3-4h, product is cooled to room temperature, obtains acidic crosslinking agent.
2. the preparation method who is applied to the acidic crosslinking agent of carboxymethyl guar glue according to claim 1 is characterized in that:
Described small molecules polyol is selected from glucose, fructose, sucrose, sorbyl alcohol, glucono-and sodium salt thereof.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012102371825A CN102757779A (en) | 2012-07-10 | 2012-07-10 | Preparation method of acidic crosslinking agent applied to carboxymethyl guar gum |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012102371825A CN102757779A (en) | 2012-07-10 | 2012-07-10 | Preparation method of acidic crosslinking agent applied to carboxymethyl guar gum |
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| CN102757779A true CN102757779A (en) | 2012-10-31 |
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| CN2012102371825A Pending CN102757779A (en) | 2012-07-10 | 2012-07-10 | Preparation method of acidic crosslinking agent applied to carboxymethyl guar gum |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104774605A (en) * | 2014-01-11 | 2015-07-15 | 中国石油化工股份有限公司 | Low damage small molecule environmental-protection type fracturing fluid and preparation method thereof |
| CN105199706A (en) * | 2015-11-02 | 2015-12-30 | 天津中海油服化学有限公司 | Organic zirconium crosslinking agent applicable to polymer fracturing fluid system and preparation method of organic zirconium crosslinking agent |
| CN111676008A (en) * | 2020-06-05 | 2020-09-18 | 中国石油大学(北京) | Acidic fracturing fluid and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220264A (en) * | 2007-12-18 | 2008-07-16 | 长庆石油勘探局 | Method of producing acidic crosslinking agent for CO2 foam compression fracture |
| CN102363727A (en) * | 2011-11-12 | 2012-02-29 | 西北大学 | Seawater-based oil gas well fracturing fluid |
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2012
- 2012-07-10 CN CN2012102371825A patent/CN102757779A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220264A (en) * | 2007-12-18 | 2008-07-16 | 长庆石油勘探局 | Method of producing acidic crosslinking agent for CO2 foam compression fracture |
| CN102363727A (en) * | 2011-11-12 | 2012-02-29 | 西北大学 | Seawater-based oil gas well fracturing fluid |
Non-Patent Citations (1)
| Title |
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| 刘祥等: "有机锆对羧甲基羟丙基瓜胶的交联性能研究", 《化学工程师》, no. 2, 25 February 2011 (2011-02-25), pages 10 - 13 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104774605A (en) * | 2014-01-11 | 2015-07-15 | 中国石油化工股份有限公司 | Low damage small molecule environmental-protection type fracturing fluid and preparation method thereof |
| CN105199706A (en) * | 2015-11-02 | 2015-12-30 | 天津中海油服化学有限公司 | Organic zirconium crosslinking agent applicable to polymer fracturing fluid system and preparation method of organic zirconium crosslinking agent |
| CN111676008A (en) * | 2020-06-05 | 2020-09-18 | 中国石油大学(北京) | Acidic fracturing fluid and preparation method and application thereof |
| CN111676008B (en) * | 2020-06-05 | 2021-07-09 | 中国石油大学(北京) | Acidic fracturing fluid and preparation method and application thereof |
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Application publication date: 20121031 |