CN109499105A - Simethicone emulsion and preparation method thereof for fracturing outlet liquid defoaming - Google Patents
Simethicone emulsion and preparation method thereof for fracturing outlet liquid defoaming Download PDFInfo
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- CN109499105A CN109499105A CN201811407238.0A CN201811407238A CN109499105A CN 109499105 A CN109499105 A CN 109499105A CN 201811407238 A CN201811407238 A CN 201811407238A CN 109499105 A CN109499105 A CN 109499105A
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- simethicone emulsion
- outlet liquid
- fracturing outlet
- silicon cream
- liquid defoaming
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0409—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
Abstract
The invention discloses a kind of simethicone emulsions and preparation method thereof for fracturing outlet liquid defoaming, including 10~20 parts of silicon cream, 3~5 parts of emulsifiers, 0.5~0.8 part of thickener and 0.6~1 part of alkali or basic salt in parts by weight.Wherein, silicon cream is mixed with by the dimethicone and fumed silica that weight ratio is 100:4, and the specific surface area of fumed silica is 150~200m2/ g, the viscosity of dimethicone are 350~1000mPas；It is in successively alkaline aqueous thickener solution and high-speed stirred is mixed to get by being prepared silicon cream using dimethicone and fumed silica, matched emulsifier being added into silicon cream, mix；The simethicone emulsion is the emulsion of stable homogeneous, has good antifoaming performance and water dispersible, and production cost is more commercially available and has the defoaming agent cost savings 30% of suitable performance, has the application of good market and promotional value.
Description
Technical field
The present invention relates to oil gas fields to defoam technical field of operation, in particular to a kind of diformazan for fracturing outlet liquid defoaming
Base silicone oil emulsion and preparation method thereof.
Background technique
It is led at present to improve the row of returning after pressing crack construction, foaming agent is usually added in fracturing fluid, lifting rate is returned in increase
The fracturing fluid being detained in the earth formation is reduced, the injury to stratum is mitigated, improves fracturing effect.During the row of returning, in high pressure gas
A large amount of foams can be generated with drain is returned under the action of foaming agent, the environmental problems such as tank boil-overs, liquid pouring pump effect reduction is generated and production is asked
Topic.With the continuous improvement of environmental requirement, returning after drain has to pass through defoaming treatment can be just further processed.It adopts at scene
Problem above is solved with the mode of addition defoaming agent.Currently used defoaming agent includes polyethers and organic silicon, wherein having
Machine silicon class defoaming agent antifoaming speed is fast, foam inhibition effect is good, is widely used in the industries such as food, papermaking, printing and dyeing, petrochemical industry.
Publication CN103041623A provides a kind of silicone antifoaming agent, by two kinds of silicone oil with it is white
Main component of the mixture of carbon black (fumed silica) composition as defoaming agent, by multiple types surfactant as cream
Agent；However the organic silicon defoamer component is more, production technology is also more complicated.Publication CN103830938A is public
The preparation method for having opened a kind of organic silicon defoamer, by dimethicone and white carbon black, i.e., fumed silica composition is mixed
Close object and be used as defoaming agent main component, emulsifier in Tween-60, Arlacel-40 or polyether silicone oil at least any one, so
And defoaming agent effect in practical emulsion process is poor, and without addition stabilizer in system, the stability of emulsion of generation is poor.
Publication CN106237662A provides a kind of preparation method of organic silicon defoamer, the defoaming agent of preparation it is main at
It is divided into silicon composition and polyether-modified polysiloxane, needs to make when leading to the higher cost of the defoaming agent, and preparing
With colloid mill, technique is cumbersome.
Summary of the invention
The object of the present invention is to provide it is a kind of low cost and meet oil gas field produced on-site quickly defoam require be used for press
Split the simethicone emulsion for returning drain defoaming.
It is a further object of the present invention to provide a kind of preparation methods for preparing above-mentioned simethicone emulsion.
For this purpose, technical solution of the present invention is as follows:
A kind of simethicone emulsion for fracturing outlet liquid defoaming, including 10~20 parts of silicon cream, 3 in parts by weight
~5 parts of emulsifiers, 0.5~0.8 part of thickener and 0.6~1 part of alkali or basic salt.Wherein, silicon cream is the two of 100:4 by weight ratio
Methyl-silicone oil and fumed silica are mixed with, and the specific surface area of fumed silica is 150~200m2/ g, diformazan
The viscosity of base silicone oil is 350~1000mPas.
It is preferred that the viscosity of dimethicone is 500mPas.
It is preferred that the specific surface area 160m of fumed silica2/g。
It is preferred that the emulsifier is to include assistant for emulsifying agent and at least one polyoxyethylated alkyl alcohol, the weight ratio of the two
For 1:2.5~4.5；Wherein, the assistant for emulsifying agent is long-chain fatty alcohol；The molecular formula of the polyoxyethylated alkyl alcohol: RmO
(CH2CH2O)nIn H, RmThe alkane for being 12~14 for carbon number, polymerization degree n value are 12~16.
It is further preferred that the polyoxyethylated alkyl alcohol is the compounding mixture of three kinds of polyoxyethylated alkyl alcohols, three kinds poly-
The molecular formula of ethylene oxide alkyl alcohol ether is followed successively by R12O(CH2CH2O)12H、R14O(CH2CH2O)14H and R14O(CH2CH2O)16H, three
Person's mass ratio is 1:(1.2~3): (1.8~2)；The assistant for emulsifying agent is positive hexadecanol.
Wherein, in practical applications, in polyoxyethylated alkyl alcohol mixture the mass ratio of three kinds of components according to dimethyl
The difference of silicon oil viscosity, adjusts within the above range, is mutually applicable in the viscosity with dimethicone.
Mentioned emulsifier specific the preparation method comprises the following steps: one or more polyoxyethylated alkyl alcohols are dissolved in aqueous solvent,
It is stirred under the conditions of 500r/min, and is warming up to 50 DEG C, then improved revolving speed to 1000r/min, added with the speed of 150mL/min
Enter assistant for emulsifying agent, stirring 30min is further continued for after being added dropwise to get compound emulsifying agent is arrived；The dosage of the aqueous solvent is polyoxy
20~35 times of vinyl alkyl alcohol ether and assistant for emulsifying agent total weight.
It is preferred that the thickener is hydroxypropyl guar, carboxymethyl guanidine glue, sodium carboxymethylcellulose or polyvinyl alcohol.It is more excellent
Choosing, the thickener are hydroxypropyl guar.
It is preferred that the alkali or basic salt are sodium carbonate, sodium hydroxide or sodium bicarbonate.
It is further preferred that the alkali or basic salt are sodium carbonate, and its additional amount is identical as the additional amount of the thickener.
A kind of preparation method of the simethicone emulsion for fracturing outlet liquid defoaming, steps are as follows:
S1, dimethicone and fumed silica are uniformly mixed under the conditions of 140~170 DEG C, form silicon cream；
Emulsifier is added into silicon cream to 50~70 DEG C, and emulsifier is mixed with silicon cream for S2, the temperature for reducing silicon cream
It is even；
S3, thickener, alkali or basic salt are dissolved in the aqueous thickener solution being configured in deionized water in alkalinity；
S4, under the mixing speed of 500~1000r/min, will in alkalinity aqueous thickener solution be added to be mixed with emulsification
In the silicon cream of agent, and continue to stir 0.5h after addition to get the simethicone emulsion for arriving stable homogeneous.
It is preferred that in step S3, preparation in alkalinity aqueous thickener solution when, the dosage of aqueous solvent be thickener and alkali (or
Basic salt) 45~50 times of gross mass；And in step S4, prepare in alkalinity aqueous thickener solution to emulsifier with
The speed being added in the mixture of silicon cream is 200mL/min.
Compared with prior art, the simethicone emulsion stable homogeneous for being used for fracturing outlet liquid defoaming has good
Antifoaming performance and water dispersible, and production cost it is more commercially available and with suitable performance defoaming agent cost savings 30%, tool
There are good market application and promotional value.
Specific embodiment
The present invention is described further combined with specific embodiments below, but following embodiments absolutely not to the present invention have appoint
What is limited.
Embodiment 1
A kind of simethicone emulsion for fracturing outlet liquid defoaming, the preparation method is as follows:
Step 1: preparing emulsifier: being 1:1.2:1.8, molecular formula R by mass ratio12O(CH2CH2O)12H、R14O
(CH2CH2O)14H and R14O(CH2CH2O)16Tri- kinds of polyoxyethylated alkyl alcohols of H are dissolved in aqueous solvent as primary emulsion,
Stirring is warming up to 50 DEG C under the conditions of 500r/min；Then improve revolving speed to 1000r/min, by the positive hexadecanol of assistant for emulsifying agent according to
The ratio that primary emulsion total mass ratio is 1:2.5 is added, and continues to stir 30min after being added dropwise to get to suitable for emulsification viscosity
For the compound emulsifying agent of the dimethicone of 350mPas；Wherein, the dosage of the aqueous solvent is three kinds of polyxyethylated alcohol
20 times of ether and assistant for emulsifying agent total weight, the addition speed of positive hexadecanol are 150mL/min；
Step 2: preparing simethicone emulsion: being 350mPas dimethicone and 150m by viscosity2/ g gas phase two
Silica 100:4 in mass ratio mixing, and be warming up to and stirred evenly at 140 DEG C, obtain silicon cream；Successively weigh 20 parts of silicon cream, creams
Then silicon cream and emulsifier are added in a kettle, is warming up to 50 for 3 parts of agent, 0.8 part of hydroxypropyl guar and 0.8 part of sodium carbonate
After DEG C, then hydroxypropyl guar and sodium carbonate be dissolved in deionized water, obtain then existing in the hydroxypropyl guar aqueous solution of alkalinity
It will be added in reaction kettle in the hydroxypropyl guar aqueous solution of alkalinity under 1000r/min mixing speed, continue to stir after addition
0.5h obtains the simethicone emulsion of stable homogeneous；Wherein, when preparation is in alkaline hydroxypropyl guar aqueous solution, aqueous solvent
Dosage be 45 times of gross mass of hydroxypropyl guar and sodium carbonate, the addition speed being added into emulsifier and silicon cream is
200mL/min。
Embodiment 2
A kind of simethicone emulsion for fracturing outlet liquid defoaming, the preparation method is as follows:
Step 1: being 1:2.2:2, molecular formula R by mass ratio12O(CH2CH2O)12H、R14O(CH2CH2O)14H and R14O
(CH2CH2O)16Tri- kinds of polyoxyethylated alkyl alcohols of H are soluble in water as primary emulsion, and heating is stirred under the conditions of 500r/min
To 50 DEG C；Then it improves revolving speed to 1000r/min, according to primary emulsion total mass ratio is 1:3 by the positive hexadecanol of assistant for emulsifying agent
Ratio be added, continue after being added dropwise stir 30min to get to be suitable for emulsify viscosity be 500mPas dimethicone
Compound emulsifying agent；Wherein, the dosage of the aqueous solvent is the 26 of three kinds of polyoxyethylated alkyl alcohols and assistant for emulsifying agent total weight
Times, the addition speed of positive hexadecanol is 150mL/min；
Step 2: preparing simethicone emulsion: being 500mPas dimethicone and 160m by viscosity2/ g gas phase two
Silica 100:4 in mass ratio mixing, and be warming up to and stirred evenly at 150 DEG C, obtain silicon cream；Successively weigh 15 parts of silicon cream, creams
Then silicon cream and emulsifier are added in a kettle, is warming up to 60 for 4 parts of agent, 0.8 part of carboxymethyl guanidine glue and 1 part of sodium bicarbonate
After DEG C, then carboxymethyl guanidine glue and sodium bicarbonate are dissolved in deionized water and obtain then existing in the carboxymethyl guanidine glue solution of alkalinity
It will be added in reaction kettle in the carboxymethyl guanidine glue solution of alkalinity under the mixing speed of 1000r/min, continue to stir after addition
0.5h is mixed, the simethicone emulsion of stable homogeneous is obtained；Wherein, when preparation is in alkaline carboxymethyl guanidine glue solution, solvent
The dosage of water is 46 times of the gross mass of carboxymethyl guanidine glue and sodium bicarbonate, and the addition speed into emulsifier and silicon cream is added
For 200mL/min.
Embodiment 3
A kind of simethicone emulsion for fracturing outlet liquid defoaming, the preparation method is as follows:
Step 1: being 1:2.5:2, molecular formula R by mass ratio12O(CH2CH2O)12H、R14O(CH2CH2O)14H and R14O
(CH2CH2O)16Tri- kinds of polyoxyethylated alkyl alcohols of H are soluble in water as primary emulsion, and heating is stirred under the conditions of 500r/min
To 50 DEG C；Then it improves revolving speed to 1000r/min, according to primary emulsion total mass ratio is 1 by the positive hexadecanol of assistant for emulsifying agent:
3.5 ratio is added, and continues to stir 30min after being added dropwise to get to suitable for emulsifying the dimethyl-silicon that viscosity is 700mPas
The compound emulsifying agent of oil；The dosage of the aqueous solvent is 30 times of three kinds of polyoxyethylated alkyl alcohols and assistant for emulsifying agent total weight,
The addition speed of positive hexadecanol is 150mL/min；
Step 2: preparing simethicone emulsion: being 700mPas dimethicone and 180m by viscosity2/ g gas phase two
Silica 100:4 in mass ratio mixing, and be warming up to and stirred evenly at 150 DEG C, obtain silicon cream；Successively weigh 12 parts of silicon cream, creams
Then silicon cream and emulsifier are added in a kettle, is warming up to 50 for 4 parts of agent, 0.5 part of hydroxypropyl guar and 0.8 part of sodium carbonate
After DEG C, then hydroxypropyl guar and sodium carbonate are dissolved in the hydroxypropyl guar aqueous solution obtained in deionized water in alkalinity；Then exist
It will be added in reaction kettle in the hydroxypropyl guar aqueous solution of alkalinity under the mixing speed of 1000r/min, continue to stir after addition
0.5h is mixed, the simethicone emulsion of stable homogeneous is obtained；Wherein, when preparation is in alkaline hydroxypropyl guar aqueous solution, solvent
The dosage of water is 48 times of the gross mass of hydroxypropyl guar and sodium carbonate, and the addition speed being added into emulsifier and silicon cream is
200mL/min。
Embodiment 4
A kind of simethicone emulsion for fracturing outlet liquid defoaming, the preparation method is as follows:
Step 1: being 1:3:2, molecular formula R by mass ratio12O(CH2CH2O)12H、R14O(CH2CH2O)14H and R14O
(CH2CH2O)16Tri- kinds of polyoxyethylated alkyl alcohols of H are soluble in water as primary emulsion, and heating is stirred under the conditions of 500r/min
To 50 DEG C；Then it improves revolving speed to 1000r/min, according to primary emulsion total mass ratio is 1 by the positive hexadecanol of assistant for emulsifying agent:
4.5 ratio is added, and continues to stir 30min after being added dropwise to get to suitable for emulsifying the dimethyl that viscosity is 1000mPas
The compound emulsifying agent of silicone oil；Wherein, the dosage of the aqueous solvent is three kinds of polyoxyethylated alkyl alcohols and assistant for emulsifying agent total weight
35 times, the addition speed of positive hexadecanol is 150mL/min；
Step 2: preparing simethicone emulsion: being 1000mPas dimethicone and 200m by viscosity2/ g gas phase two
Silica 100:4 in mass ratio mixing, and be warming up to and stirred evenly at 170 DEG C, obtain silicon cream；Successively weigh 10 parts of silicon cream, cream
Then silicon cream and emulsifier, heating is added in 5 parts of agent, 0.8 part of sodium carboxymethylcellulose and 0.6 part of sodium carbonate in a kettle
To after 70 DEG C, then sodium carboxymethylcellulose and sodium carbonate are dissolved in deionized water and obtain being in that alkaline sodium carboxymethylcellulose is water-soluble
Liquid will then be added in reaction kettle, addition under the mixing speed of 1000r/min in the sodium carboxymethyl cellulose solution of alkalinity
After continue stir 0.5h, obtain the simethicone emulsion of stable homogeneous；Wherein, preparation is in alkaline carboxymethyl cellulose
When sodium water solution, the dosage of aqueous solvent is 50 times of the gross mass of sodium carboxymethylcellulose and sodium carbonate, is added to emulsifier
It is 200mL/min with the addition speed in silicon cream.
Performance test:
It chooses certain commercially available organic silicon modified by polyether class defoaming agent and returns row for pressure break with what Examples 1 to 4 was prepared
The simethicone emulsion of liquid defoaming carries out performance comparison.Specific experimental method is as follows:
(1) antifoam performance: 200mL foam liquid is poured into high-speed stirred cup, stirs 5min with 3000r/min, blistering is high
Degree in 300mL or so, half foam life period > 300s, be then added with foaming agent defoaming agent identical in quality, while opening stopwatch
Record foam vanishing time；
(2) suds suppressing properties: the solution after above-mentioned antifoam performance is tested will be completed and stirred under 3000r/min revolving speed, recorded
Foam reaches the time of 100mL volume；
(3) centrifugal stability: 8mL defoaming agent being added into 10mL centrifuge tube, is centrifuged with the revolving speed of 3000r/min
Whether 30min, observation lotion are layered；
(4) water dispersible: 0.5g defoaming agent is added in the beaker for filling 100mL water, its dispersion feelings in water is observed
Condition.Wherein, if dispersion is rapid and liquid level is without grease, dispersion performance is excellent；If dispersion is very fast and liquid level is without grease, divide
It is good for dissipating performance；If dispersion is slow, and there is a small amount of floccule in liquid level, then during dispersion performance is；If be not easy to disperse, and floccule compared with
Hardly possible disappears, then dispersion performance is poor.
Test result is as follows shown in table 1.
Table 1:
| Sample ID | Foam time (s) | The foam inhibition time (s) | Centrifugal stability | Water dispersible |
| Embodiment 1 | 46 | > 300 | It is not stratified | It is good |
| Embodiment 2 | 27 | > 300 | It is not stratified | It is excellent |
| Embodiment 3 | 58 | > 300 | It is not stratified | It is good |
| Embodiment 4 | 38 | > 300 | It is not stratified | It is excellent |
| Commercial antifoam agent | 33 | > 300 | It is not stratified | It is excellent |
From table 1 it follows that Examples 1 to 4 preparation simethicone emulsion defoaming agent foam time be 27~
58s, foam inhibition time > 300s, centrifugal stability and the water dispersible that the emulsion of stable homogeneous is obtained after emulsification are preferable, that is, have
There are good antifoaming performance and water dispersible, the performance with the organic silicon modified by polyether class defoaming agent of presently commercially available excellent performance
Quite, but cost is lower, has the application of good market and promotional value.
Claims (10)
1. a kind of simethicone emulsion for fracturing outlet liquid defoaming, which is characterized in that including 10 in parts by weight~
20 parts of silicon cream, 3~5 parts of emulsifiers, 0.5~0.8 part of thickener and 0.6~1 part of alkali or basic salt；Wherein, silicon cream is by weight ratio
It being mixed with for the dimethicone and fumed silica of 100:4, the viscosity of dimethicone is 350~
1000mPas, the specific surface area of fumed silica are 150~200m2/g。
2. the simethicone emulsion according to claim 1 for fracturing outlet liquid defoaming, which is characterized in that described two
The viscosity of methyl-silicone oil is 500mPas.
3. the simethicone emulsion according to claim 1 for fracturing outlet liquid defoaming, which is characterized in that the gas
The specific surface area 160m of aerosil2/g。
4. the simethicone emulsion according to claim 1 for fracturing outlet liquid defoaming, which is characterized in that the cream
Agent be include assistant for emulsifying agent and at least one polyoxyethylated alkyl alcohol, the weight ratio of the two is 1:2.5~4.5；Wherein, institute
Stating assistant for emulsifying agent is long-chain fatty alcohol；The molecular formula of the polyoxyethylated alkyl alcohol: RmO(CH2CH2O)nIn H, RmIt is for carbon number
12~14 alkane, polymerization degree n value are 12~16.
5. the simethicone emulsion according to claim 1 for fracturing outlet liquid defoaming, which is characterized in that described poly-
Ethylene oxide alkyl alcohol ether is the compounding mixture of three kinds of polyoxyethylated alkyl alcohols, the molecular formula of three kinds of polyoxyethylated alkyl alcohols
Respectively R12O(CH2CH2O)12H、R14O(CH2CH2O)14H and R14O(CH2CH2O)16H, three's mass ratio are 1:(1.2~3):
(1.8~2).
6. the simethicone emulsion according to claim 1 for fracturing outlet liquid defoaming, which is characterized in that described to help
Emulsifier is positive hexadecanol.
7. the simethicone emulsion according to claim 1 for fracturing outlet liquid defoaming, which is characterized in that the increasing
Thick dose is hydroxypropyl guar, carboxymethyl guanidine glue, sodium carboxymethylcellulose or polyvinyl alcohol.
8. the simethicone emulsion according to claim 1 for fracturing outlet liquid defoaming, which is characterized in that the alkali
Or basic salt is sodium carbonate, sodium hydroxide or sodium bicarbonate.
9. a kind of preparation method for the simethicone emulsion of fracturing outlet liquid defoaming as described in claim 1, special
Sign is that steps are as follows:
S1, dimethicone and fumed silica are uniformly mixed under the conditions of 140~170 DEG C, form silicon cream；
Emulsifier is added into silicon cream to 50~70 DEG C, and emulsifier is uniformly mixed with silicon cream for S2, the temperature for reducing silicon cream；
S3, thickener, alkali or basic salt are dissolved in the aqueous thickener solution being configured in deionized water in alkalinity；
S4, under the mixing speed of 500~1000r/min, will be added in the aqueous thickener solution of alkalinity to being mixed with emulsifier
In silicon cream, and continue to stir 0.5h after addition to get the simethicone emulsion for arriving stable homogeneous.
10. preparation method according to claim 9, which is characterized in that in the addition speed of the aqueous thickener solution of alkalinity
For 200mL/min.
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Application publication date: 20190322 |