CN109135714A - A kind of preparation method of long-acting antiseptic resistance-reducing agent - Google Patents
A kind of preparation method of long-acting antiseptic resistance-reducing agent Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of long-acting antiseptic resistance-reducing agent, belong to conductive material technical field.Modified powder colloidal sol is mixed with aniline dispersion liquid, and initiator is added, after being stirred to react, filtering is stood, dry, pulverize, be sieved, obtain No. 1 additive；Graphene oxide dispersion is mixed with No. 2 mixed-powders, obtains graphene oxide mixture, graphene oxide mixture is mixed with galla turcica, and zinc acetate is added, after being stirred to react, is filtered, it is dry, obtain No. 2 additives；By No. 1 additive and No. 2 additives during 1:1~2:1 is mixed in mass ratio, and mixing bentonite and mixed metal powder is added, after being stirred, obtains long-acting antiseptic resistance-reducing agent.Gained long-acting antiseptic resistance-reducing agent of the invention has excellent resistance-reducing performance and long-term effect.
Description
Technical field
The invention discloses a kind of preparation methods of long-acting antiseptic resistance-reducing agent, belong to conductive material technical field.
Background technique
With the large-scale development of shale gas, one " shale gas revolution " is started, many countries all start shale gas
Exploration and development plan.Currently, we have also started the upsurge of one investment exploration exploitation in shale gas field.Shale belongs to ultralow
Permeability reservoir, seepage channel needed for can not providing the economic exploitation need to improve the flow conductivity of reservoir by fracturing work
It can be only achieved the purpose of commercial mining.Currently, a small amount of friction reducer, proppant and some additive structures is added in main use in water
At slippery water, pressure break is carried out to reservoir using slippery water as the fracturing technology of working solution.
Different from traditional fracturing fluid, the concentration of polymer is lower in slippery water fracturing fluid, is relatively conventionally formed the pressure break of gel
The viscosity of liquid is low.The main component of slippery water fracturing fluid is water, sliding under conditions of express pump note since water is Newtonian fluid
Slipping water fracturing fluid, turbulent flow phenomenon is serious in flow process in pipeline, there is biggish frictional resistance resistance between fluid and tube wall.Friction
Resistance hinders the flowing of slippery water fracturing fluid in the duct, causes pipeline throughput rate to reduce and increases with energy consumption.
Friction reducer is the chemical assistant for reducing fluid flow resistance.A small amount of high polymer drop resistance is added in fracturing fluid
Agent reduces the flow resistance of fracturing fluid under turbulent condition.Currently, oil gas field is in recovery process mainly with linear glue, guanidine
Based on glue or import friction reducer, linear glue, guanidine glue resistance-reducing efficiency are low and formation damage is big, and import friction reducer is expensive.
Therefore, exploitation of oil-gas field is badly in need of the friction reducer of super quality and competitive price.At present traditional friction reducer effective component be easy to run off cause to drop it is resistive
Decline, long-term effect decline, and due to the not formed conductive path of effective component, keep the resistance reducing effect of product bad, therefore also need
It is studied.
Summary of the invention
The present invention solves the technical problem of: be easy to run off for traditional friction reducer effective component cause to drop it is resistive under
Drop, long-term effect decline, and due to the not formed conductive path of effective component, the problem for keeping the resistance reducing effect of product bad provides
A kind of preparation method of long-acting antiseptic resistance-reducing agent.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
(1) by potassium carbonate, 1.0:4.0~1.2:4.0 is mixed in molar ratio with titanium dioxide, is ground, and calcining obtains pretreatment powder,
It is polished that powder will be pre-processed, calcined again, discharged, drying is washed, obtain mixed-powder, mixed-powder is divided into two parts,
Respectively No. 1 mixed-powder and No. 2 mixed-powders；
(2) No. 1 mixed-powder is mixed with hydrochloric acid 1:80~1:120 in mass ratio, impregnates filtering, repeated to mix, impregnate filtering
After process 2~3 times, wash, it is dry, obtain modified powder；By modified powder and tetrabutylammonium hydroxide solution 1:10 in mass ratio
~1:18 mixing, is stirred, and impregnates, and centrifuge separation removes upper liquid, obtains modified powder colloidal sol；
(3) modified powder colloidal sol is mixed with aniline dispersion liquid 1:3~1:5 in mass ratio, and aniline dispersion liquid quality 0.1 is added
~0.2 initiator after being stirred to react, stands filtering, dry, pulverize, is sieved, obtains No. 1 additive；
(4) graphene oxide dispersion is mixed with No. 2 mixed-powder 8:1~8:2 in mass ratio, after being stirred, must be aoxidized
Graphene oxide mixture is mixed with gallic acid 100:1~150:1 in mass ratio, and oxidation is added by graphene mixture
The zinc acetate that 0.01~0.05 times of graphene mixture quality after being stirred to react, filters, dry, obtains No. 2 additives；
(5) No. 1 additive is mixed with No. 2 additive 1:1~2:1 in mass ratio, and No. 1 additive quality 0.1~0.2 is added
Mixing bentonite and No. 1 0.1~0.3 times of additive quality of mixed metal powder again after being stirred, obtains long-effective corrosion drop
Resist.
Step (1) calcination temperature is 700~880 DEG C.
Step (3) the aniline dispersion liquid is to mix aniline with hydrochloric acid solution 3:10~4:10 in mass ratio, ultrasound point
It dissipates, obtains aniline dispersion liquid.
Step (3) initiator is potassium peroxydisulfate, any one in ammonium persulfate or sodium peroxydisulfate.
Step (4) graphene oxide dispersion is by graphene oxide and dehydrated alcohol 1:150~1 in mass ratio:
250 mixing, ultrasonic disperse obtain graphene oxide dispersion.
Step (5) the mixing bentonite is to mix calcium-base bentonite with sodium base bentonite 1:1~1:2 in mass ratio,
Bentonite must be mixed.
Step (5) mixed metal powder is to mix nickel powder with zinc powder 2:1~3:1 in mass ratio, obtains mixed metal
Powder.
The beneficial effects of the present invention are:
(1) No. 1 additive is added when preparing long-acting antiseptic resistance-reducing agent by the present invention, firstly, contain four metatitanic acids in No. 1 additive,
After acidleach, the potassium ion in lamellar structure forms four metatitanic acids and is therefore being added potassium tetratitanate replaced hydrogen ion
After aniline, aniline can be under the action of electrostatic force, into the interlayer structure of four metatitanic acids, and in four titaniums in subsequent processes
Polyaniline is formed in the lamellar structure of acid, and then improves the electric conductivity of No. 1 additive, after being added in product, product can be made
The resistive raising of drop, and due in No. 1 additive without containing ionization anion, so as to improve the anti-corrosive properties of product,
Simultaneously because polyaniline is not easy to die with water flow, and then improve the long-term effect of product；Secondly as containing in the interlayer structure of four metatitanic acids
There is anion, it is adsorbable that the metal ion formed after metal powder corrosion is added, to further increase the conduction of No. 1 additive
Property, and then further increase the resistance-reducing performance of product；
(2) No. 2 additives are added when preparing long-acting antiseptic resistance-reducing agent by the present invention, on the one hand, the graphite being added in No. 2 additives
Alkene, and coated on the outside of graphene by the lamellar structure of potassium tetratitanate, since potassium tetratitanate is semiconductor structure, it can
The electric conductivity of No. 2 additives is improved, and then makes the resistive raising of the drop of product, on the other hand, since graphene oxide is restoring
It joined gallic acid when preparing graphene, reduced graphene surface can be made with negative electrical charge, dimension is added in No. 2 additives
After in product, conductive path can be formed under the action of electrostatic force in product system with No. 1 additive in use, from
And make that the drop of product is resistive to be further increased, also, be dispersed in water since graphene is more difficult, thus make the long-term effect of product into
One step improves；Also, it since potassium tetratitanate is metastable-state crystal, can be powered in use under the action of generating heat gradually
Be converted into potassium hexatitanate, be concurrently born from it is poly-, so that the long-term effect of product be made to further increase.
Specific embodiment
Hydrochloric acid solution 3:10~4:10 in mass ratio that aniline and mass fraction are 5~12% mix, in frequency for 45~
Under conditions of 55kHz after 15~30min of ultrasonic disperse, aniline dispersion liquid is obtained；Graphene oxide and dehydrated alcohol in mass ratio 1:
150~1:250 mixing obtains graphene oxide dispersion under conditions of frequency is 50~60kHz after 25~40min of ultrasonic disperse
Liquid；By potassium carbonate, 1.0:4.0~1.2:4.0 is mixed in grinder in molar ratio with titanium dioxide, 50~80min of mixed grinding
Afterwards, pretreatment powder batch is obtained, after calcining 11~12h with pretreatment powder, discharging obtains pretreatment powder, will pre-process powder
After the ground machine in end grinds 30~60min, after calcining 11~12h again, discharging obtains mixed-powder blank, by mixed-powder base
It after material first washs 5~10 times with the hydrochloric acid solution that mass fraction is 5~10%, then is washed with deionized 5~8 times, after washing
Mixed-powder blank be 80~90 DEG C in temperature under conditions of after dry 1~2h, obtain mixed-powder, mixed-powder be divided into
Two parts, respectively No. 1 mixed-powder and No. 2 mixed-powders；The hydrochloric acid that No. 1 mixed-powder is 20~30% with mass fraction is pressed
Mass ratio 1:80~1:120 mixing, after impregnating 50~80min under room temperature, filtering repeats to mix, impregnates filter process 2
After~3 times, modified powder blank is obtained, after modified powder blank is washed with water 3~6 times, the condition for being 60~85 DEG C in temperature
After 2~3h of lower drying, modified powder is obtained；The tetrabutylammonium hydroxide solution that modified powder is 10~18% with mass fraction is pressed
Mass ratio 1:10~1:18 mixing is 55~70 DEG C in temperature, revolving speed is stirred 2 under conditions of being 300~500r/min~
After 3h, and under room temperature impregnate 1~2h after, obtain modified powder collosol intermixture, by modified powder collosol intermixture in turn
After speed is centrifugated 30~40min under conditions of being 2000~3000r/min, upper liquid is removed, modified powder colloidal sol is obtained；It will change
Property powder colloidal sol and aniline dispersion liquid 1:3~1:5 in mass ratio be mixed in beaker, and into beaker be added aniline dispersion liquid matter
Amount 0.1~0.2 initiator, control initiator be added rate be 2~3mL/min, in temperature be 55~80 DEG C, revolving speed 300
Under conditions of~400r/min, after being stirred to react 1~3h, and after standing 2~3h under room temperature, filtering obtains No. 1 additive
Blank crushes under conditions of being 60~90 DEG C in temperature by No. 1 additive blank after dry 3~5h, crosses 80 meshes, obtain No. 1 and add
Add agent；Graphene oxide dispersion and No. 2 mixed-powder 8:1~8:2 in mass ratio are mixed in flask, in temperature be 30~
50 DEG C, under conditions of revolving speed is 300~400r/min, after being stirred 30~40min, graphene oxide mixture is obtained, by oxygen
Graphite alkene mixture and gallic acid 100:1~150:1 in mass ratio are mixed in three-necked flask, and are added into three-necked flask
The zinc acetate for entering 0.01~0.05 times of graphene oxide mixture quality is 45~70 DEG C in temperature, and revolving speed is 300~350r/
Under conditions of min, after being stirred to react 1~2h, then by three-necked flask material be added hydrothermal reaction kettle, in temperature be 150~180
Under conditions of DEG C, after 1~2h of hydro-thermal reaction, filtering, obtain No. 2 additive blanks, by No. 2 additive blanks in temperature be 65~90
Under conditions of DEG C after dry 3~4h, No. 2 additives are obtained；No. 1 additive is mixed with No. 2 additive 1:1~2:1 in mass ratio
In blender, and into blender be added No. 1 0.1~0.2 times of additive quality mixing bentonite and No. 1 additive quality
0.1~0.3 times of mixed metal powder is 40~50 DEG C in temperature, and under conditions of revolving speed is 300~600r/min, stirring is mixed
After closing 30~60min, long-acting antiseptic resistance-reducing agent is obtained.The calcination temperature is 700~880 DEG C.The initiator is potassium peroxydisulfate,
Any one in ammonium persulfate or sodium peroxydisulfate.The mixing bentonite be by calcium-base bentonite and sodium base bentonite in mass ratio
1:1~1:2 mixing, obtains mixing bentonite.The mixed metal powder is to mix nickel powder with zinc powder 2:1~3:1 in mass ratio,
Obtain mixed metal powder.
Aniline is mixed with the hydrochloric acid solution 4:10 in mass ratio that mass fraction is 12%, under conditions of frequency is 55kHz
After ultrasonic disperse 30min, aniline dispersion liquid is obtained；Graphene oxide is mixed with dehydrated alcohol 1:250 in mass ratio, is in frequency
Under conditions of 60kHz after ultrasonic disperse 40min, graphene oxide dispersion is obtained；In molar ratio by potassium carbonate and titanium dioxide
1.2:4.0 is mixed in grinder, after mixed grinding 80min, obtains pretreatment powder batch, will calcine 12h with pretreatment powder
Afterwards, it discharges, obtains pretreatment powder, after pre-processing the ground machine grinding 60min of powder, after calcining 12h again, discharging is obtained mixed
Powder batch is closed, after mixed-powder blank is first washed 10 times with the hydrochloric acid solution that mass fraction is 10%, then is washed with deionized water
It washs 8 times, the mixed-powder blank after washing after dry 2h, is obtained into mixed-powder, by mixed powder under the conditions of at a temperature of 90 °C
End is divided into two parts, respectively No. 1 mixed-powder and No. 2 mixed-powders；The salt for being 30% by No. 1 mixed-powder and mass fraction
Acid 1:120 in mass ratio mixing, after impregnating 80min under room temperature, filtering repeats to mix, after impregnating filter process 3 times,
Modified powder blank is obtained, after modified powder blank is washed with water 6 times, under conditions of being 85 DEG C in temperature after dry 3h, must be changed
Property powder；Modified powder is mixed with the tetrabutylammonium hydroxide solution 1:18 in mass ratio that mass fraction is 18%, is in temperature
70 DEG C, after revolving speed is stirred 3h under conditions of being 500r/min, and after impregnating 2h under room temperature, obtain modified powder colloidal sol
Mixture removes upper layer after modified powder collosol intermixture is centrifugated 40min under conditions of revolving speed is 3000r/min
Liquid obtains modified powder colloidal sol；Modified powder colloidal sol and aniline dispersion liquid 1:5 in mass ratio are mixed in beaker, and to beaker
It is middle be added aniline dispersion liquid quality 0.2 initiator, control initiator be added rate be 3mL/min, in temperature be 80 DEG C, revolving speed
Under conditions of 400r/min, after being stirred to react 3h, and after standing 3h under room temperature, filtering obtains No. 1 additive blank,
No. 1 additive blank after dry 5h, is crushed under the conditions of at a temperature of 90 °C, crosses 80 meshes, obtain No. 1 additive；It will oxidation
Graphene dispersing solution and No. 2 mixed-powder 8:2 in mass ratio are mixed in flask, in temperature be 50 DEG C, revolving speed 400r/min
Under conditions of, after being stirred 40min, graphene oxide mixture is obtained, graphene oxide mixture and gallic acid are pressed into matter
Amount is mixed in three-necked flask than 150:1, and 0.05 times of graphene oxide mixture quality of acetic acid is added into three-necked flask
Zinc, in temperature be 70 DEG C, revolving speed be 350r/min under conditions of, after being stirred to react 2h, then by three-necked flask material be added water
Thermal response kettle, under conditions of temperature is 180 DEG C, after hydro-thermal reaction 2h, filtering obtains No. 2 additive blanks, by No. 2 additives
Blank after dry 4h, obtains No. 2 additives under the conditions of at a temperature of 90 °C；By No. 1 additive and No. 2 additives in mass ratio 2:
1 is mixed in blender, and into blender be added No. 1 0.2 times of additive quality mixing bentonite and No. 1 additive quality
0.3 times of mixed metal powder is 50 DEG C in temperature, under conditions of revolving speed is 600r/min, after being stirred 60min, obtains length
Imitate antiseptic resistance-reducing agent.The calcination temperature is 880 DEG C.The initiator is potassium peroxydisulfate.The mixing bentonite is by calcium base
Bentonite is mixed with sodium base bentonite 1:2 in mass ratio, obtains mixing bentonite.The mixed metal powder is by nickel powder and zinc powder
The mixing of 3:1 in mass ratio, obtains mixed metal powder.
Aniline is mixed with the hydrochloric acid solution 4:10 in mass ratio that mass fraction is 12%, under conditions of frequency is 55kHz
After ultrasonic disperse 30min, aniline dispersion liquid is obtained；Graphene oxide is mixed with dehydrated alcohol 1:250 in mass ratio, is in frequency
Under conditions of 60kHz after ultrasonic disperse 40min, graphene oxide dispersion is obtained；In molar ratio by potassium carbonate and titanium dioxide
1.2:4.0 is mixed in grinder, after mixed grinding 80min, obtains pretreatment powder batch, will calcine 12h with pretreatment powder
Afterwards, it discharges, obtains pretreatment powder, after pre-processing the ground machine grinding 60min of powder, after calcining 12h again, discharging is obtained mixed
Powder batch is closed, after mixed-powder blank is first washed 10 times with the hydrochloric acid solution that mass fraction is 10%, then is washed with deionized water
It washs 8 times, the mixed-powder blank after washing after dry 2h, is obtained into mixed-powder, by mixed powder under the conditions of at a temperature of 90 °C
End is divided into two parts, respectively No. 1 mixed-powder and No. 2 mixed-powders；Graphene oxide dispersion and No. 2 mixed-powders are pressed
Mass ratio 8:2 is mixed in flask, is 50 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred 40min, is obtained
Graphene oxide mixture and gallic acid 150:1 in mass ratio are mixed in three-necked flask by graphene oxide mixture, and
0.05 times of graphene oxide mixture quality of zinc acetate is added into three-necked flask, in temperature be 70 DEG C, revolving speed 350r/
Under conditions of min, after being stirred to react 2h, then hydrothermal reaction kettle is added in material in three-necked flask, in temperature be 180 DEG C of condition
Under, after hydro-thermal reaction 2h, filtering obtains No. 2 additive blanks, and No. 2 additive blanks are dry under the conditions of at a temperature of 90 °C
After 4h, No. 2 additives are obtained；No. 2 additives are added in blender, and No. 2 0.1 times of additive quality is added into blender
Bentonite and No. 2 0.15 times of additive quality of mixed metal powder are mixed, is 50 DEG C in temperature, revolving speed is the item of 600r/min
Under part, after being stirred 60min, long-acting antiseptic resistance-reducing agent is obtained.The calcination temperature is 880 DEG C.The initiator is persulfuric acid
Potassium.The mixing bentonite is to mix calcium-base bentonite with sodium base bentonite 1:2 in mass ratio, obtains mixing bentonite.It is described
Mixed metal powder is to mix nickel powder with zinc powder 3:1 in mass ratio, obtains mixed metal powder.
Aniline is mixed with the hydrochloric acid solution 4:10 in mass ratio that mass fraction is 12%, under conditions of frequency is 55kHz
After ultrasonic disperse 30min, aniline dispersion liquid is obtained；Graphene oxide is mixed with dehydrated alcohol 1:250 in mass ratio, is in frequency
Under conditions of 60kHz after ultrasonic disperse 40min, graphene oxide dispersion is obtained；In molar ratio by potassium carbonate and titanium dioxide
1.2:4.0 is mixed in grinder, after mixed grinding 80min, obtains pretreatment powder batch, will calcine 12h with pretreatment powder
Afterwards, it discharges, obtains pretreatment powder, after pre-processing the ground machine grinding 60min of powder, after calcining 12h again, discharging is obtained mixed
Powder batch is closed, after mixed-powder blank is first washed 10 times with the hydrochloric acid solution that mass fraction is 10%, then is washed with deionized water
It washs 8 times, the mixed-powder blank after washing after dry 2h, is obtained into mixed-powder, by mixed powder under the conditions of at a temperature of 90 °C
End is divided into two parts, respectively No. 1 mixed-powder and No. 2 mixed-powders；The salt for being 30% by No. 1 mixed-powder and mass fraction
Acid 1:120 in mass ratio mixing, after impregnating 80min under room temperature, filtering repeats to mix, after impregnating filter process 3 times,
Modified powder blank is obtained, after modified powder blank is washed with water 6 times, under conditions of being 85 DEG C in temperature after dry 3h, must be changed
Property powder；Modified powder is mixed with the tetrabutylammonium hydroxide solution 1:18 in mass ratio that mass fraction is 18%, is in temperature
70 DEG C, after revolving speed is stirred 3h under conditions of being 500r/min, and after impregnating 2h under room temperature, obtain modified powder colloidal sol
Mixture removes upper layer after modified powder collosol intermixture is centrifugated 40min under conditions of revolving speed is 3000r/min
Liquid obtains modified powder colloidal sol；Modified powder colloidal sol and aniline dispersion liquid 1:5 in mass ratio are mixed in beaker, and to beaker
It is middle be added aniline dispersion liquid quality 0.2 initiator, control initiator be added rate be 3mL/min, in temperature be 80 DEG C, revolving speed
Under conditions of 400r/min, after being stirred to react 3h, and after standing 3h under room temperature, filtering obtains No. 1 additive blank,
No. 1 additive blank after dry 5h, is crushed under the conditions of at a temperature of 90 °C, crosses 80 meshes, obtain No. 1 additive；No. 1 is added
Add agent be added blender in, and into blender be added No. 1 0.2 times of additive quality mixing bentonite and No. 1 additive matter
The mixed metal powder of 0.3 times of amount is 50 DEG C in temperature, under conditions of revolving speed is 600r/min, after being stirred 60min, obtains
Long-acting antiseptic resistance-reducing agent.The calcination temperature is 880 DEG C.The initiator is potassium peroxydisulfate.The mixing bentonite is by calcium
Base bentonite is mixed with sodium base bentonite 1:2 in mass ratio, obtains mixing bentonite.The mixed metal powder is by nickel powder and zinc
Powder 3:1 in mass ratio mixing, obtains mixed metal powder.
Aniline is mixed with the hydrochloric acid solution 4:10 in mass ratio that mass fraction is 12%, under conditions of frequency is 55kHz
After ultrasonic disperse 30min, aniline dispersion liquid is obtained；Graphene oxide is mixed with dehydrated alcohol 1:250 in mass ratio, is in frequency
Under conditions of 60kHz after ultrasonic disperse 40min, graphene oxide dispersion is obtained；In molar ratio by potassium carbonate and titanium dioxide
1.2:4.0 is mixed in grinder, after mixed grinding 80min, obtains pretreatment powder batch, will calcine 12h with pretreatment powder
Afterwards, it discharges, obtains pretreatment powder, after pre-processing the ground machine grinding 60min of powder, after calcining 12h again, discharging is obtained mixed
Powder batch is closed, after mixed-powder blank is first washed 10 times with the hydrochloric acid solution that mass fraction is 10%, then is washed with deionized water
It washs 8 times, the mixed-powder blank after washing after dry 2h, is obtained into mixed-powder, by mixed powder under the conditions of at a temperature of 90 °C
End is divided into two parts, respectively No. 1 mixed-powder and No. 2 mixed-powders；The salt for being 30% by No. 1 mixed-powder and mass fraction
Acid 1:120 in mass ratio mixing, after impregnating 80min under room temperature, filtering repeats to mix, after impregnating filter process 3 times,
Modified powder blank is obtained, after modified powder blank is washed with water 6 times, under conditions of being 85 DEG C in temperature after dry 3h, must be changed
Property powder；Modified powder is mixed with the tetrabutylammonium hydroxide solution 1:18 in mass ratio that mass fraction is 18%, is in temperature
70 DEG C, after revolving speed is stirred 3h under conditions of being 500r/min, and after impregnating 2h under room temperature, obtain modified powder colloidal sol
Mixture removes upper layer after modified powder collosol intermixture is centrifugated 40min under conditions of revolving speed is 3000r/min
Liquid obtains modified powder colloidal sol；Modified powder colloidal sol and aniline dispersion liquid 1:5 in mass ratio are mixed in beaker, and to beaker
It is middle be added aniline dispersion liquid quality 0.2 initiator, control initiator be added rate be 3mL/min, in temperature be 80 DEG C, revolving speed
Under conditions of 400r/min, after being stirred to react 3h, and after standing 3h under room temperature, filtering obtains No. 1 additive blank,
No. 1 additive blank after dry 5h, is crushed under the conditions of at a temperature of 90 °C, crosses 80 meshes, obtain No. 1 additive；It will oxidation
Graphene dispersing solution and No. 2 mixed-powder 8:2 in mass ratio are mixed in flask, in temperature be 50 DEG C, revolving speed 400r/min
Under conditions of, after being stirred 40min, graphene oxide mixture is obtained, graphene oxide mixture and gallic acid are pressed into matter
Amount is mixed in three-necked flask than 150:1, and 0.05 times of graphene oxide mixture quality of acetic acid is added into three-necked flask
Zinc, in temperature be 70 DEG C, revolving speed be 350r/min under conditions of, after being stirred to react 2h, then by three-necked flask material be added water
Thermal response kettle, under conditions of temperature is 180 DEG C, after hydro-thermal reaction 2h, filtering obtains No. 2 additive blanks, by No. 2 additives
Blank after dry 4h, obtains No. 2 additives under the conditions of at a temperature of 90 °C；By No. 1 additive and No. 2 additives in mass ratio 2:
1 is mixed in blender, and No. 1 0.3 times of additive quality of mixed metal powder is added into blender, in temperature be 50
DEG C, under conditions of revolving speed is 600r/min, after being stirred 60min, obtain long-acting antiseptic resistance-reducing agent.The calcination temperature is 880
℃.The initiator is potassium peroxydisulfate.The mixed metal powder is to mix nickel powder with zinc powder 3:1 in mass ratio, must be mixed
Metal powder.
Aniline is mixed with the hydrochloric acid solution 4:10 in mass ratio that mass fraction is 12%, under conditions of frequency is 55kHz
After ultrasonic disperse 30min, aniline dispersion liquid is obtained；Graphene oxide is mixed with dehydrated alcohol 1:250 in mass ratio, is in frequency
Under conditions of 60kHz after ultrasonic disperse 40min, graphene oxide dispersion is obtained；In molar ratio by potassium carbonate and titanium dioxide
1.2:4.0 is mixed in grinder, after mixed grinding 80min, obtains pretreatment powder batch, will calcine 12h with pretreatment powder
Afterwards, it discharges, obtains pretreatment powder, after pre-processing the ground machine grinding 60min of powder, after calcining 12h again, discharging is obtained mixed
Powder batch is closed, after mixed-powder blank is first washed 10 times with the hydrochloric acid solution that mass fraction is 10%, then is washed with deionized water
It washs 8 times, the mixed-powder blank after washing after dry 2h, is obtained into mixed-powder, by mixed powder under the conditions of at a temperature of 90 °C
End is divided into two parts, respectively No. 1 mixed-powder and No. 2 mixed-powders；The salt for being 30% by No. 1 mixed-powder and mass fraction
Acid 1:120 in mass ratio mixing, after impregnating 80min under room temperature, filtering repeats to mix, after impregnating filter process 3 times,
Modified powder blank is obtained, after modified powder blank is washed with water 6 times, under conditions of being 85 DEG C in temperature after dry 3h, must be changed
Property powder；Modified powder is mixed with the tetrabutylammonium hydroxide solution 1:18 in mass ratio that mass fraction is 18%, is in temperature
70 DEG C, after revolving speed is stirred 3h under conditions of being 500r/min, and after impregnating 2h under room temperature, obtain modified powder colloidal sol
Mixture removes upper layer after modified powder collosol intermixture is centrifugated 40min under conditions of revolving speed is 3000r/min
Liquid obtains modified powder colloidal sol；Modified powder colloidal sol and aniline dispersion liquid 1:5 in mass ratio are mixed in beaker, and to beaker
It is middle be added aniline dispersion liquid quality 0.2 initiator, control initiator be added rate be 3mL/min, in temperature be 80 DEG C, revolving speed
Under conditions of 400r/min, after being stirred to react 3h, and after standing 3h under room temperature, filtering obtains No. 1 additive blank,
No. 1 additive blank after dry 5h, is crushed under the conditions of at a temperature of 90 °C, crosses 80 meshes, obtain No. 1 additive；It will oxidation
Graphene dispersing solution and No. 2 mixed-powder 8:2 in mass ratio are mixed in flask, in temperature be 50 DEG C, revolving speed 400r/min
Under conditions of, after being stirred 40min, graphene oxide mixture is obtained, graphene oxide mixture and gallic acid are pressed into matter
Amount is mixed in three-necked flask than 150:1, and 0.05 times of graphene oxide mixture quality of acetic acid is added into three-necked flask
Zinc, in temperature be 70 DEG C, revolving speed be 350r/min under conditions of, after being stirred to react 2h, then by three-necked flask material be added water
Thermal response kettle, under conditions of temperature is 180 DEG C, after hydro-thermal reaction 2h, filtering obtains No. 2 additive blanks, by No. 2 additives
Blank after dry 4h, obtains No. 2 additives under the conditions of at a temperature of 90 °C；By No. 1 additive and No. 2 additives in mass ratio 2:
1 is mixed in blender, and No. 1 0.2 times of additive quality of mixing bentonite is added into blender, in temperature be 50 DEG C,
Under conditions of revolving speed is 600r/min, after being stirred 60min, long-acting antiseptic resistance-reducing agent is obtained.The calcination temperature is 880 DEG C.
The initiator is potassium peroxydisulfate.The mixing bentonite is to mix calcium-base bentonite with sodium base bentonite 1:2 in mass ratio,
Bentonite must be mixed.
Comparative example: the friction reducer of Beijing Science and Technology Ltd. production.
1 to 5 gained friction reducer of example and comparative example product are subjected to performance detection, the specific detection method is as follows:
The above-mentioned friction reducer of 0.1%(w) is dissolved in water, fracturing fluid is conveyed by pump after dissolving 5min, is measured through spinner flowmeter
Enter experimental section afterwards.Pressure drop of the fracturing fluid by experimental section is measured after pressure gauge is stablized, resistance-reducing yield (K) is calculated with formula (1).
K=[(Δ p0Δ p)/Δ p0] × 100% (1)
In formula, Δ p0Pressure difference when for clear water under F flow by test pipeline, MPa；Δ p is that friction reducer aqueous solution is logical under F flow
Cross pressure difference when test pipeline, MPa.
After 10 min of continuous shear stress, resistance-reducing yield is detected again.
Specific testing result is as shown in table 1:
Table 1: performance detection table
| Detection content | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| Resistance-reducing yield/% | 63.5 | 61.2 | 58.7 | 59.2 | 60.3 | 54.6 |
| Shear 10 min resistance-reducing yields/% | 57.5 | 52.3 | 50.8 | 50.2 | 51.3 | 47.5 |
By 1 testing result of table it is found that present invention gained long-acting antiseptic resistance-reducing agent has excellent resistance-reducing performance and long-term effect.
Claims (7)
1. a kind of preparation method of long-acting antiseptic resistance-reducing agent, which is characterized in that specific preparation step are as follows:
(1) by potassium carbonate, 1.0:4.0~1.2:4.0 is mixed in molar ratio with titanium dioxide, is ground, and calcining obtains pretreatment powder,
It is polished that powder will be pre-processed, calcined again, discharged, drying is washed, obtain mixed-powder, mixed-powder is divided into two parts,
Respectively No. 1 mixed-powder and No. 2 mixed-powders；
(2) No. 1 mixed-powder is mixed with hydrochloric acid 1:80~1:120 in mass ratio, impregnates filtering, repeated to mix, impregnate filtering
After process 2~3 times, wash, it is dry, obtain modified powder；By modified powder and tetrabutylammonium hydroxide solution 1:10 in mass ratio
~1:18 mixing, is stirred, and impregnates, and centrifuge separation removes upper liquid, obtains modified powder colloidal sol；
(3) modified powder colloidal sol is mixed with aniline dispersion liquid 1:3~1:5 in mass ratio, and aniline dispersion liquid quality 0.1 is added
~0.2 initiator after being stirred to react, stands filtering, dry, pulverize, is sieved, obtains No. 1 additive；
(4) graphene oxide dispersion is mixed with No. 2 mixed-powder 8:1~8:2 in mass ratio, after being stirred, must be aoxidized
Graphene oxide mixture is mixed with gallic acid 100:1~150:1 in mass ratio, and oxidation is added by graphene mixture
The zinc acetate that 0.01~0.05 times of graphene mixture quality after being stirred to react, filters, dry, obtains No. 2 additives；
(5) No. 1 additive is mixed with No. 2 additive 1:1~2:1 in mass ratio, and No. 1 additive quality 0.1~0.2 is added
Mixing bentonite and No. 1 0.1~0.3 times of additive quality of mixed metal powder again after being stirred, obtains long-effective corrosion drop
Resist.
2. a kind of preparation method of long-acting antiseptic resistance-reducing agent according to claim 1, it is characterised in that: step (1) is described
Calcination temperature is 700~880 DEG C.
3. a kind of preparation method of long-acting antiseptic resistance-reducing agent according to claim 1, it is characterised in that: step (3) is described
Aniline dispersion liquid is to mix aniline with hydrochloric acid solution 3:10~4:10 in mass ratio, and ultrasonic disperse obtains aniline dispersion liquid.
4. a kind of preparation method of long-acting antiseptic resistance-reducing agent according to claim 1, it is characterised in that: step (3) is described
Initiator is potassium peroxydisulfate, any one in ammonium persulfate or sodium peroxydisulfate.
5. a kind of preparation method of long-acting antiseptic resistance-reducing agent according to claim 1, it is characterised in that: step (4) is described
Graphene oxide dispersion is to mix graphene oxide with dehydrated alcohol 1:150~1:250 in mass ratio, and ultrasonic disperse obtains
Graphene oxide dispersion.
6. a kind of preparation method of long-acting antiseptic resistance-reducing agent according to claim 1, it is characterised in that: step (5) is described
Mixing bentonite is to mix calcium-base bentonite with sodium base bentonite 1:1~1:2 in mass ratio, obtains mixing bentonite.
7. a kind of preparation method of long-acting antiseptic resistance-reducing agent according to claim 1, it is characterised in that: step (5) is described
Mixed metal powder is to mix nickel powder with zinc powder 2:1~3:1 in mass ratio, obtains mixed metal powder.
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