CN106749736B - A kind of cross-linking type both sexes xanthan gum and preparation method thereof - Google Patents
A kind of cross-linking type both sexes xanthan gum and preparation method thereof Download PDFInfo
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- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0033—Xanthan, i.e. D-glucose, D-mannose and D-glucuronic acid units, saubstituted with acetate and pyruvate, with a main chain of (beta-1,4)-D-glucose units; Derivatives thereof
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- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
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Abstract
The present invention provides a kind of cross-linking type both sexes xanthan gum and preparation method thereof, the method includes first being alkalized in a solvent using alkali to xanthan gum, then etherification reaction is carried out to the xanthan gum after alkalization using cationic etherifying agent, it finally reuses crosslinking agent and cross-linking reaction is carried out to the xanthan gum after etherificate, obtain the cross-linking type both sexes xanthan gum.Compared to xanthan gum, the viscoelastic property and network structure of cross-linking type both sexes xanthan gum are been significantly enhanced, and when being used for fracturing fluid, thickening agent dosage can be not only reduced, but also the viscoelastic property of fracturing fluid can be improved, to reduce cost.
Description
Technical field
The invention belongs to oil mining fields, specifically, are related to a kind of cross-linking type both sexes xanthan gum and preparation method thereof.
Especially a kind of low crosslinking degree both sexes xanthan gum and preparation method thereof.
Background technique
Xanthan gum is the macromolecule polysaccharide generated by carbohydrate through Xanthomonas campestris fermentation, intermolecular to be wound double helix
Structure is a kind of microbial polysaccharide thickening agent of function admirable that can replace natural plant gum, is widely used, has in petroleum industry
There are good thickening and rheological property；Xanthan gum is a kind of typical pseudoplastic fluid, has good water-soluble, resistance to acid and alkali
And salt tolerance, and have the characteristics that viscoelastic property height and solid-carrying performance are good, therefore can be used as non-crosslinked fracturing fluid and use.
For existing xanthan gum when configuring fracturing fluid as thickening agent, dosage is all larger.Application No. is
201310286824.5, the Chinese invention patent of Publication No. CN103361042A, the non-crosslinked fracturing fluid of xanthan gum, its preparation side
Method and purposes provide a kind of preparation method of 120 DEG C of heatproof of non-crosslinked xanthans fracturing fluid, the quality that xanthan gum uses
Score reaches 0.6%.
Its thickening capabilities and heat resistance mainly are improved by being modified to xanthan gum at present, reduces making for xanthan gum
Use concentration.Application No. is 201410475166.9, the Chinese patent application of Publication No. CN104312571A, a kind of modified xanthan
Glue thickening agent and its prepare in fracturing fluid application provide a kind of preparation method of modified xantham gum, although modified Huang
The apparent viscosity of virgin rubber increases 1 times, but its amount of modifier is larger (xanthan gum: modifying agent=10:3), modified higher cost.
Therefore, research and develop a kind of modified xantham gum thickening, make its modification is at low cost, viscoelastic property increase it is significant, and
Guarantee to reduce the concentration that xanthan gum uses while good solid-carrying performance, thus the problem of reducing cost, be still urgent need to resolve.
Summary of the invention
It is an object of the present invention to provide a kind of cross-linking type both sexes xanthan gum.
Another object of the present invention is to provide a kind of preparation methods of cross-linking type both sexes xanthan gum.
In order to achieve the above object, on the one hand, the present invention provides a kind of preparation methods of cross-linking type both sexes xanthan gum, wherein
The method includes first being alkalized in a solvent using alkali to xanthan gum, then using cationic etherifying agent to the Huang after alkalization
Virgin rubber carries out etherification reaction, finally reuses crosslinking agent and carries out cross-linking reaction to the xanthan gum after etherificate, obtains the cross-linking type
Both sexes xanthan gum.
Some specific embodiments according to the present invention, wherein by xanthan gum quality be 10 parts in terms of, alkali, cationic etherifying agent
Dosage with crosslinking agent is respectively 0.2-0.3 parts, 0.3-0.5 parts and 0.1-0.2 parts.
Some specific embodiments according to the present invention, wherein the alkali is sodium hydroxide or potassium hydroxide.
Some specific embodiments according to the present invention, wherein the cationic etherifying agent is selected from the chloro- 2- hydroxypropyl trimethylammonium of 3-
The one or more of the chloro- 2- hydroxypropyl triethylammonium chloride of ammonium chloride, 3- and the chloro- 2- hydroxypropyl tripropyl ammonium chloride of 3-.
Some specific embodiments according to the present invention, wherein the crosslinking agent is epoxychloropropane or sodium trimetaphosphate.
Some specific embodiments according to the present invention, wherein the solvent is alcohol/aqueous solution.
Some specific embodiments according to the present invention, wherein the alcohol is one of methanol, ethyl alcohol and isopropanol or more
The mixing solvent quality dosage of kind is 2-4 times of xanthan gum quality.
Some specific embodiments according to the present invention, wherein the volumetric concentration of the alcohol/aqueous solution is 70%-85%.
Some specific embodiments according to the present invention, wherein the alkalization includes alcohol/aqueous solution that xanthan gum is added to alkali
In, 0.5-1h is stirred at room temperature.
Some specific embodiments according to the present invention, wherein the etherification reaction includes that cationic etherifying agent is added instead
It answers in solution, reacts 1-3h at 55-70 DEG C.
Some specific embodiments according to the present invention, wherein the cross-linking reaction includes that reaction solution is added in crosslinking agent
In, 1-3h is reacted at 50-70 DEG C.
Some specific embodiments according to the present invention, wherein the reaction further includes that will react after the completion of cross-linking reaction
Solution is cooled to room temperature, and filtering washs away the complete reactant of unreacted with ethanol aqueous wash, and then drying obtains the crosslinking
Type both sexes xanthan gum.
Some specific embodiments according to the present invention, wherein the drying is in 50-60 DEG C of drying 10-15h.
Some specific embodiments according to the present invention, wherein described to wash away complete anti-of unreacted with ethanol aqueous wash
The step of answering object includes mixing filter cake with the ethanol water and filter cake of mass concentration 60-70% after filtering reaction solution
Filtering, is then successively repeated the above steps again with the ethanol water of 70-80%, 80-90%, 100%, is finally filtered after even.
" repeating the above steps " described here refers to that the filter cake that will be obtained after filtering uses the ethanol water of 70-80% again
It filters, then filters filter cake after mixing with the ethanol water of 80-90% again after mixing, filter cake is again with 100%
Ethanol water (dehydrated alcohol) filter after mixing.
The present invention successively use 60-70%, 70-80%, 80-90% and 100% ethanol water to filtering every time
The filter cake arrived carries out mixing, washing, to wash off the complete raw material of unreacted, wherein washing ethanol water concentration used every time upper
State sequential selection in range, for example can be respectively 70%, 70%, 80% and 100%, be also possible to 65%, 75%, 85%,
100% etc.；And some specific embodiments according to the present invention, per rear primary concentration and previous concentration difference is 3-
20%.
Some specific embodiments according to the present invention, wherein described to be filtered into suction filtration.
Some specific embodiments according to the present invention, wherein the method specifically includes:
(1) 100 parts of water/alcohol mixed solvents are configured；
(2) 0.2~0.3 part of alkali is added in the water in step (1)/alcohol in the mixed solvent, at room temperature stirring to dissolution；
(3) 10~20 parts of xanthan gum are added in the system in step (2), and stirring makes it suspend uniformly, at room temperature
Alkalization 0.5~1 hour；
(4) under stiring, 0.3-0.5 parts of cationic etherifying reagents are added to system made from step (3), at 55~70 DEG C
At a temperature of, it reacts 1~3 hour；
(5) under stiring, 0.1~0.2 part of crosslinking agent is added to system made from step (4), in 50~70 DEG C of temperature
Under, it reacts 1~3 hour, the crosslinking agent is epoxychloropropane；
(6) system made from step (5) is cooled to room temperature, is respectively that 60%, 80%, 90% ethyl alcohol is molten with mass concentration
Liquid and dehydrated alcohol washing are filtered 4 times, dried 10 hours at 60 DEG C or more, modified xantham gum then can be obtained after crushed,
That is cross-linking type both sexes xanthan gum.
On the other hand, the present invention also provides the cross-linking type both sexes xanthan gum that the preparation method is prepared.
In conclusion the present invention provides a kind of cross-linking type both sexes xanthan gum and preparation method thereof.Xanthan gum of the invention
It has the advantages that
1. the preparation process of cross-linking type both sexes xanthan gum is simple, raw material is easy to get, and amount of modifier is few, and modification is at low cost.
2. cross-linking type both sexes xanthan gum has degradability, no pollution to the environment is a kind of environment-friendly materials.
3. the viscoelastic property and network structure of cross-linking type both sexes xanthan gum are been significantly enhanced compared to xanthan gum, it is used for
When fracturing fluid, thickening agent dosage can be not only reduced, but also the viscoelastic property of fracturing fluid can be improved, to reduce cost.
Detailed description of the invention
Fig. 1 is the apparent viscosity comparison of rear xanthan gum solution before modified.
Fig. 2 is the viscoelastic property of rear xanthan gum solution before modified.
Fig. 3 is the thixotropic property of rear xanthan gum solution before modified.
Fig. 4 is the temperature and shearing sustainability of modified xantham gum solution.
Specific embodiment
Below by way of the beneficial effect of the specific embodiment implementation process that the present invention will be described in detail and generation, it is intended to which help is read
Reader more fully understands essence and feature of the invention, does not limit the scope of the present invention.
Embodiment 1
Prepare modified xantham gum: under the conditions of being stirred at room temperature, in the mixed solvent of 100 parts of isopropanol-waters (mass ratio 8:2)
In, 0.25 part of sodium hydroxide is added, stirs evenly, adds 10 parts of xanthan rubber powders, stirring makes it suspend uniformly, in 20 DEG C of temperature
Under degree, alkalize 1 hour；Then 0.5 part of 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride is added and carries out etherification reaction, in 55 DEG C of temperature
Under degree, react 2 hours；Add 0.15 part of epoxychloropropane and carry out cross-linking reaction, 70 DEG C at a temperature of, react 1 hour；Most
System is cooled to room temperature afterwards, is respectively that 60%, 80%, 90% ethanol solution and dehydrated alcohol wash filtering 4 with mass concentration
It is secondary, in 60 DEG C of drying 12h or more, cross-linking type both sexes xanthan gum, i.e. modified xantham gum thickening can be obtained after crushing.
Embodiment 2
Prepare modified xantham gum: under the conditions of being stirred at room temperature, in the mixed solvent of 100 parts of isopropanol-waters (mass ratio 8:2)
In, 0.2 part of sodium hydroxide is added, stirs evenly, adds 10 parts of xanthan rubber powders, stirring makes it suspend uniformly, in 20 DEG C of temperature
Under degree, alkalize 0.5 hour；Then the chloro- 2- hydroxypropyl triethylammonium chloride of 0.3 part of 3- is added and carries out etherification reaction, at 70 DEG C
At a temperature of, it reacts 1 hour；Add 0.17 part of epoxychloropropane and carry out cross-linking reaction, 50 DEG C at a temperature of, react 3 hours；
Finally system is cooled to room temperature, is respectively that 60%, 80%, 90% ethanol solution and dehydrated alcohol wash filtering with mass concentration
4 times, in 60 DEG C of drying 12h or more, cross-linking type both sexes xanthan gum, i.e. modified xantham gum thickening can be obtained after crushing.
Embodiment 3
Prepare modified xantham gum: under the conditions of being stirred at room temperature, in the mixed solvent of 100 parts of alcohol-waters (mass ratio 8:2)
In, 0.3 part of sodium hydroxide is added, stirs evenly, adds 10 parts of xanthan rubber powders, stirring makes it suspend uniformly, in 20 DEG C of temperature
Under degree, alkalize 1 hour；Then the chloro- 2- hydroxypropyl triethylammonium chloride of 0.4 part of 3- is added and carries out etherification reaction, in 60 DEG C of temperature
Under degree, react 3 hours；Add 0.2 part of epoxychloropropane and carry out cross-linking reaction, 60 DEG C at a temperature of, react 2 hours；Most
System is cooled to room temperature afterwards, is respectively that 60%, 80%, 90% ethanol solution and dehydrated alcohol wash filtering 4 with mass concentration
It is secondary, in 60 DEG C of drying 12h or more, cross-linking type both sexes xanthan gum, i.e. modified xantham gum thickening can be obtained after crushing.
Test example 1
This test example is used to detect 0.4% modified xantham gum thickening that 1-3 of the embodiment of the present invention is prepared water-soluble
Apparent viscosity (170s in liquid-1), test equipment uses RheolabQC rheometer, and test result is shown in Table 1.
Table 1
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Apparent viscosity (25 DEG C)/mPas | 128.66 | 126.55 | 140.23 |
Test example 2
This test example is used to compare the performance of xanthan rubber powder and the modified xantham gum in embodiment 1.
The apparent viscosity of xanthan gum after comparison before modified, in 30 DEG C, 170s-1Under, not using RheolabQC rheometer measurement
The apparent viscosity of same concentration (0.3%-0.6%) xanthan gum solution and modified xantham gum aqueous solution, test result are shown in Fig. 1.Fig. 1
For the apparent viscosity comparison of rear xanthan gum solution before modified, as shown in Figure 1, with modified xantham gum under concentration, (i.e. embodiment 1 is made
Standby cross-linking type both sexes xanthan gum) apparent viscosity be significantly greater than the apparent viscosity of xanthan gum, 0.6% modified xantham gum and
The apparent viscosity of 0.6% xanthan gum is respectively 199mPas and 85mPas, increases 134%.
The viscoelastic property of xanthan gum after comparison before modified, 20 DEG C, under oscillation mode, using the advanced rotational rheometer of Hakke
II test macro of Mars (rotor model C35/1 ° of TiL, diameter 35.00mm, 1 ° of cone angle), to 0.4% before modified after xanthan gum
Aqueous solution performs a scan (strain γ=1%, angular frequency=0.1~10rad/s), obtains viscoelasticity index G ', G ", tries
It tests result and sees Fig. 2.Fig. 2 is the viscoelastic property of rear xanthan gum solution before modified, and as shown in Figure 2, G ', the G " of modified xantham gum are equal
Greater than G ', the G " of xanthan gum, illustrate that modified xantham gum has better viscoelastic property and stronger network structure.
The thixotropic property of xanthan gum after comparison before modified at 20 DEG C, is tested using the advanced rotational rheometer Mars II of Hakke
System (rotor model C35/1 ° of TiL, diameter 35.00mm, 1 ° of cone angle), to 0.6% before modified after xanthan gum solution carry out
(shear rate first rises to 170s by 0 for thixotropy test-1, time 30s；Again by 170s-1It is down to 0, time 30s), test knot
Fruit sees Fig. 3.Fig. 3 is the thixotropic property of rear xanthan gum solution before modified, from the figure 3, it may be seen that the thixotropic loop area of modified xantham gum
Greater than the thixotropic loop area of xanthan gum, illustrate that the network structure of modified xantham gum formation is better than the network structure of xanthan gum.
Test example 3
This test is for detecting the temperature and shearing sustainability of the modified xantham gum prepared in embodiment 1.
In the 2%KCl aqueous solution of 100mL, 0.4g modified xantham gum is added, is tested after being swollen completely.Test
Method is referring to oil and gas industry standard SY/T5107-2005 " aqueous fracturing fluid method of evaluating performance ", and measuring device is
RS6000 rheometer, as a result referring to fig. 4.
Fig. 4 is the temperature and shearing sustainability of modified xantham gum solution.As shown in Figure 4, the 0.4% of 2%KCl aqueous solution configuration
Modified xantham gum solution is in 120 DEG C, 170s-1Under the conditions of shear 90 minutes after reservation viscosity still have a 61mPas, and 0.4% is yellow
Virgin rubber solution is only 48mPas in 30 DEG C of apparent viscosity (see Fig. 1)；Compared with xanthan gum solution before modified, under concentration
Modified xantham gum has better temperature and shearing sustainability and solid-carrying performance.
Claims (8)
1. a kind of preparation method of cross-linking type both sexes xanthan gum, wherein the method includes in a solvent first using alkali to xanthan
Glue alkalizes, and then carries out etherification reaction to the xanthan gum after alkalization using cationic etherifying agent, finally reuses crosslinking agent
Cross-linking reaction is carried out to the xanthan gum after etherificate, obtains the cross-linking type both sexes xanthan gum；By xanthan gum quality be 10 parts in terms of,
The quality dosage of alkali, cationic etherifying agent and crosslinking agent is respectively 0.2-0.3 parts, 0.3-0.5 parts and 0.1-0.2 parts；The sun
Ion etherifying agent is selected from 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride, the chloro- 2- hydroxypropyl triethylammonium chloride of 3- and the chloro- 2- hydroxyl of 3-
The one or more of propyl tripropyl ammonium chloride, the crosslinking agent are epoxychloropropane or sodium trimetaphosphate；The alkalization includes
Xanthan gum is added in alcohol/aqueous solution of alkali, 0.5-1h is stirred at room temperature；The etherification reaction is that cationic etherifying agent is added instead
It answers in solution, reacts 1-3h at 55-70 DEG C；The cross-linking reaction is that crosslinking agent is added in reaction solution, at 50-70 DEG C
React 1-3h.
2. preparation method according to claim 1, wherein the alkali is sodium hydroxide or potassium hydroxide.
3. preparation method according to claim 1, wherein the alcohol is one of methanol, ethyl alcohol and isopropanol or more
The mixing of kind.
4. preparation method according to claim 1, wherein the solvent quality dosage is 4-10 times of xanthan gum quality.
5. preparation method according to claim 1, wherein the volumetric concentration of the alcohol/aqueous solution is 70%-85%.
6. preparation method according to claim 1, wherein the reaction further includes that will react molten after the completion of cross-linking reaction
Liquid is cooled to room temperature, and filtering washs away the complete reactant of unreacted with ethanol aqueous wash, and then drying obtains the cross-linking type
Both sexes xanthan gum.
7. preparation method according to claim 6, wherein the reaction further includes that will react molten after the completion of cross-linking reaction
Liquid is cooled to room temperature, and filtering filters filter cake with the ethanol water of mass concentration 60-70% and filter cake, so after mixing
It is successively repeated the above steps with the ethanol water of 70-80%, 80-90%, 100%, is finally filtered again afterwards, then in 50-60
DEG C drying 10-15h, obtain the cross-linking type both sexes xanthan gum.
8. the cross-linking type both sexes xanthan gum that preparation method described in claim 1~7 any one is prepared.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104974266A (en) * | 2014-04-10 | 2015-10-14 | 中国石油化工股份有限公司 | Etherification-modified microorganism gum and preparation method thereof, water-base gel fracturing fluid containing the microorganism gum and application thereof |
| CN105820264A (en) * | 2016-04-15 | 2016-08-03 | 北京化工大学 | Modified xanthan gum, preparation method thereof and fracturing fluid containing modified xanthan gum |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104974266A (en) * | 2014-04-10 | 2015-10-14 | 中国石油化工股份有限公司 | Etherification-modified microorganism gum and preparation method thereof, water-base gel fracturing fluid containing the microorganism gum and application thereof |
| CN105820264A (en) * | 2016-04-15 | 2016-08-03 | 北京化工大学 | Modified xanthan gum, preparation method thereof and fracturing fluid containing modified xanthan gum |
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| Title |
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| 三偏磷酸钠交联黄原胶的制备及其溶液流变性;刘茹等;《应用化学》;20150930;第32卷(第9期);第1061-1069页 |
| 环氧氯丙烷交联黄原胶溶液的流变及抗温性能;杨婷婷等;《高分子材料科学与工程》;20150531;第31卷(第5期);第39-43页 |
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