CN103788220A - Preparation method of instant hydroxypropyl guar - Google Patents
Preparation method of instant hydroxypropyl guar Download PDFInfo
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- CN103788220A CN103788220A CN201210435549.4A CN201210435549A CN103788220A CN 103788220 A CN103788220 A CN 103788220A CN 201210435549 A CN201210435549 A CN 201210435549A CN 103788220 A CN103788220 A CN 103788220A
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- hydroxypropyl guar
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Abstract
The invention provides a preparation method of instant hydroxypropyl guar. The method comprises the following steps: a, adding 100 parts by weight of raw guar powder and 50 to 300 parts by weight of weak-polar or non-polar solvent to a high-pressure reaction kettle under room temperature, uniformly agitating, then dropwise adding 10 to 50 parts by weight of basic catalyst aqueous solution at the mass concentration of 20 to 80% under agitating, and soaking and alkalifying for 20 to 100 minutes; b, adding 5 to 20 parts by weight of nonionic etherifying agent and 1 to 5 parts by weight of rate-accelerating additives to the alkalified guar dispersoid during agitating, charging nitrogen and pressurizing to be 0.1 to 0.4MPa, and reacting for 4 to 6 hours under the temperature of 25 to 80 DEG C; and c, neutralizing with acid until reaching pH (Power of Hydrogen) of 6 to 8 after the reaction is done, and then performing suction filtration, drying, and crushing to obtain the instant hydroxypropyl guar.
Description
Technical field
The present invention relates to a kind of preparation method of instant type hydroxypropyl guar gum.
Background technology
Waterfrac treatment is to utilize ground high-pressure pump group, with the discharge capacity that exceedes formation absorption ability, high-viscous liquid (fracturing liquid) is pumped in well, has suppressed high pressure in shaft bottom, reaches after tensile strength of rock, just in generation crack, shaft bottom when this pressure overcomes Around A Borehole terrestrial stress.Continue to inject the fracturing liquid with propping agent, crack continues to extend, and propping agent is filling in crack.After termination of pumping, due to the supporting role of propping agent fracture, can in stratum, form sufficiently long, have the sand packed fracture of certain flow conductivity.The Fracturing of Oil/gas Well is the effective ways of transformation hydrocarbon zone, is the effective measure of Oil/gas Well, well volume increase, augmented injection.This technology has accumulated the experience of more than 50 year, is widely used in In Oil Field Exploration And Development.
Main water-based fracturing liquid system is that organic boron is linking agent take melon glue or derivatives thereof as thickening material at present, and adds the fracturing fluid system that other additives form.Melon glue is a kind of natural polygalactomannan, belongs to non-ionic type polymer.Structurally, take the interconnective D-MANNOSE of β-Isosorbide-5-Nitrae key unit as main chain, on the C6 position of some D-MANNOSE unit of main chain, connect again single D-semi-lactosi (β-1 unevenly, 6 keys) be side chain, its semi-lactosi is about 1: 1.8 with the ratio of seminose.
Traditional melon glue class aqueous fracturing fluid base fluid preparation method is: in wet tank or dosing pond, add clear water, with liquid distributing vehicle or dosing pump suction melon glue or guar gum derivative, 15-30min is dissolved in circulation, measure after soltion viscosity reaches requirement and dissolve fracturing fluid additive (comprising clay stabilizer, cleanup additive, sterilant etc.), finally add pH adjusting agent, after placement 4h, can use.In the time of pressing crack construction, fracturing liquid base fluid is pumped to truck-mounted blender, on truck-mounted blender, adds linking agent, gel breaker and propping agent, then by pressure break pump truck, fracturing fluid gel and propping agent are pumped in crack, shaft bottom.Traditional melon glue class fracturing liquid compound method has long, the shortcoming such as obtaining liq is perishable of process for preparation time, and this is mainly by melon glue or guar gum derivative dissolution rate is low causes.If can improve the dissolution rate of melon glue or guar gum derivative, just can before pressing crack construction, prepare all fracturing liquid base fluids, but at pressing crack construction preparing fracturing fluid simultaneously, realize fracturing liquid and prepare online, reach the object of saving fracturing liquid cost, improving pressing crack construction efficiency.
The online preparation of fracturing liquid or continuously mixture are the technology of preparing fracturing fluid in pressing crack construction, are mainly made up of fracturing liquid technology and construction technology technology.The essence of the online compounding process of fracturing liquid is the quick dissolving that reaches thickening material within the shorter dosing time, and therefore requiring is that thickening material dissolves rapidly, proposes thus the concept of instant type hydroxypropyl guar gum.Instant type melon glue product is had to certain research both at home and abroad.Us 4828034, us 5046856, us 6387853, us 7497263 etc. have proposed preparation and the application method of instant type melon glue product, and apparent viscosity when general instant type melon glue product 3min dissolution time reaches the more than 80% of final viscosity.If can further improve the dissolution rate of instant type melon glue product, just can within the shorter time, realize of the fracturing fluid preparation, thereby can improve pressing crack construction scale and discharge capacity, simplify uphole equipment configuration.
Summary of the invention
The object of this invention is to provide a kind of solubility property that can further improve instant type melon glue product, realize 1min and dissolve percentage ratio and reach the preparation method of the instant type hydroxypropyl guar gum of more than 80% dissolution rate.
Object of the present invention can be achieved by the following technical measures:
The preparation method of this instant type hydroxypropyl guar gum carries out as follows:
A. under room temperature, in autoclave, add 100 weight part melon collagen powder and 50-300 weight part weight part low-pole or non-polar solvent, stir, the alkaline catalyst solution that is then 20-80% in the mass concentration that stirs the lower 10-50 of dropping weight part again, soaks alkalization; Then logical nitrogen is forced into 0.1-0.4MPa, then is down to normal pressure, repeats 3 times;
B. the melon glue dispersion after alkalization is added to 5-20 weight part nonionic etherifying agent and 1-5 weight part rate accelerating material(RAM) under stirring, then logical nitrogen is forced into 0.1-0.4MPa and reacts 4-6h at 25-80 ℃;
C., after reaction finishes, be neutralized to pH=6-8 with acid, through suction filtration, dry, pulverize, obtain product.
Object of the present invention also can be achieved by the following technical measures:
Immersion alkalization time described in above-mentioned a step is 20-100min; Low-pole described in a step or non-polar solvent are selected from methyl alcohol, ethanol, n-propyl alcohol, Virahol, sherwood oil, acetone, tetrahydrofuran (THF) or methyl-sulphoxide; Basic catalyst described in a step is selected from sodium hydroxide, potassium hydroxide, thanomin, diethanolamine, trolamine or choline, wherein preferred sodium hydroxide; Nonionic etherifying agent described in b step is selected from propylene oxide; Rate accelerating material(RAM) described in b step is Repone K, sodium-chlor, ammonium chloride, sodium formiate, sodium acetate, potassium formiate or potassium acetate, wherein preferable formic acid potassium; Acid described in c step is hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid or acetic acid, wherein preferred acetic acid.
The Main Function of rate accelerating material(RAM) is to reduce Hyarogen-bonding between melon xanthan molecule, improves product dissolution rate.
Instant type hydroxypropyl guar gum method for testing performance:
Get 20 ℃ of clear water 350mL and add the mixed tolerance cup of adjusting, add therein 4-5 to drip Span80, adjust the mixed device voltage of adjusting to 30V, add 2.1g melon glue base polymer, start timing; After dissolving 45s, stop stirring, liquid is poured into six fast viscometer measuring cups in 15s and packed into six fast viscometers and measure, 300rpm(511s
-1) time recording liquid apparent viscosity η
1, apparent viscosity when viscosity number is now instant melon peptization solution 1min; Keep six fast viscometer 300rpm, continuously stirring 20min, when 20min, liquid apparent viscosity is basicly stable, records the now apparent viscosities il of liquid
20.Instant type hydroxypropyl guar gum 1min dissolves percentage ratio to be seen described in following formula:
Instant type hydroxypropyl guar gum 1min prepared by the inventive method dissolves percentage ratio can reach 80%-90%, and viscosity can reach 105-110mPa s, and water-insoluble reaches 3.5%-5.0%.
The present invention has improved the chemical preparation process of instant type hydroxypropyl guar gum, the instant type hydroxypropyl guar gum of preparation has further improved the dissolution rate of instant type melon glue product, thereby within the shorter time, realize of the fracturing fluid preparation, pressing crack construction scale and discharge capacity are improved, simplify uphole equipment configuration, further improve its solubility property, realized 1min dissolving percentage ratio and reached more than 80% dissolution rate.
Embodiment:
Embodiment 1:
The method is carried out as follows:
A. under room temperature, in autoclave, add 100 weight part melon collagen powder and 50 weight part industrial methanols, stir, then, again in stirring the aqueous sodium hydroxide solution that the lower mass concentration that drips 10 weight parts is 50%, soak alkalization 20min; Then logical nitrogen is forced into 0.3MPa, then is down to normal pressure, repeats 3 times;
B. the melon glue dispersion after alkalization is added to 5 weight part propylene oxide and 1 weight part Repone K under stirring, then logical nitrogen is forced into 0.1MPa and reacts 6h at 80 ℃;
C., after reaction finishes, be neutralized to pH=6 with hydrochloric acid, through vacuum filtration, methanol wash, dry, pulverize, obtain product.
Embodiment 2:
The method is carried out as follows:
A. under room temperature, in autoclave, add 100 weight part melon collagen powder and 300 weight part industrial methanols, stir, then, again in stirring the aqueous sodium hydroxide solution that the lower mass concentration that drips 50 weight parts is 20%, soak alkalization 100min; Then logical nitrogen is forced into 0.5MPa, then is down to normal pressure, repeats 3 times;
B. the melon glue dispersion after alkalization is added to 20 weight part propylene oxide and 5 weight part Repone K under stirring, then logical nitrogen is forced into 0.4MPa and reacts 4h at 25 ℃;
C., after reaction finishes, be neutralized to pH=7 with hydrochloric acid, through vacuum filtration, methanol wash, dry, pulverize, obtain product.
Embodiment 3:
The method is carried out as follows:
A. under room temperature, in autoclave, add 100 weight part melon collagen powder and 150 weight part industrial methanols, stir, then, again in stirring the aqueous sodium hydroxide solution that the lower mass concentration that drips 30 weight parts is 50%, soak alkalization 60min; Then logical nitrogen is forced into 0.4MPa, then is down to normal pressure, repeats 3 times;
B. the melon glue dispersion after alkalization is added to 10 weight part propylene oxide and 2 weight part Repone K under stirring, then logical nitrogen is forced into 0.2MPa and reacts 5h at 50 ℃;
C., after reaction finishes, be neutralized to pH=6.5 with hydrochloric acid, through vacuum filtration, low-pole or non-polar solvent washing, dry, pulverize, obtain product.
Embodiment 4:
Different is to replace methyl alcohol with ethanol, and all the other are respectively with embodiment 1-3.
Embodiment 5:
Different is to replace methyl alcohol with n-propyl alcohol, and all the other are respectively with embodiment 1-3.
Embodiment 6:
Different is to replace methyl alcohol with Virahol, and all the other are respectively with embodiment 1-3.
Embodiment 7:
Different is to replace methyl alcohol with sherwood oil, and all the other are respectively with embodiment 1-3.
Embodiment 8:
Different is to replace methyl alcohol with acetone, and all the other are respectively with embodiment 1-3.
Embodiment 9:
Different is to replace methyl alcohol with tetrahydrofuran (THF), and all the other are respectively with embodiment 1-3.
Embodiment 10:
Different is to replace methyl alcohol with methyl-sulphoxide, and all the other are respectively with embodiment 1-3.
Embodiment 11:
Different is to replace sodium hydroxide with potassium hydroxide, and all the other are respectively with embodiment 1-10.
Embodiment 12:
Different is to replace sodium hydroxide with thanomin, and all the other are respectively with embodiment 1-10.
Embodiment 13:
Different is to replace sodium hydroxide with diethanolamine, and all the other are respectively with embodiment 1-10.
Embodiment 14:
Different is to replace sodium hydroxide with trolamine, and all the other are respectively with embodiment 1-10.
Embodiment 15:
Different is to replace sodium hydroxide with choline, and all the other are respectively with embodiment 1-10.
Embodiment 16:
Different is to replace propylene oxide with oxyethane, and all the other are respectively with embodiment 1-15.
Embodiment 17:
Different is to replace Repone K with sodium-chlor, and all the other are respectively with embodiment 1-16.
Embodiment 18:
Different is to replace Repone K with ammonium chloride, and all the other are respectively with embodiment 1-16.
Embodiment 19:
Different is to replace Repone K with sodium formiate, and all the other are respectively with embodiment 1-16.
Embodiment 20:
Different is to replace Repone K with sodium acetate, and all the other are respectively with embodiment 1-16.
Embodiment 21:
Different is to replace Repone K with potassium formiate, and all the other are respectively with embodiment 1-16.
Embodiment 22:
Different is to replace Repone K with potassium acetate, and all the other are respectively with embodiment 1-16.
Embodiment 23:
Different is to replace hydrochloric acid with sulfuric acid, and all the other are respectively with embodiment 1-22.
Embodiment 24:
Different is to replace hydrochloric acid with nitric acid, and all the other are respectively with embodiment 1-22.
Embodiment 25:
Different is to replace hydrochloric acid with phosphoric acid, and all the other are respectively with embodiment 1-22.
Embodiment 26:
Different is to replace hydrochloric acid with formic acid, and all the other are respectively with embodiment 1-22.
Embodiment 27:
Different is to replace hydrochloric acid with acetic acid, and all the other are respectively with embodiment 1-22.
Claims (10)
1. a preparation method for instant type hydroxypropyl guar gum, is characterized in that the method carries out as follows:
A. under room temperature, in autoclave, add 100 weight part melon collagen powder and 50-300 weight part low-pole or non-polar solvents, stir, the alkaline catalyst solution that is then 20-80% in the mass concentration that stirs the lower 10-50 of dropping weight part again, soaks alkalization;
B. the melon glue dispersion after alkalization is added to 5-20 weight part nonionic etherifying agent and 1-5 weight part rate accelerating material(RAM) under stirring, then logical nitrogen is forced into 0.1-0.4MPa and reacts 4-6h at 25-80 ℃;
C., after reaction finishes, be neutralized to pH=6-8 with acid, through suction filtration, dry, pulverize, obtain product.
2. the preparation method of a kind of instant type hydroxypropyl guar gum according to claim 1, is characterized in that the immersion alkalization time described in a step is 20-100min.
3. the preparation method of a kind of instant type hydroxypropyl guar gum according to claim 1, is characterized in that low-pole or the non-polar solvent described in a step is methyl alcohol, ethanol, n-propyl alcohol, Virahol, sherwood oil, acetone, tetrahydrofuran (THF) or methyl-sulphoxide.
4. the preparation method of a kind of instant type hydroxypropyl guar gum according to claim 1, is characterized in that the basic catalyst described in a step is sodium hydroxide, potassium hydroxide, thanomin, diethanolamine, trolamine or choline.
5. the preparation method of a kind of instant type hydroxypropyl guar gum according to claim 1, is characterized in that the nonionic etherifying agent described in b step is selected from propylene oxide.
6. the preparation method of a kind of instant type hydroxypropyl guar gum according to claim 1, is characterized in that the rate accelerating material(RAM) described in b step is Repone K, sodium-chlor, ammonium chloride, sodium formiate, sodium acetate, potassium formiate or potassium acetate.
7. the preparation method of a kind of instant type hydroxypropyl guar gum according to claim 1, is characterized in that the acid described in c step is hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, formic acid or acetic acid.
8. the preparation method of a kind of instant type hydroxypropyl guar gum according to claim 4, is characterized in that described basic catalyst is sodium hydroxide.
9. the preparation method of a kind of instant type hydroxypropyl guar gum according to claim 6, is characterized in that described rate accelerating material(RAM) is potassium formiate.
10. the preparation method of a kind of instant type hydroxypropyl guar gum according to claim 7, is characterized in that described acid is acetic acid.
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| CN201210435549.4A CN103788220B (en) | 2012-11-05 | 2012-11-05 | A kind of preparation method of Instant hydroxypropyl guar gum |
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Cited By (2)
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| CN104262498A (en) * | 2014-08-27 | 2015-01-07 | 北京林业大学 | Method for increasing viscosity of guar gum |
| CN104312571A (en) * | 2014-09-17 | 2015-01-28 | 华东理工大学 | Modified xanthan gum thickener and its application in preparation of fracturing fluid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262498A (en) * | 2014-08-27 | 2015-01-07 | 北京林业大学 | Method for increasing viscosity of guar gum |
| CN104262498B (en) * | 2014-08-27 | 2018-11-23 | 北京林业大学 | A kind of method that Guar polysaccharide gum increases viscosity |
| CN104312571A (en) * | 2014-09-17 | 2015-01-28 | 华东理工大学 | Modified xanthan gum thickener and its application in preparation of fracturing fluid |
| CN104312571B (en) * | 2014-09-17 | 2017-07-14 | 华东理工大学 | A kind of modified xantham gum thickening and its application in fracturing fluid is prepared |
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| CN103788220B (en) | 2016-12-21 |
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