CN106701055A - Preparation method of lightweight and high-strength fracturing propping agent - Google Patents
Preparation method of lightweight and high-strength fracturing propping agent Download PDFInfo
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Abstract
The invention discloses a preparation method of a lightweight and high-strength fracturing propping agent, and belongs to the technical field of propping agent preparation. Silicon dioxide generated by calcination is taken as a kernel, hydroxyapatite and aluminum oxide generated by calcination coat the surface, one part of silicon dioxide reacts with carbon in a high-temperature state to generate silicon carbide and the other part of silicon dioxide reacts with sodium carbonate generated by evaporative crystallization at a high temperature to generate sodium silicate, and the sodium silicate is removed through washing and dissolving to form a hollow structure. Hollow microspheres formed by silicon carbide, aluminum oxide and hydroxyapatite are fully utilized to reach the lightweight and high-strength effects; the density of the lightweight and high-strength fracturing propping agent is reduced by over 10% in comparison with a conventional ceramsite fracturing propping agent; the problem that loss of fracturing equipment is easily caused by over-high density of the traditional ceramsite fracturing propping agent is effectively solved.
Description
Technical field
The invention discloses a kind of preparation method of high-strength light fracturing propping agents, belong to proppant preparing technical field.
Background technology
During fracturing propping agents are oil, gas industry hydraulic fracturing process, formation fracture is pumped into fracturing fluid
In rise supporting crack, increase oil gas water conservancy diversion rate proprietary material.Ceramic fracturing propping agent has compared with quartz sand, resin burnt-in sand
Percentage of damage is low, corrosion-resistant, flow conductivity is good and the characteristics of cost performance high, is used by increasing oil field.
Hydraulic fracturing technology is tested successfully so far from nineteen forty-seven in the U.S., has become a kind of production practice skill of maturation
Art, it is widely used by each oil gas field in the world.In hydraulic fracturing totle drilling cost, fracturing propping agents expense accounts for the ratio of whole operating cost
Example is big, not only represents most of Oil/gas Well initial stage cost, and decide the economic life in Oil/gas Well or oil field；Waterpower
The success or failure of fracturing effect, the length of the term of validity depends primarily on the quality of proppant.Current proppant mainly has three classes：Haydite,
Quartz sand and resin burnt-in sand.Chip after quartz sand low intensity and rupture can block crack, reduce water conservancy diversion rate, it is impossible to meet deep
The requirement of well exploitation；Various resin burnt-in sands solve the problem of quartz sand low intensity, but production cost is high, complex process；Sintering
Haydite is widely used by increasing oil field because of the cost performance that intensity is high, chemical stability is good, superior, but density is higher,
Easily fracturing unit is caused damage.China's ceramsite propping agent was developed since the eighties, and earliest product is the aluminium of injection
Alumina proppant in high intensity, is developed so far more than 30 years, and domestic some enterprise products or research institutions' achievement have caught up with the world
Advanced level, some properties of product have been even more than advanced international standard.As society constantly carries to the demand of petroleum gas
Height, oil gas well depth increases year by year, the density of ceramsite propping agent how is reduced on the premise of high intensity is kept and is explored new
Ceramsite propping agent has become one of the study hotspot in inorganic material or oil and gas exploitation field.
The content of the invention
The present invention solves the technical problem of：It is higher for conventional sintering haydite type fracturing propping agents density, make
Easily fracturing unit is caused damage during, the problem of influence oil and natural gas exploitation, there is provided it is a kind of with sodium metasilicate and
White precipitate obtained in hydrochloric acid reaction is kernel, in one layer of calcium hydroxy phosphate of Surface coating, and aluminum nitrate and uric acid, ammoniacal liquor etc.
Reaction produces aluminum hydroxide precipitate, after mix with carbon black, the calcining under argon gas guard mode, then after mixing with sodium carbonate liquor
Evaporative crystallization, and calcine again, the method for high-strength light fracturing propping agents most is obtained through washing and drying afterwards.The present invention is calcining
The silica of generation is kernel, in the aluminum oxide that Surface coating hydroxyapatite and calcining are produced, at high operating temperatures one
Part of silica and carbon reaction generation carborundum, and the sodium carbonate that another part silica is generated with evaporative crystallization is in high temperature
Lower reaction generation sodium metasilicate, then sodium metasilicate is removed through washing dissolving, hollow-core construction is formed, the present invention makes full use of carborundum, oxygen
Change the tiny balloon that aluminium and hydroxyapatite are formed, reach the effect of high-strength light, the more conventional haydite type fracturing propping agents of density
More than 10% is reduced, efficiently solves that traditional haydite type fracturing propping agents density is higher, loss is easily caused to fracturing unit
Problem.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
(1) 150~200mL mass fractions are measured for 10% sodium silicate solution, are poured into the there-necked flask with dropping funel,
There-necked flask is placed in into digital display again to test the speed in constant temperature blender with magnetic force, is 55~60 DEG C in temperature, rotating speed is 300~500r/min
Under the conditions of, by dropping funel to adding 120~160mL concentration for 2mol/L hydrochloric acid in there-necked flask, control in 30~45min
Inside drip off, treat completion of dropping, continue constant temperature 30~45min of stirring reaction, obtain white suspension；
(2) by above-mentioned gained white suspension with 280~380mL mass fractions for 8~10% aluminum nitrate solutions mix
After even, pour into there-necked flask, add 20~40g urea, 30~40g nano-hydroxy phosphoric acid calcium, 40~60mL diethanol amine,
There-necked flask then is placed in into digital display to test the speed in constant temperature blender with magnetic force, is 65~70 DEG C in temperature, rotating speed is 400~600r/
Under the conditions of min, constant temperature stirs 15~20min, then by dropping funel to 400~500mL of addition mass point in there-necked flask
Number is 15% ammoniacal liquor, continues 45~60min of constant temperature stirring reaction；
(3) question response terminates, filtering, collects filter cake, and filter cake is washed with deionized up to cleaning solution is in neutrality, then will
Filter cake after washing is transferred in baking oven, is dried to constant weight under the conditions of being 105~110 DEG C in temperature, then by dried filter cake and 3
The carbon black that~5g is crushed to 325~500 mesh is well mixed, and is transferred to Muffle furnace, with 3~5mL/min speed to being passed through argon in stove
Gas, under argon gas guard mode, 680~700 DEG C, after 20~30min of insulation calcining is warming up to 6~8 DEG C/min rate programs,
Continue to be warming up to 1100~1200 DEG C with 10~15 DEG C/min rate programs, insulation 45~60min of calcining cools to room with the furnace
Temperature, discharging, obtains calcined mixed powder；
(4) above-mentioned gained calcined mixed powder is poured into and fills 400~600mL mass fractions for 10~15% sodium carbonate are molten
In the evaporating dish of liquid, after stirring 10~15min of mixing with glass bar, then be transferred to for material in evaporating dish to dry by heating evaporation
In tube type resistance furnace, 30~45min, room temperature to be cooled to the furnace, by tubular type are calcined under the conditions of being 1100~1200 DEG C in temperature
Material is poured into the beaker for filling 1~2L water in resistance furnace, and after stirring 15~20min of mixing with glass bar, filter is collected in filtering
Cake, and gained filter cake is placed in baking oven, dried to constant weight under the conditions of being 105~110 DEG C in temperature, obtain final product high-strength light pressure break
Proppant.
The fracturing propping agents performance prepared using the present invention is as follows, and volume density is 0.9~1.6g/cm3, apparent density be 2.0
~2.2g/cm3, circularity and sphericity are 0.7~0.9, and turbidity is 25~30FTU, and 20/40 mesh product is broken under 48MPa pressure
Broken rate is less than 10%, and apparent density is minimum can reach 2.2g/cm3, far below the apparent density of current sintered bauxite proppant
(2.6~3.5g/cm3)。
The beneficial effects of the invention are as follows：
(1) present invention gained high-strength light fracturing propping agents density is low, and precipitation is difficult during use, is easy to pumping, drop
The low requirement to fracturing fluid viscosity, reduces the injury to pump, effectively reduces difficulty of construction and cost；
(2) present invention gained high-strength light fracturing propping agents intensity is high, and percentage of damage is low during use, can effectively keep pressure
Split the water conservancy diversion rate of liquid, it is adaptable to deep well fracturing, there are wide market prospects.
Specific embodiment
150~200mL mass fractions are measured for 10% sodium silicate solution, is poured into the there-necked flask with dropping funel, then
There-necked flask is placed in into digital display to test the speed in constant temperature blender with magnetic force, is 55~60 DEG C in temperature, rotating speed is 300~500r/min bars
Under part, by dropping funel to adding 120~160mL concentration for 2mol/L hydrochloric acid in there-necked flask, control in 30~45min
Drip off, treat completion of dropping, continue constant temperature 30~45min of stirring reaction, obtain white suspension；By above-mentioned gained white suspension with
280~380mL mass fractions are after 8~10% aluminum nitrate solutions are well mixed, to pour into there-necked flask, add 20~40g
There-necked flask is then placed in digital display and tested the speed constant temperature magnetic by urea, 30~40g nano-hydroxy phosphoric acid calcium, 40~60mL diethanol amine
It it is 65~70 DEG C in temperature in power agitator, rotating speed is under the conditions of 400~600r/min, constant temperature stirs 15~20min, then
To 400~500mL mass fractions are added in there-necked flask be 15% ammoniacal liquor by dropping funel, continue constant temperature stirring reaction 45~
60min；Question response terminates, filtering, collects filter cake, and filter cake is washed with deionized up to cleaning solution is in neutrality, then will washing
Filter cake afterwards is transferred in baking oven, is dried to constant weight under the conditions of being 105~110 DEG C in temperature, then by dried filter cake and 3~5g
The carbon black for being crushed to 325~500 mesh is well mixed, and is transferred to Muffle furnace, with 3~5mL/min speed to being passed through argon gas in stove,
Under argon gas guard mode, 680~700 DEG C are warming up to 6~8 DEG C/min rate programs, after 20~30min of insulation calcining, continued
1100~1200 DEG C are warming up to 10~15 DEG C/min rate programs, insulation 45~60min of calcining cools to room temperature with the furnace, goes out
Material, obtains calcined mixed powder；It is 10~15% above-mentioned gained calcined mixed powder to be poured into and fills 400~600mL mass fractions
In the evaporating dish of sodium carbonate liquor, after stirring 10~15min of mixing with glass bar, heating evaporation to dry, then by evaporating dish
Material is transferred in tube type resistance furnace, and 30~45min, room to be cooled to the furnace are calcined under the conditions of being 1100~1200 DEG C in temperature
Temperature, material in tube type resistance furnace is poured into the beaker for filling 1~2L water, after stirring 15~20min of mixing with glass bar, mistake
Filter, collects filter cake, and gained filter cake is placed in baking oven, is dried to constant weight under the conditions of being 105~110 DEG C in temperature, obtains final product light
The high-strength fracturing propping agents of matter.
Example 1
150mL mass fractions are measured for 10% sodium silicate solution, is poured into the there-necked flask with dropping funel, then by three mouthfuls
Flask is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 55 DEG C in temperature, under the conditions of rotating speed is 300r/min, is leaked by dropping liquid
It is 2mol/L hydrochloric acid to struggle against to 120mL concentration is added in there-necked flask, and control is dripped off in 30min, treats completion of dropping, continues constant temperature
Stirring reaction 30min, obtains white suspension；It is 8% aluminum nitrate solution by above-mentioned gained white suspension and 280mL mass fractions
After well mixed, pour into there-necked flask, add 20g urea, 30g nano-hydroxy phosphoric acid calcium, 40mL diethanol amine then will
There-necked flask is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 65 DEG C in temperature, and under the conditions of rotating speed is 400r/min, constant temperature is stirred
15min is mixed, constant temperature stirring is then continued to adding 400mL mass fractions for 15% ammoniacal liquor in there-necked flask by dropping funel
Reaction 45min；Question response terminates, filtering, collects filter cake, and filter cake is washed with deionized up to cleaning solution is in neutrality, then will
Filter cake after washing is transferred in baking oven, is dried to constant weight under the conditions of being 105 DEG C in temperature, then dried filter cake and 3g are crushed
Carbon black to 325 mesh is well mixed, and is transferred to Muffle furnace, with 3mL/min speed to argon gas is passed through in stove, in argon gas guard mode
Under, 680 DEG C are warming up to 6 DEG C/min rate programs, after insulation calcining 20min, continuation is warming up to 10 DEG C/min rate programs
1100 DEG C, insulation calcining 45min cools to room temperature with the furnace, discharges, and obtains calcined mixed powder；By above-mentioned gained calcined mixed powder
End is poured into filling the evaporating dish that 400mL mass fractions are 10% sodium carbonate liquor, after stirring mixing 10min with glass bar, plus
Then be transferred to material in evaporating dish in tube type resistance furnace to dry by thermal evaporation, and 30min is calcined under the conditions of being 1100 DEG C in temperature,
Room temperature to be cooled to the furnace, material in tube type resistance furnace is poured into the beaker for filling 1L water, and mixing 15min is stirred with glass bar
Afterwards, filter, collect filter cake, and gained filter cake is placed in baking oven, dried to constant weight under the conditions of being 105 DEG C in temperature, obtain final product light
The high-strength fracturing propping agents of matter.
The fracturing propping agents performance prepared using the present invention is as follows, and volume density is 0.9g/cm3, apparent density be 2.0g/cm3,
Circularity and sphericity are 0.7, and turbidity is 25FTU, and percentage of damage of the 20/40 mesh product under 48MPa pressure is 9%, and apparent density is remote
Less than the apparent density of current sintered bauxite proppant.
Example 2
180mL mass fractions are measured for 10% sodium silicate solution, is poured into the there-necked flask with dropping funel, then by three mouthfuls
Flask is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 58 DEG C in temperature, under the conditions of rotating speed is 400r/min, is leaked by dropping liquid
It is 2mol/L hydrochloric acid to struggle against to 140mL concentration is added in there-necked flask, and control is dripped off in 40min, treats completion of dropping, continues constant temperature
Stirring reaction 35min, obtains white suspension；It is 9% aluminum nitrate solution by above-mentioned gained white suspension and 320mL mass fractions
After well mixed, pour into there-necked flask, add 30g urea, 35g nano-hydroxy phosphoric acid calcium, 50mL diethanol amine then will
There-necked flask is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 68 DEG C in temperature, and under the conditions of rotating speed is 500r/min, constant temperature is stirred
18min is mixed, constant temperature stirring is then continued to adding 450mL mass fractions for 15% ammoniacal liquor in there-necked flask by dropping funel
Reaction 50min；Question response terminates, filtering, collects filter cake, and filter cake is washed with deionized up to cleaning solution is in neutrality, then will
Filter cake after washing is transferred in baking oven, is dried to constant weight under the conditions of being 108 DEG C in temperature, then dried filter cake and 4g are crushed
Carbon black to 400 mesh is well mixed, and is transferred to Muffle furnace, with 4mL/min speed to argon gas is passed through in stove, in argon gas guard mode
Under, 690 DEG C are warming up to 7 DEG C/min rate programs, after insulation calcining 25min, continuation is warming up to 12 DEG C/min rate programs
1150 DEG C, insulation calcining 50min cools to room temperature with the furnace, discharges, and obtains calcined mixed powder；By above-mentioned gained calcined mixed powder
End is poured into filling the evaporating dish that 500mL mass fractions are 12% sodium carbonate liquor, after stirring mixing 12min with glass bar, plus
Then be transferred to material in evaporating dish in tube type resistance furnace to dry by thermal evaporation, and 40min is calcined under the conditions of being 1150 DEG C in temperature,
Room temperature to be cooled to the furnace, material in tube type resistance furnace is poured into the beaker for filling 1L water, and mixing 18min is stirred with glass bar
Afterwards, filter, collect filter cake, and gained filter cake is placed in baking oven, dried to constant weight under the conditions of being 108 DEG C in temperature, obtain final product light
The high-strength fracturing propping agents of matter.
The fracturing propping agents performance prepared using the present invention is as follows, and volume density is 1.2g/cm3, apparent density be 2.1g/cm3,
Circularity and sphericity are 0.8, and turbidity is 28FTU, and percentage of damage of the 20/40 mesh product under 48MPa pressure is 8%, and apparent density is remote
Less than the apparent density of current sintered bauxite proppant.
Example 3
200mL mass fractions are measured for 10% sodium silicate solution, is poured into the there-necked flask with dropping funel, then by three mouthfuls
Flask is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 60 DEG C in temperature, under the conditions of rotating speed is 500r/min, is leaked by dropping liquid
It is 2mol/L hydrochloric acid to struggle against to 160mL concentration is added in there-necked flask, and control is dripped off in 45min, treats completion of dropping, continues constant temperature
Stirring reaction 45min, obtains white suspension；It is that 10% aluminum nitrate is molten by above-mentioned gained white suspension and 380mL mass fractions
After liquid is well mixed, pour into there-necked flask, add 40g urea, 40g nano-hydroxy phosphoric acid calcium, 60mL diethanol amine, then
There-necked flask is placed in into digital display to test the speed in constant temperature blender with magnetic force, in temperature be 70 DEG C, under the conditions of rotating speed is 600r/min, constant temperature
Stirring 20min, is then continued constant temperature and stirred by dropping funel to adding 500mL mass fractions for 15% ammoniacal liquor in there-necked flask
Mix reaction 60min；Question response terminates, filtering, collects filter cake, and filter cake is washed with deionized up to cleaning solution is in neutrality, then
Filter cake after washing is transferred in baking oven, is dried to constant weight under the conditions of being 110 DEG C in temperature, then by dried filter cake and 5g powder
The carbon black for being broken to 500 mesh is well mixed, and is transferred to Muffle furnace, with 5mL/min speed to argon gas is passed through in stove, shape is protected in argon gas
Under state, 700 DEG C are warming up to 8 DEG C/min rate programs, after insulation calcining 30min, continue to be heated up with 15 DEG C/min rate programs
To 1200 DEG C, insulation calcining 60min cools to room temperature with the furnace, discharges, and obtains calcined mixed powder；By above-mentioned gained calcined mixed
Powder is poured into filling the evaporating dish that 600mL mass fractions are 15% sodium carbonate liquor, after stirring mixing 15min with glass bar,
Then be transferred to material in evaporating dish in tube type resistance furnace to dry by heating evaporation, is calcined under the conditions of being 1200 DEG C in temperature
45min, room temperature to be cooled to the furnace is poured into material in tube type resistance furnace in the beaker for filling 2L water, stirs mixed with glass bar
After closing 20min, filter cake is collected in filtering, and gained filter cake is placed in baking oven, is dried to constant weight under the conditions of being 110 DEG C in temperature,
Obtain final product high-strength light fracturing propping agents.
The fracturing propping agents performance prepared using the present invention is as follows, and volume density is 1.6g/cm3, apparent density be 2.2g/cm3,
Circularity and sphericity are 0.9, and turbidity is 30FTU, and percentage of damage of the 20/40 mesh product under 48MPa pressure is less than 10%, and apparent density
Far below the apparent density of current sintered bauxite proppant.
Claims (1)
1. a kind of preparation method of high-strength light fracturing propping agents, it is characterised in that specific preparation process is：
(1) 150~200mL mass fractions are measured for 10% sodium silicate solution, is poured into the there-necked flask with dropping funel, then will
There-necked flask is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 55~60 DEG C in temperature, and rotating speed is 300~500r/min conditions
Under, by dropping funel to adding 120~160mL concentration for 2mol/L hydrochloric acid in there-necked flask, control is dripped in 30~45min
It is complete, completion of dropping is treated, continue constant temperature 30~45min of stirring reaction, obtain white suspension；
(2) after above-mentioned gained white suspension is well mixed with 280~380mL mass fractions for 8~10% aluminum nitrate solutions,
Pour into there-necked flask, add 20~40g urea, 30~40g nano-hydroxy phosphoric acid calcium, 40~60mL diethanol amine, then
There-necked flask is placed in into digital display to test the speed in constant temperature blender with magnetic force, is 65~70 DEG C in temperature, rotating speed is 400~600r/min bars
Under part, constant temperature stirs 15~20min, is to addition 400~500mL mass fractions in there-necked flask by dropping funel then
15% ammoniacal liquor, continues 45~60min of constant temperature stirring reaction；
(3) question response terminates, filtering, collects filter cake, and filter cake is washed with deionized up to cleaning solution is in neutrality, then will washing
Filter cake afterwards is transferred in baking oven, is dried to constant weight under the conditions of being 105~110 DEG C in temperature, then by dried filter cake and 3~5g
The carbon black for being crushed to 325~500 mesh is well mixed, and is transferred to Muffle furnace, with 3~5mL/min speed to being passed through argon gas in stove,
Under argon gas guard mode, 680~700 DEG C are warming up to 6~8 DEG C/min rate programs, after 20~30min of insulation calcining, continued
1100~1200 DEG C are warming up to 10~15 DEG C/min rate programs, insulation 45~60min of calcining cools to room temperature with the furnace, goes out
Material, obtains calcined mixed powder；
(4) it is 10~15% sodium carbonate liquors to pour into above-mentioned gained calcined mixed powder and fill 400~600mL mass fractions
In evaporating dish, after stirring 10~15min of mixing with glass bar, material in evaporating dish is then transferred to tubular type by heating evaporation to dry
In resistance furnace, 30~45min, room temperature to be cooled to the furnace, by tubular electric resistance are calcined under the conditions of being 1100~1200 DEG C in temperature
Material is poured into the beaker for filling 1~2L water in stove, and after stirring 15~20min of mixing with glass bar, filter cake is collected in filtering, and
Gained filter cake is placed in baking oven, is dried to constant weight under the conditions of being 105~110 DEG C in temperature, obtain final product the support of high-strength light pressure break
Agent.
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| CN108219768A (en) * | 2017-12-12 | 2018-06-29 | 常州莱尚纺织品有限公司 | A kind of ceramsite petroleum fracturing propping agents and preparation method thereof |
| CN110330312A (en) * | 2019-07-11 | 2019-10-15 | 江苏爱园健康科技有限公司 | It is a kind of it is high absorption, Gao Baoshui porous ceramic grain production line |
| CN110372326A (en) * | 2019-06-12 | 2019-10-25 | 魏炎梅 | A kind of preparation method of heatproof and shockproof ceramic filtering material |
| CN112500170A (en) * | 2020-12-21 | 2021-03-16 | 西南石油大学 | Low-density silicon carbide-based complex-phase ceramsite proppant and preparation method thereof |
| CN114956855A (en) * | 2022-07-11 | 2022-08-30 | 郑州市新郑梅久实业有限公司 | Environment-friendly ceramsite production process |
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