CN106747371A - Ceramic fracturing sand with oil-wet behavior and preparation method thereof - Google Patents
Ceramic fracturing sand with oil-wet behavior and preparation method thereof Download PDFInfo
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- CN106747371A CN106747371A CN201611043938.7A CN201611043938A CN106747371A CN 106747371 A CN106747371 A CN 106747371A CN 201611043938 A CN201611043938 A CN 201611043938A CN 106747371 A CN106747371 A CN 106747371A
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- oil
- fracturing sand
- wet behavior
- ceramic
- ceramic fracturing
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- 239000000919 ceramic Substances 0.000 title claims abstract description 51
- 239000004576 sand Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005520 cutting process Methods 0.000 claims abstract description 42
- 238000003795 desorption Methods 0.000 claims abstract description 36
- 229910001570 bauxite Inorganic materials 0.000 claims abstract description 25
- 239000011521 glass Substances 0.000 claims abstract description 24
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims abstract description 21
- 150000004645 aluminates Chemical class 0.000 claims abstract description 14
- 239000007822 coupling agent Substances 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000428 dust Substances 0.000 claims description 16
- 229910000278 bentonite Inorganic materials 0.000 claims description 15
- 239000000440 bentonite Substances 0.000 claims description 15
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000007493 shaping process Methods 0.000 claims description 8
- 239000012467 final product Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000005096 rolling process Methods 0.000 claims description 6
- 239000002689 soil Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000012805 post-processing Methods 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 238000009413 insulation Methods 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 15
- 239000000843 powder Substances 0.000 abstract description 9
- 239000003795 chemical substances by application Substances 0.000 abstract description 7
- 230000006835 compression Effects 0.000 abstract description 7
- 238000007906 compression Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 230000000149 penetrating effect Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 46
- 239000007789 gas Substances 0.000 description 11
- 238000012986 modification Methods 0.000 description 9
- 230000004048 modification Effects 0.000 description 9
- 239000012153 distilled water Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 239000000654 additive Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000005553 drilling Methods 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 235000012054 meals Nutrition 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000002920 hazardous waste Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000024241 parasitism Effects 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 239000010734 process oil Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003220 pyrenes Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
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Abstract
The invention discloses a kind of ceramic fracturing sand with oil-wet behavior, using oil-based drill cuttings residue, potassium feldspar, bauxite, bentonitic different ratio after Thermal desorption, can also improve the performance of ceramic fracturing sand by adding a small amount of waste glass powder, and load by aluminate coupling agent makes the ceramic fracturing sand of preparation have oil-wet behavior.Ceramic fracturing sand with oil-wet behavior of the present invention, with compression strength is big, density is low, it is high to adapt to clossing pressure, the low deep-seated oil gas well fracturing ceramsite propping agent of penetrating power；And sintering temperature relative reduction, between 1,040 1260 DEG C, effective reducing energy consumption can save energy 20% to scope；Reach the small effect of percentage of damage simultaneously.
Description
Technical field
Shale gas exploration and development the invention belongs to environmental protection produces changing rejected material to useful resource technical field and oil, natural
Gas exploits field.More particularly to a kind of ceramic fracturing sand with oil-wet behavior and preparation method thereof.
Background technology
Oil-based drill cuttings are a kind of solid waste produced during shale gas exploration and development, its bulky and composition
Complexity, in addition to containing a large amount of residual oils, also containing noxious materials such as benzene homologues, phenols, anthracene, pyrenes, substantial amounts of pathogen, parasitism
The heavy metals such as worm, copper, chromium, lead, the poisonous and harmful substance of the difficult degradation such as salt and Polychlorinated biphenyls.If oil-based drill cuttings are without effectively place
Reason is just discharged, and not only takes a large amount of soils, and can cause environmental pollution, threatens human health.Oil-based drill cuttings have been put into《State
Family's Hazardous Waste List》, its harmless treatment and recycling also cause the highest attention of people.
Pintsch process technology is that oil-base mud is heated into uniform temperature under conditions of anoxybiotic, the light component oil in waste
Class and moisture are heated and initially evaporate out, it is impossible to which the heavy constituent oils of evaporation is acted on by thermal decomposition and is converted into light component, hydro carbons
Material is separated in complicated hydration and cracking reaction, then is evaporated in a gaseous form, and condenses recovery, so as to realize
The purpose that oil with drilling cuttings separate.The gas phase produced in Pintsch process process forms three kinds of phase materials after cooling, and gas phase is with H2、
CH4, based on CO etc.；Liquid phase is with gasoline, diesel oil, paraffin hydrocarbon and H2Based on O；Solid phase is mud solid formation and carbon residue.Pintsch process work
More thoroughly, the residue oil-containing after treatment can reach 0.01% (100mg/kg) below to the ratio that skill is processed oil-base mud, be
Compare the method for being successfully processed, but the heavy constituent such as residue the inside bituminous.Mainly pass through Thermal desorption pair currently for oil-based drill cuttings
Oil is reclaimed, and realizes resource reutilization, but《National Hazard waste register》It has been specified that after oil-based drill cuttings Thermal desorption
Residue remains as dangerous waste.Residue after current Thermal desorption carries out landfill disposal and there is environmentally friendly risk, by Oil And Gas Fields
Each place Environmental Protection Agency prohibites.How to process oil-based drill cuttings residue after substantial amounts of Thermal desorption is still asking for urgent need to resolve
Topic.
At present, the patent such as publication number CN101787270B, CN 101787270A, CN103173204A using gangue and
Flyash is waste fracturing sand, so as to realize the recycling of waste, but needs to add multiple additives and auxiliary material；Still
It was found that by the use of oil-based drill cuttings Thermal desorption residue as the report and patent of waste fracturing sand.
The content of the invention
Residue is still dangerous waste after the technical problems to be solved by the invention are directed to oil-based drill cuttings pyrolysis, it is impossible to realize nothing
The problem of evilization and resource and new approaches that the hazardous waste that proposes is recycled, there is provided a kind of haydite pressure with oil-wet behavior
Sand is split, with compression strength is big, density is low, it is high to adapt to clossing pressure, the low deep-seated oil gas well fracturing haydite branch of penetrating power
Support agent.
It is a further object of the present invention to provide the preparation method of the above-mentioned ceramic fracturing sand with oil-wet behavior.
The present invention is to solve the problems, such as that used technical scheme set forth above is：
Ceramic fracturing sand with oil-wet behavior, particle diameter is 30-100 mesh, and it is mainly by oil-based drill cuttings Thermal desorption residue, aluminium
Alumina, potassium feldspar, bentonite are constituted, and each raw material is according to the mass fraction：5-50 parts of oil-based drill cuttings Thermal desorption residue, bauxite
10-60 parts, potassium feldspar 5-20 parts, bentonite 3-20 parts.
By such scheme, glass dust is also included in the raw material of the haydite with oil-wet behavior, in the form of additive
Add, the addition of glass dust accounts for the 0-20% of other raw material gross weights.
By such scheme, the oil-based drill cuttings Thermal desorption residue is that the solid produced during shale gas exploration and development gives up
Gurry is by the residue after Thermal desorption treatment.The mainly SiO containing 50-60% in oil-based drill cuttings Thermal desorption residue2, 5-10%'s
Al2O3, the Fe of 1-3%2O3, the MgO of 0.1-3%, the CaO of 5-10%, less than 0.3%, others are exactly inorganic mineral substance to oil-containing
Thing and inevitable impurity (percentage is in terms of mass fraction in oil-based drill cuttings Thermal desorption residue).
By such scheme, the bauxite is the grade bauxite high, middle of quality of alumina content 50-90%.
The method of the ceramic fracturing sand with oil-wet behavior of the present invention, it is comprised the following steps：
(1) oil-based drill cuttings Thermal desorption residue need not carry out de-oiling and dry pretreatment, directly carry out follow-up dispensing；
(2) according to the mass fraction, by 5-50 parts of oil-based drill cuttings Thermal desorption residue, bauxite 10-60 parts, potassium feldspar 5-20
Part, bentonite 3-20 parts of mixing and ball milling are uniformly sieved afterwards；
(3) by the material rolling shaping after step (2) gained ball milling sieving, the size of control material granularity, balling-up time
Length, prepare particle diameter be 30-100 mesh haydite green compact；
(4) the haydite green compact after step (3) gained shaping are heated up and is sintered, sintering temperature is 1040-1260 DEG C, high
Warm soaking time is 1-3 hours, and sieving is cooled down after the completion of sintering, and (particle diameter the is 30-100 mesh) haydite for obtaining different size is produced
Product；
(5) after step (4) gained haydite being washed into the post processing such as drying through peracid foam washing, it is soaked in modified solution to load and changes
Property after dry, obtain final product the ceramic fracturing sand with oil-wet behavior.
Preferably, the cigarette that the flue gas that the sintering process in the step (4) is produced is adsorbed by lime and SCR denitration is constituted
Discharged after gas processing system treatment, the flue gas of discharge meets discharge standard.
Preferably, the performance of haydite, glass can be improved in the raw material of the step (2) by adding a small amount of waste glass powder
The addition of powder accounts for the 0-20% of total other raw material gross weights.
Preferably, heating rate is 3-7 DEG C/min in the step (4).
Preferably, the haydite for being prepared in the step (5) is post-processed, and last handling process is mainly first uses haydite
Water cleans drying, then uses H2SO4After solution (PH≤3) immersion 12-24h, then rinsed to neutrality, dry for standby with water.
Preferably, the modified solution is mainly formulated by aluminate coupling agent, water, ethanol；Preferably, Aluminate idol
Connection agent, water, the mass ratio of ethanol are 1:8:10；Also, the pH value control of modified solution is adjusted in 3-6 using inorganic acid.
Preferably, loaded modified temperature is 60-90 DEG C in the step (5), and the loaded modified time is 20-60min.
The present invention is subject to a certain amount of potassium feldspar, bauxite, bentonite with oil-based drill cuttings Thermal desorption residue as primary raw material
Deng the ceramic fracturing sand being made through high temperature sintering with higher-strength and with oil-wet behavior.Wherein, potassium feldspar and high, middle grade
Bauxite is mainly used in adjusting the chemical composition of ceramic fracturing sand, makes its SiO2-Al2O3-K2O is controlled in zone of reasonableness, so as to protect
Card ceramic fracturing sand has compression strength and preferable acid-alkali-corrosive-resisting higher.Meanwhile, potassium feldspar and oil-based drill cuttings are pyrolyzed
Analysis residue in organic principle pyroreaction can be provided required for gas phase and liquid phase environment, make ceramic fracturing sand that there is certain hole
Gap rate and absorption property.Bentonite is mainly used in improving the balling-up efficiency of material；Glass dust is mainly used in improving the resistance to compression of haydite
Intensity；Aluminate coupling agent is in ceramic fracturing sand microcellular structure, to make it by stabilization after load as the effect of modifying agent
Oil-wet behavior is improved.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) the ceramic fracturing sand with oil-wet behavior of the present invention, with compression strength is big, density is low, adapts to close
Resultant pressure is high, the low deep-seated oil gas well fracturing ceramsite propping agent of penetrating power；And sintering temperature relative reduction, scope exists
Between 1040-1260 DEG C, effective reducing energy consumption can save energy 20%；Reach the small effect of percentage of damage simultaneously.
(2) the ceramic fracturing sand compression strength with oil-wet behavior of the present invention is big, acid-alkali-corrosive-resisting is good, be difficult
Powder, can make various function fracturing sands of clossing pressure 52MPa, 69MPa and 86Mpa；And, the ceramic fracturing sand added value
Height, while realizing that dangerous waste is thoroughly innoxious, with economic benefit higher.
(3) primary raw material oil-based drill cuttings Thermal desorption residue of the invention produces discarded oil base from shale gas exploration and development
Drilling cuttings, high, middle grade bauxite is prepared as primary raw material with high, middle grade bauxite with oil-based drill cuttings Thermal desorption residue and made pottery
Grain fracturing sand, meets the innoxious of fixed-end forces, minimizing and resource principle.
(4) the oleophylic water resistance characteristic of ceramic fracturing sand, aluminic acid are strengthened in the present invention as modifying agent using aluminate coupling agent
The load of ester coupling agent, additionally enhances the oleophylic performance of ceramic fracturing sand, and passing through for water is hindered under elevated pressure, accelerates fluid
Pass through.
(5) present invention has for the innoxious of oil-based drill cuttings Thermal desorption residue, resource and industrialization treatment provide one
Effect approach, oil-based drill cuttings Thermal desorption residue utilization rate is high, non-secondary pollution, added value are high, especially meets the nothing of fixed-end forces
Evilization, minimizing and resource principle, with vast potential for future development, with preferable economic benefit and environmental benefit.
Brief description of the drawings
Fig. 1 is the process chart of the ceramic fracturing sand with oil-wet behavior prepared by the present invention.
Specific embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention is not
It is limited only to the following examples.
In the present invention unless otherwise specified, percentage is by percentage to the quality.
Embodiment 1
Ceramic fracturing sand with oil-wet behavior, it is mainly by oil-based drill cuttings Thermal desorption residue, bauxite, potassium feldspar, swollen
Profit local soil type is into each raw material is according to the mass fraction：20 parts of the oil-based drill cuttings Thermal desorption residue of oil content 0.3%, high, middle grade aluminum
60 parts of alumina, 15 parts of potassium feldspar, 5 parts of bentonite.
The preparation method of the above-mentioned ceramic fracturing sand with oil-wet behavior, it is comprised the following steps：
(1) by base drilling cuttings Thermal desorption residue, high, middle grade bauxite, potassium feldspar, bentonite is with 20：60：15：5 weight
Than carrying out mixing and ball milling, the material after ball milling crosses screen cloth；
(2) material after ball milling sieving is put into rolling shaping in nodulizer, the size, balling-up time according to raw meal particle size
Length, prepares the haydite green compact that particle diameter is 30-100 mesh；
(3) the haydite green compact after being molded are sintered by rotary kiln, and sintering temperature is 1160 DEG C, are incubated 2.5h, cooling
After sieving, the ceramic product of different size is obtained；
(4) haydite that will be prepared first washes drying, then with the H of 1mol/L2SO4Immersion 24h, after rushed with water again
It is washed till neutrality, dry for standby；
(5) haydite that step (4) is treated is soaked in and is configured to by aluminate coupling agent, distilled water, absolute ethyl alcohol
(aluminate coupling agent, distilled water, the mass ratio of absolute ethyl alcohol are 1 in modified solution:8:10), modification temperature is 90 DEG C, is changed
Property time 20min, be modified after with vacuum drier dry, obtain final product the ceramic fracturing sand with oil-wet behavior.
Embodiment 2
Ceramic fracturing sand with oil-wet behavior, it is mainly by oil-based drill cuttings Thermal desorption residue, bauxite, potassium feldspar, swollen
Profit soil, glass dust are constituted, and each raw material is according to the mass fraction：45 parts of the oil-based drill cuttings Thermal desorption residue of oil content 0.2%, high,
35 parts of middle grade bauxite, 10 parts of potassium feldspar, 10 parts of bentonite；Glass dust is added in the form of additive, the addition of glass dust
Amount accounts for the 15% of other raw material gross weights.
The preparation method of the above-mentioned haydite with oil-wet behavior, it is comprised the following steps：
(1) base drilling cuttings Thermal desorption residue, high, middle grade bauxite, potassium feldspar, bentonite is with 45：35：10：10 weight
Than being mixed, and by the 15% additional waste glass powder ball milling together of compound gross mass, the material after ball milling crosses screen cloth；
(2) material after ball milling sieving is put into rolling shaping in nodulizer, the size, balling-up time according to raw meal particle size
Length can prepare the haydite green compact that particle diameter is 30-100 mesh；
(3) the haydite green compact after being molded are sintered by rotary kiln, and sintering temperature is 1200 DEG C, are incubated 2.5h, cooling
After sieving, the ceramic product of different size is obtained；
(4) haydite that will be prepared is pre-processed, and mainly first washes drying, then with the H of 1mol/L2SO4Leaching
Bubble 18h, after rinsed to neutrality, dry for standby with water again；
(5) by pretreated haydite be soaked in by aluminate coupling agent, distilled water, absolute ethyl alcohol be configured to it is modified molten
(aluminate coupling agent, distilled water, the mass ratio of absolute ethyl alcohol are 1 in liquid:8:10), modification temperature is 80 DEG C, modification time
30min, is dried after being modified with vacuum drier, obtains final product the ceramic fracturing sand with oil-wet behavior.
Embodiment 3
Ceramic fracturing sand with oil-wet behavior, it is mainly by oil-based drill cuttings Thermal desorption residue, bauxite, potassium feldspar, swollen
Profit soil, glass dust are constituted, and each raw material is according to the mass fraction：30 parts of the oil-based drill cuttings Thermal desorption residue of oil content 0.1%, high,
40 parts of middle grade bauxite, 20 parts of potassium feldspar, 10 parts of bentonite；Glass dust is added in the form of additive, the addition of glass dust
Amount accounts for the 20% of other raw material gross weights.
The preparation method of the above-mentioned ceramic fracturing sand with oil-wet behavior, it is comprised the following steps：
(1) oil-based drill cuttings Thermal desorption residue, high, middle grade bauxite, potassium feldspar, bentonite is with 30：40：20：10 weight
Amount ratio is mixed, and by the 20% additional waste glass powder ball milling together of compound gross mass, the material after ball milling crosses screen cloth；
(2) material after ball milling sieving is put into rolling shaping in nodulizer, the size, balling-up time according to raw meal particle size
Length can prepare the haydite green compact that particle diameter is 30-100 mesh；
(3) the haydite green compact after being molded are sintered by rotary kiln, and sintering temperature is 1230 DEG C, are incubated 2.5h, cooling
After sieving, the ceramic product of different size is obtained；
(4) haydite that will be prepared is pre-processed, and mainly first washes drying, then with the H of 1mol/L2SO4Leaching
Bubble 16h, after rinsed to neutrality, dry for standby with water again；
(5) by pretreated haydite be soaked in by aluminate coupling agent, distilled water, absolute ethyl alcohol be configured to it is modified molten
(aluminate coupling agent, distilled water, the mass ratio of absolute ethyl alcohol are 1 in liquid:8:10), modification temperature is 60 DEG C, modification time
60min, is dried after being modified with vacuum drier, obtains final product the ceramic fracturing sand with oil-wet behavior.
Embodiment 4
Ceramic fracturing sand with oil-wet behavior, it is mainly by oil-based drill cuttings Thermal desorption residue, bauxite, potassium feldspar, swollen
Profit soil, glass dust are constituted, and each raw material is according to the mass fraction：50 parts of oil-based drill cuttings Thermal desorption residue, high, middle grade bauxite 15
Part, 15 parts of potassium feldspar, 5 parts of bentonite；Glass dust is added in the form of additive, and the addition of glass dust accounts for other raw material gross weights
The 5% of amount.
The preparation method of the above-mentioned ceramic fracturing sand with oil-wet behavior, it is comprised the following steps：
(1) oil-based drill cuttings Thermal desorption residue, high, middle grade bauxite, potassium feldspar, bentonite is with 50：15：15：5 weight
Than being mixed, and by the 5% additional waste glass powder ball milling together of compound gross mass, the material after ball milling crosses screen cloth；
(2) in waste glass powder being added into step (2) mixed material, added ratio is compound 85%, waste glass powder
15%, ball milling again after addition, the material after ball milling sieving is put into rolling shaping in nodulizer, size according to raw meal particle size, into
The length of ball time can prepare the haydite green compact that particle diameter is 30-100 mesh；
(3) the haydite green compact after being molded are sintered by rotary kiln, and sintering temperature is 1180 DEG C, are incubated 2.5h, cooling
After sieving, the ceramic product of different size is obtained；
(4) haydite that will be prepared is pre-processed, and mainly first washes drying, then with the H of 1mol/L2SO4Leaching
Bubble 12h, after rinsed to neutrality, dry for standby with water again；
(5) by pretreated haydite be soaked in by aluminate coupling agent, distilled water, absolute ethyl alcohol be configured to it is modified molten
(aluminate coupling agent, distilled water, the mass ratio of absolute ethyl alcohol are 1 in liquid:8:10), modification temperature is 90 DEG C, modification time
30min, is dried after being modified with vacuum drier, obtains final product the ceramic fracturing sand with oil-wet behavior.
The ceramic fracturing sand with oil-wet behavior prepared by above-described embodiment 1-4, its physical and chemical performance test is as follows
Table：
The ceramic fracturing sand inside that gained of the invention has oil-wet behavior is full of space and even aperture distribution, and this is haydite
Why fracturing sand possesses the internal cause of low-density and higher-strength, is also based primarily upon this, just can carry out preferable parent to haydite
Oily modification.As seen from the above table：Gained of the invention has the ceramic fracturing sand of oil-wet behavior, with compression strength is big, density
Low, adaptation clossing pressure is high, the low deep-seated oil gas well fracturing ceramsite propping agent of penetrating power；And the relative drop of sintering temperature
Low, between 1040-1260 DEG C, effective reducing energy consumption can save energy 20% to scope；Reach the small effect of percentage of damage simultaneously.
The above is only the preferred embodiment of the present invention, it is noted that come for one of ordinary skill in the art
Say, without departing from the concept of the premise of the invention, can also make some modifications and variations, these belong to of the invention
Protection domain.
Claims (9)
1. there is the ceramic fracturing sand of oil-wet behavior, it is characterised in that main long by oil-based drill cuttings Thermal desorption residue, bauxite, potassium
Stone, bentonite are constituted, and each raw material is according to the mass fraction：5-50 parts of oil-based drill cuttings Thermal desorption residue, bauxite 10-60 parts, potassium
Feldspar 5-20 parts, bentonite 3-20 parts.
2. the ceramic fracturing sand with oil-wet behavior according to claim 1, it is characterised in that also include in the raw material
Glass dust, the addition of glass dust accounts for the 0-20% of other raw material gross weights.
3. the ceramic fracturing sand with oil-wet behavior according to claim 1, it is characterised in that the oil-based drill cuttings pyrolysis
Analysis residue mainly includes the residue for producing oil-based drill cuttings to be produced after Thermal desorption during shale gas exploitation.
4. the ceramic fracturing sand with oil-wet behavior according to claim 1, it is characterised in that the bauxite is oxidation
The grade bauxite high, middle of aluminium mass content 50-90%.
5. there is the preparation method of the ceramic fracturing sand of oil-wet behavior, it is characterised in that it is comprised the following steps：
(1) according to the mass fraction, by 5-50 parts of oil-based drill cuttings Thermal desorption residue, bauxite 10-60 parts, potassium feldspar 5-20 parts, it is swollen
Profit 3-20 parts of mixing and ball milling of soil is uniformly sieved afterwards；
(2) by the material rolling shaping after step (1) gained ball milling sieving, prepare the haydite that particle diameter is 30-100 mesh and give birth to
Base；
(3) the haydite green compact after step (2) gained shaping are sintered, sintering temperature is 1040-1260 DEG C, 1-3 is small for insulation
When, sieving is cooled down after the completion of sintering, obtain ceramic product；
(4) step (3) gained haydite is dried after loaded modified in after post processing purification, being soaked in modified solution, is obtained final product
Ceramic fracturing sand with oil-wet behavior.
6. one kind according to claim 5 is produced with oil-wet behavior ceramic fracturing sand using oil-based drill cuttings Thermal desorption residue
Method, it is characterised in that be also added with glass dust in the raw material of the step (1), the addition of glass dust accounts for raw material gross weight
0-20%.
7. the preparation method of the ceramic fracturing sand with oil-wet behavior according to claim 5, it is characterised in that the step
Suddenly post processing purification process is mainly haydite is first washed drying in (4), then uses H2SO4After solution immersion 12-24h, then
Drying is washed to neutrality with water.
8. the preparation method of the ceramic fracturing sand with oil-wet behavior according to claim 5, it is characterised in that described to change
Property solution is mainly formulated by aluminate coupling agent, water, ethanol, and pH is 3-6.
9. the preparation method of the ceramic fracturing sand with oil-wet behavior according to claim 5, it is characterised in that the step
Suddenly loaded modified temperature is 60-90 DEG C in (4), and the loaded modified time is 20-60min.
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| CN108641704A (en) * | 2018-04-23 | 2018-10-12 | 中国石油天然气集团有限公司 | A kind of fracturing propping agents and its preparation method and application |
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| CN114426429A (en) * | 2020-09-02 | 2022-05-03 | 中国石油化工股份有限公司 | Filling sand mixture, ceramsite filling sand, and preparation method and application thereof |
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| CN112500170B (en) * | 2020-12-21 | 2021-11-30 | 西南石油大学 | Low-density silicon carbide-based complex-phase ceramsite proppant and preparation method thereof |
| 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 |
| CN114988849A (en) * | 2021-03-01 | 2022-09-02 | 中国石油化工股份有限公司 | Method for preparing high-strength ceramsite by using dried drilling mud as raw material |
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