CN117736718A - Tectorial membrane long-acting porous ceramsite scale inhibition propping agent, preparation method and application - Google Patents
Tectorial membrane long-acting porous ceramsite scale inhibition propping agent, preparation method and application Download PDFInfo
- Publication number
- CN117736718A CN117736718A CN202211159667.7A CN202211159667A CN117736718A CN 117736718 A CN117736718 A CN 117736718A CN 202211159667 A CN202211159667 A CN 202211159667A CN 117736718 A CN117736718 A CN 117736718A
- Authority
- CN
- China
- Prior art keywords
- scale
- propping agent
- ceramsite
- porous ceramsite
- proppant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 230000005764 inhibitory process Effects 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 210000002489 tectorial membrane Anatomy 0.000 title description 3
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 78
- 239000002455 scale inhibitor Substances 0.000 claims abstract description 69
- 238000002156 mixing Methods 0.000 claims abstract description 35
- 239000000919 ceramic Substances 0.000 claims abstract description 26
- 239000000412 dendrimer Substances 0.000 claims abstract description 26
- 229920000736 dendritic polymer Polymers 0.000 claims abstract description 26
- 239000006260 foam Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 20
- 229920003169 water-soluble polymer Polymers 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 114
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000007864 aqueous solution Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000004821 distillation Methods 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000002861 polymer material Substances 0.000 claims description 10
- 239000005457 ice water Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000011403 purification operation Methods 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 6
- 239000004927 clay Substances 0.000 claims description 5
- 229940087646 methanolamine Drugs 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 108010010803 Gelatin Proteins 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 229920006327 polystyrene foam Polymers 0.000 claims description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 229910001570 bauxite Inorganic materials 0.000 claims description 2
- 239000010881 fly ash Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000010802 sludge Substances 0.000 claims description 2
- 230000002401 inhibitory effect Effects 0.000 claims 13
- 238000002485 combustion reaction Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 12
- 238000011161 development Methods 0.000 abstract description 7
- 238000011068 loading method Methods 0.000 abstract description 5
- 230000007774 longterm Effects 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 23
- 239000000243 solution Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000012530 fluid Substances 0.000 description 6
- 238000002791 soaking Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000007664 blowing Methods 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 230000018109 developmental process Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 241000258957 Asteroidea Species 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000004793 Polystyrene Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 230000000857 drug effect Effects 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 229920002223 polystyrene Polymers 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- FDGBQHCDMSYZRC-UHFFFAOYSA-N 2-hydroxy-2-oxo-1,3,2$l^{5}-dioxaphosphinan-4-amine Chemical compound NC1CCOP(O)(=O)O1 FDGBQHCDMSYZRC-UHFFFAOYSA-N 0.000 description 2
- PTLXXCCTGURQMN-UHFFFAOYSA-N CC1OP(O)(=O)OP(=O)(OO)O1 Chemical compound CC1OP(O)(=O)OP(=O)(OO)O1 PTLXXCCTGURQMN-UHFFFAOYSA-N 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 238000007112 amidation reaction Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 238000006845 Michael addition reaction Methods 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- DDAQLPYLBPPPRV-UHFFFAOYSA-N [4-(hydroxymethyl)-2-oxo-1,3,2lambda5-dioxaphosphetan-2-yl] dihydrogen phosphate Chemical compound OCC1OP(=O)(OP(O)(O)=O)O1 DDAQLPYLBPPPRV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- XTOQOJJNGPEPMM-UHFFFAOYSA-N o-(2-oxo-1,3,2$l^{5}-dioxaphosphinan-2-yl)hydroxylamine Chemical compound NOP1(=O)OCCCO1 XTOQOJJNGPEPMM-UHFFFAOYSA-N 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 229940093429 polyethylene glycol 6000 Drugs 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to the technical field of oil and gas field development, and particularly relates to a coated long-acting porous ceramsite scale inhibition propping agent, a preparation method and application. The invention mixes the ceramic slurry with the burnout organic foam, and screens the mixture after sintering at 1100 ℃ to prepare porous ceramsite with certain strength; mixing the porous ceramsite with the spherical dendritic polymer scale inhibitor, and drying to load the spherical dendritic polymer scale inhibitor on the pores and the surface of the porous ceramsite; finally, the outer surface is covered with a layer of water-soluble polymer film to prepare the film-covered long-acting porous ceramsite scale inhibition propping agent. The propping agent prepared by the invention has large drug-loading capacity and high strength; the high-temperature scale inhibition effect is good, the scale inhibitor can be slowly released under stratum conditions, the action period is long, and the scale inhibition rate is more than 60% in 300 days at 100 ℃; the long-term scale inhibition effect can be achieved on a reservoir and a shaft, the scaling problem after fracturing is effectively relieved, and technical support is provided for economic and efficient development of oil fields.
Description
Technical Field
The invention belongs to the technical field of oil and gas field development, and particularly relates to a coated long-acting porous ceramsite scale inhibition propping agent, a preparation method and application.
Background
At present, fracturing reformation is required for the development of unconventional tight oil reservoirs. The fracturing process is characterized in that a large amount of external fluid enters the stratum, well entering liquid interacts with reservoir rock and stratum water, and the fracturing process causes temperature, pressure and pH change, so that the problems of reservoir and wellbore scaling after fracturing are increasingly prominent. The scaling can cause reservoir blockage, sharp reduction of yield, and series of problems such as pump clamps, sucker rod clamps and the like in a shaft, and seriously affect normal production and development. Aiming at the scaling problem, the prior oil field mainly uses a liquid scale inhibitor, and the liquid scale inhibitor is continuously added into a shaft or enters a stratum along with fracturing fluid, but the continuous adding process of the shaft is complex and can not prevent reservoir scaling, and the liquid scale inhibitor is quickly discharged along with flowback after being added into the fracturing fluid, so that the effective period is short (1-3 months), and the long-acting scale inhibition effect can not be achieved. And a small amount of solid scale inhibitor solidified by the liquid scale inhibitor is mixed with the propping agent and enters the stratum, but the scale inhibitor is easy to break and dissolve under the stratum, has a short effective period, blocks crack pores and reduces the diversion capacity. In addition, most of the currently used scale inhibitors are effective at medium and low temperatures, and less effective at high temperatures.
In order to solve the problem, the long-acting scale inhibitor is developed to be mixed with the conventional proppant and then enter the stratum, and the scale inhibitor can be slowly released under the stratum so as to achieve the long-term scale prevention effect.
The invention patent CN106928953A takes hydroxyethylidene diphosphate, polyol phosphate, sodium hexametaphosphate and sodium molybdate as main scale inhibitor, and then the cementing agent is added into the main scale inhibitor to prepare the solid scale inhibitor, so that the problems that the liquid scale inhibitor needs to be continuously filled and the drug effect period is short are effectively solved, but the filling mode is bottom hole filling, and the problem of scaling of a reservoir after fracturing cannot be solved.
The invention patent CN 106753319A utilizes a Hydroxyl Ethylidene Diphosphate (HEDP) and amino trimethylene phosphate (ATMP) scale inhibitor to modify a ceramic proppant, and solves the problem of scale formation in a reservoir, but the effect aging of the scale inhibitor is short and the drug effect period is short because the adsorption strength of the small molecular scale inhibitor such as HEDP/ATMP on the ceramic surface is low.
The invention patent CN 114032084A utilizes the method that the scale control slow release agent is coated on the surface of the propping agent to carry out slow release scale control, solves the problem of slow release of the scale control agent, but because the part playing the role of scale control is coated on the surface of the propping agent, the release period of the propping agent with smaller drug loading is still relatively shorter, meanwhile, the propping agent starts to release the scale control agent when being injected into the fracturing fluid, the general scaling problem at the initial stage of flowback is not obvious, and at the moment, a large amount of scale control agent is released and wasted.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides the coated long-acting porous ceramsite scale inhibition propping agent, which can slowly release the scale inhibition agent under stratum conditions and has long-acting scale inhibition effect on a reservoir and a shaft.
In order to achieve the purpose of the invention, the technical scheme adopted is as follows:
a coated long-acting porous ceramsite scale inhibition propping agent comprises raw materials of porous ceramsite, dendritic polymer scale inhibition agent and water-soluble high polymer material.
Preferably, the water-soluble polymer material is at least one of gelatin, polyacrylamide and polyethylene glycol. The water-soluble high molecular material is characterized by being capable of being dissolved or swelled in water.
Preferably, the water-soluble polymer material is polyethylene glycol.
Preferably, the preparation method of the porous ceramsite comprises the following steps of mixing organic foam with ceramic slurry, firstly burning the organic foam at 200-500 ℃, and then heating and sintering the porous ceramsite.
Preferably, the ceramic slurry is at least one of bauxite, clay, sludge, shale powder, gangue powder and fly ash.
Preferably, the organic foam is at least one of polystyrene foam, polyethylene foam, and phenolic resin foam. The density is 0.1-0.4 g/cm 3 Of these, polystyrene foam is preferred.
Preferably, the organic foam accounts for 10-30% of the volume fraction of the whole system, the burning time is 2-5h, the temperature is raised to 1000-1200 ℃, and the sintering time is 2-5h.
Preferably, the preparation method of the dendritic polymer scale inhibitor comprises the following steps:
(1) Mixing ethylenediamine and methanol, adding methyl acrylate, and reacting to obtain a product G0.5;
(2) Mixing the product G0.5 with methanol, adding ethylenediamine, and reacting to obtain a product G1.0;
(3) Mixing the product G1.0 with methanol, adding methyl acrylate, and reacting to obtain a product G1.5;
(4) Mixing the product G1.5 methanol, adding ethylenediamine, and reacting to obtain a product G2.0;
(5) And adding the product G2.0 into NaOH aqueous solution for hydrolysis to obtain the dendrimer scale inhibitor.
Preferably, the molar ratio of ethylenediamine or product G1.0 to methanol in steps (1) and (3) is 1:8-20;
preferably, the molar ratio of ethylenediamine or product G1.0 to methyl acrylate in step (1) and step (3) is from 1:1.1 to 1:5.
Preferably, the mixing is carried out in an ice-water bath at 0 ℃ and stirred and mixed uniformly under the protection of nitrogen; the reaction temperature is 20-30 ℃, the reaction time is 20-28h, and the purification is needed after the reaction, wherein the purification operation is reduced pressure distillation to remove excessive methanol and methyl acrylate.
Preferably, the molar ratio of G0.5 or G1.5 to methanol in steps (2) and (4) is 1:15-25; the temperature of the reaction is 20-30 ℃, and the reaction time is 20-28h; and after the reaction, the reaction needs to be purified, and the purification operation is reduced pressure distillation to remove excessive methanol and ethylenediamine.
Preferably, the mass-to-volume ratio of the product G2.0 to the NaOH aqueous solution in the step (5) is 1:4, the mass concentration of the NaOH aqueous solution is 10%, and the hydrolysis temperature is 45-55 ℃.
The invention also provides a preparation method of the scale inhibition propping agent, which comprises the following steps:
(1) Preparing an aqueous solution of the dendrimer scale inhibitor, mixing with the porous ceramsite, and stirring; obtaining the adsorbed ceramsite;
(2) Drying the adsorbed ceramsite, and obtaining a porous ceramsite scale inhibition propping agent;
(3) And (3) dissolving the water-soluble polymer material in water, spraying the water-soluble polymer material on the porous ceramsite scale inhibition propping agent, and drying to obtain the porous ceramsite scale inhibition propping agent.
Preferably, the concentration of the aqueous solution in the step (1) is 3-30%, the stirring is performed in a water bath at 40-60 ℃, and the stirring time is 10-14h.
Preferably, the temperature of the drying in the step (2) is 90-100 ℃, and the drying time is 10-14h.
Preferably, in the step (3), the concentration of the water-soluble polymer material after being dissolved in water is 10% -30%, the drying temperature is 80-100 ℃, and the drying time is 6-12 h.
The invention mixes the ceramic slurry with the burnout organic foam, and screens the mixture after sintering at 1100 ℃ to prepare porous ceramsite with certain strength; then, through repeated iteration by utilizing Michael addition reaction and amidation reaction of polyamine-acrylic ester, synthesizing a spherical dendritic high-temperature-resistant polymer scale inhibitor with carboxyl at the tail end; mixing the prepared porous ceramsite with a spherical dendritic polymer scale inhibitor, and drying to load the spherical dendritic polymer scale inhibitor on the pores and the surface of the porous ceramsite; and finally, coating a layer of water-soluble polymer film on the outer surface of the porous ceramsite loaded by the polymer scale inhibitor to prepare the coated long-acting porous ceramsite scale inhibition propping agent.
The invention also aims to provide the application of the scale inhibition propping agent, and the scale inhibition propping agent is mixed with propping agent with the same particle size according to the volume ratio of 1:9-1:99 and then used for fracturing operation.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, the ceramic slurry is used for mixing burnout organic foam, the high-strength porous ceramic particles are prepared through sintering, the spherical dendritic high-temperature-resistant polymer scale inhibitor with rich chelating groups is synthesized, in view of the characteristics that the spherical dendritic polymer scale inhibitor has strong adsorption capacity and the porous ceramic particles have larger specific surface, the spherical dendritic polymer scale inhibitor is loaded in the porous ceramic particles and after the porous ceramic particles have the surface, so that the porous ceramic particle scale inhibitor has larger drug loading capacity, meanwhile, the porous ceramic particle scale inhibitor has high-temperature-resistant property due to rich chelating sites, and finally, the porous ceramic particle scale inhibitor is wrapped on the surface of the ceramic particle scale inhibitor by a water-soluble polymer film, so that the early stage of fracturing flowback is ensured, the scale inhibitor in the ceramic particle scale inhibitor is not easy to run off, and the long-acting slow release effect is achieved. The technology can effectively solve the problem of scale formation of a reservoir and a shaft in the development process of an oil-gas field, and has the advantages of high temperature resistance, large drug loading capacity, high strength, slow release and controllable release.
(2) The propping agent prepared by the invention has large drug-loading rate and high strength, and the crushing rate is basically not influenced under 69Mpa after the propping agent is mixed with the regular haydite with the same particle size according to the volume ratio of 1:9-1:99; the high-temperature scale inhibition effect is good, the scale inhibitor can be slowly released under stratum conditions, the action period is long, and the scale inhibition rate is more than 60% in 300 days at 100 ℃; the long-term scale inhibition effect can be achieved on a reservoir and a shaft, the scaling problem after fracturing is effectively relieved, and technical support is provided for economic and efficient development of oil fields.
Detailed Description
The invention is further described in connection with the following detailed description.
Example 1
The preparation method of the porous ceramsite scale inhibition propping agent comprises the following steps:
A. preparation of porous ceramsite:
20% of 0.2g/cm 3 Fully mixing polystyrene organic foam (manufactured by Fu Xin environmental protection materials science and technology Co., ltd.) with 80% clay ceramic slurry (manufactured by Zhengzhou Kerui refractory Co., ltd.), placing the mixture in an oven at 500 ℃ for 5 hours, sintering the organic foam at 1100 ℃ for 2 hours after the organic foam is completely burnt out, cooling, taking out ceramsite, and sieving to obtain the porous ceramsite propping agent.
Taking 30-50 mesh prepared porous ceramsite propping agent and 1.65g/cm 3 Conventional ceramsite propping agents (manufactured by Shanghai Starfish energy science and technology Co., ltd.) are mixed according to a volume ratio of 1:10, the test breaking rate is 4.7% under the closing pressure of 52MPa, and the test breaking rate is 6.9% under the closing pressure of 69 MP. In contrast, the conventional ceramsite proppant had a breakage rate of 4.0% at 52MPa and 6.1% at a closing pressure of 69 MP. The conventional ceramic propping agent is mixed with a certain porous propping agent, and the supporting strength and the crushing rate of the porous propping agent are basically unchanged.
B. Synthesis of dendrimer scale inhibitor:
(1) Adding ethylenediamine and methanol with a molar ratio of 1:8 into a three-neck flask provided with a magnetic stirring, reflux condensing tube and a constant pressure dropping funnel;
(2) Then placing the three-mouth bottle into an ice water bath with the temperature of 0 ℃ and stirring and mixing uniformly under the protection of nitrogen;
(3) Slowly dropwise adding methyl acrylate with the molar ratio of ethylenediamine to 1:1.2, slowly raising the temperature to the normal temperature of 25 ℃ after the dropwise adding is completed, and reacting for 24 hours;
(4) Removing excessive methanol and methyl acrylate by reduced pressure rotary distillation to obtain a pale yellow product G0.5;
(5) Adding the synthesized G0.5 and methanol into a three-neck flask according to the mol ratio of 1:15, and slowly dropwise adding the mixture with the mol ratio of 1:8, reacting for 24 hours at normal temperature, and carrying out the same purification operation as G0.5 to obtain a yellowish viscous product G1.0;
(6) Mixing G1.0 and methanol according to a molar ratio of 1:20, then placing the three-mouth bottle into an ice water bath with the temperature of 0 ℃, and stirring and mixing uniformly under the protection of nitrogen; slowly dropwise adding methyl acrylate with the molar ratio of 1:1.2 to ethylenediamine, slowly raising the temperature to the normal temperature of 25 ℃ after the dropwise adding is completed, and reacting for 24 hours; removing excessive methanol and methyl acrylate by reduced pressure rotary distillation to obtain a pale yellow product G1.5;
mixing G1.5 with methanol, adding the mixture into a three-neck flask according to a molar ratio of 1:25, and slowly dropwise adding the mixture and the molar ratio of the slowly dropwise adding mixture to the methanol being 1:8, reacting for 24 hours at normal temperature, and removing excessive methanol and ethylenediamine by reduced pressure rotary distillation to obtain a pale yellow viscous product G2.0;
(7) And adding G2.0 into 10% NaOH aqueous solution according to the ratio of 1:4, and slowly hydrolyzing at 50 ℃ to obtain the dendritic polymer scale inhibitor G2.0-COONa with all carboxyl at the tail end. The spherical dendritic polymer scale inhibitor with carboxyl end is synthesized by repeated iteration through Michael specific addition reaction and amidation reaction of polyamine-acrylic ester.
C. Preparation of porous ceramsite scale inhibition propping agent
20G of the prepared porous ceramsite proppant is placed in a 250ml beaker, 100ml of prepared aqueous solution G2.0-COONa of 20% of spherical dendrimer scale inhibitor is poured into the beaker, the solution is completely immersed in the proppant, the proppant is placed in a water bath kettle at 40 ℃ for full absorption for 12 hours, and then the ceramsite is taken out and dried at 100 ℃ to obtain the dendrimer scale inhibitor loaded porous ceramsite proppant.
D. Preparation of coated porous ceramsite scale inhibition propping agent
Blowing the prepared supported scale inhibitor proppant into a fluidized bed, spraying 20% polyethylene glycol 6000 aqueous solution on the surface of the proppant, and drying at 100 ℃ by blowing air to obtain the coated porous ceramsite scale inhibitor proppant.
Example 2
A. Preparation of porous ceramsite:
10% of 0.2g/cm 3 Fully mixing polystyrene organic foam with 80% clay ceramic slurry, then placing the mixture in a 255 ℃ oven for 5 hours, sintering the mixture at 1000 ℃ for 5 hours after the organic foam is completely burnt out, cooling, taking out ceramsite, and screening to obtain the porous ceramsite proppant.
Taking 1.65g/cm of 30-50 mesh prepared porous ceramsite propping agent and Shanghai Starfish month energy science and technology Co., ltd 3 Conventional ceramsite propping agent is prepared according to the volume ratio of 1:10, the breaking rate was 4.6% at a closing pressure of 52MPa and 6.7% at a closing pressure of 69 MP. In contrast, the conventional ceramsite proppant had a breakage rate of 4.0% at 52MPa and 6.1% at a closing pressure of 69 MP. The conventional ceramic propping agent is mixed with a certain porous propping agent, and the supporting strength and the crushing rate of the porous propping agent are basically unchanged.
B. Synthesis of dendrimer scale inhibitor:
(1) Adding ethylenediamine and methanol with a molar ratio of 1:20 into a three-neck flask equipped with a magnetic stirring, reflux condenser and a constant pressure dropping funnel;
(2) Then placing the three-mouth bottle into an ice water bath with the temperature of 0 ℃ and stirring and mixing uniformly under the protection of nitrogen;
(3) Slowly dropwise adding methyl acrylate with the molar ratio of ethylenediamine to 1:1.5, slowly raising the temperature to the normal temperature of 20 ℃ after the dropwise adding is completed, and reacting for 26 hours;
(4) Removing excessive methanol and methyl acrylate by reduced pressure rotary distillation to obtain a pale yellow product G0.5;
(5) Adding the synthesized G0.5 and methanol into a three-neck flask according to the molar ratio of 1:20, and slowly dropwise adding the mixture with the molar ratio of 1:20, reacting for 24 hours at normal temperature, and carrying out the same purification operation as G0.5 to obtain a pale yellow viscous product G1.0;
(6) Mixing G1.0 and methanol according to a molar ratio of 1:20, then placing the three-mouth bottle into an ice water bath with the temperature of 0 ℃, and stirring and mixing uniformly under the protection of nitrogen; slowly dropwise adding methyl acrylate with the molar ratio of ethylenediamine to ethylenediamine of 1:1.5, slowly raising the temperature to the normal temperature of 25 ℃ after the dropwise adding is completed, and reacting for 24 hours; removing excessive methanol and methyl acrylate by reduced pressure rotary distillation to obtain a pale yellow product G1.5;
mixing G1.5 with methanol, adding into a three-neck flask according to a molar ratio of 1:20, slowly dropwise adding ethylenediamine, reacting for 24 hours at normal temperature, and performing reduced pressure rotary distillation to remove excessive methanol and ethylenediamine to obtain a pale yellow viscous product G2.0;
(7) G2.0 is added into 10 percent NaOH aqueous solution according to the proportion of 1:4, and is slowly hydrolyzed at 50 ℃ to obtain 33 percent of dendritic polymer scale inhibitor G2.0-COONa with all carboxyl ends.
C. Preparation of porous ceramsite scale inhibition propping agent
20G of the prepared porous ceramsite proppant is placed in a 250ml beaker, 100ml of prepared 10% aqueous solution G2.0-COONa of the spherical dendritic polymer scale inhibitor is poured into the beaker, the solution is completely immersed in the proppant, the proppant is placed in a water bath kettle at 40 ℃ for fully adsorbing for 12 hours, and then the ceramsite is taken out and dried at 100 ℃ to obtain the dendritic no-scale agent loaded porous ceramsite proppant.
D. Preparation of coated porous ceramsite scale inhibition propping agent
Blowing the prepared supported scale inhibitor propping agent into a fluidized bed, spraying a 20% gelatin aqueous solution on the surface of the propping agent, and drying the blown air at 100 ℃ to prepare the coated porous ceramsite scale inhibitor propping agent.
Example 3
B. Preparation of porous ceramsite:
20% of 0.2g/cm 3 Fully mixing polystyrene organic foam with 80% clay ceramic slurry, then placing the mixture into a baking oven at 500 ℃ for 5 hours, sintering the organic foam at 1100 ℃ for 2 hours after the organic foam is completely burnt out, cooling, taking out ceramsite, and sieving to obtain the porous ceramsite proppant.
Taking 1.65g/cm of 30-50 mesh prepared porous ceramsite propping agent and Shanghai Starfish month energy science and technology Co., ltd 3 The conventional ceramsite propping agent is mixed according to the volume ratio of 1:10, the test breaking rate is 4.7% under the closing pressure of 52MPa, and the test breaking rate is 6.9% under the closing pressure of 69 MP. In contrast, the conventional ceramsite proppant had a breakage rate of 4.0% at 52MPa and 6.1% at a closing pressure of 69 MP. The conventional ceramic propping agent is mixed with a certain porous propping agent, and the supporting strength and the crushing rate of the porous propping agent are basically unchanged.
B. Synthesis of dendrimer scale inhibitor:
(1) Adding ethylenediamine and methanol with a molar ratio of 1:10 into a three-neck flask equipped with a magnetic stirring, reflux condenser and a constant pressure dropping funnel;
(2) Then placing the three-mouth bottle into an ice water bath with the temperature of 0 ℃ and stirring and mixing uniformly under the protection of nitrogen;
(3) Slowly dropwise adding methyl acrylate with the molar ratio of 1:1.1 to ethylenediamine, slowly raising the temperature to the normal temperature of 25 ℃ after the dropwise adding is completed, and reacting for 24 hours;
(4) Removing excessive methanol and methyl acrylate by reduced pressure rotary distillation to obtain a pale yellow product G0.5;
(5) Adding synthesized G0.5 and methanol into a three-neck flask according to a molar ratio of 1:20, slowly dropwise adding ethylenediamine, reacting for 24 hours at normal temperature, and performing the same purification operation as that of G0.5 to obtain a light yellow sticky product G1.0;
(6) Mixing G1.0 and methanol according to a molar ratio of 1:10, then placing the three-mouth bottle into an ice water bath with the temperature of 0 ℃, and stirring and mixing uniformly under the protection of nitrogen; slowly dropwise adding methyl acrylate, slowly raising the temperature to normal temperature of 25 ℃ after the dropwise adding is completed, and reacting for 24 hours; removing excessive methanol and methyl acrylate by reduced pressure rotary distillation to obtain a pale yellow product G1.5;
mixing G1.5 with methanol, adding into a three-neck flask according to a molar ratio of 1:20, slowly dropwise adding ethylenediamine, reacting for 24 hours at normal temperature, and performing reduced pressure rotary distillation to remove excessive methanol and ethylenediamine to obtain a yellowish viscous product G1.0;
(7) G2.0 is added into 10 percent NaOH aqueous solution according to the proportion of 1:4, and is slowly hydrolyzed at 50 ℃ to obtain 33 percent of dendritic polymer scale inhibitor G2.0-COONa with all carboxyl ends.
C. Preparation of porous ceramsite scale inhibition propping agent
20G of the prepared porous ceramsite proppant is placed in a 250ml beaker, 100ml of prepared 30% aqueous solution G2.0-COONa of the spherical dendritic polymer scale inhibitor is poured into the beaker, the solution is completely immersed in the proppant, the proppant is placed in a water bath kettle at 40 ℃ for fully adsorbing for 12 hours, and then the ceramsite is taken out and dried at 100 ℃ to obtain the dendritic no-scale agent loaded porous ceramsite proppant.
D. Preparation of coated porous ceramsite scale inhibition propping agent
Blowing the prepared supported scale inhibitor propping agent into a fluidized bed, spraying a 20% polyacrylamide aqueous solution on the surface of the propping agent, and drying the blown air at 100 ℃ to prepare the coated porous ceramsite scale inhibitor propping agent.
Experiment one, determination of scale inhibition effect of scale inhibition propping agent of coated porous ceramsite
Firstly, preparing 3 cups of 50ml A (1% CaCl) 2 ) Solution, 2 cups of 50ml B solution (1% NaHCO) 3 ),
Mixing 50ml of solution A in a 1 st cup with 50ml of deionized water at an experimental temperature of 50 ℃ to obtain a sample 1;
50ml of solution A and 50ml of solution B of a 2 nd cup are mixed to obtain a sample 2,
a solid-liquid mixture sample 3 was obtained by mixing 50ml of the solution A in 3 rd cup with 5g of the coated porous ceramic scale inhibition proppant prepared in example 1 and 50mlB th cup.
Samples 1, 2 and 3 were filtered respectively and 2ml of the filtrate was diluted to 100ml, 0.1% aqueous NaOH solution was added, and Ca was added respectively 2+ An indicator was titrated with 0.01mol/L EDTA solution to obtain the amount of EDTA V consumed by samples 1, 2 and 3, respectively 1 、V 2 、V 3 . Using scale inhibition formula E f ＝(V 3 -V 1 )/(V 2 -V 1 ) Scale inhibition was calculated at 100%. The proppant of example 1 has a scale inhibition up to 90%. The measurement methods of examples 2 to 3 were the same as those of example 1, and the results are shown in Table 1 below.
TABLE 1
Experiment II, influence of soaking time on scale inhibition stability
5g of the porous ceramsite scale inhibition propping agent prepared in the examples 1-3 are respectively placed in 100mL of water at 100 ℃ for respectively soaking for 30, 50, 100, 150, 200 and 300 days, the water on the surface of the porous ceramsite scale inhibition propping agent is dried after being wiped, the scale inhibition rate of the solution after soaking is respectively measured according to the method of the experiment I, and the test results are shown in the table 2.
TABLE 2 Polymer porous ceramsite scale inhibition proppant soaking time and scale inhibition rate relationship
From table 2, it can be seen that the scale inhibition rate of the prepared porous ceramsite scale inhibition propping agent can still reach 60% after being soaked for 300 days.
Comparative example 1
30g of the porous ceramic proppant prepared in example 1 was placed in a conical flask, a 20% Hydroxyl Ethylidene Diphosphate (HEDP) scale inhibitor was added thereto until the solution level was higher than the proppant, and the mixture was placed at 40℃for adsorption for 12 hours, followed by drying, to prepare an organic phosphoric acid scale inhibitor. The organic phosphoric acid scale inhibition proppants were soaked in clear water according to a first experiment method, and then scale inhibition rate tests were carried out, and the test results are shown in table 3.
Comparative example 2
30g of the porous ceramsite proppant prepared in example 1 is placed in a conical flask, 30% of aminotrimethylene phosphate (ATMP) scale inhibitor is added into the conical flask until the solution is fully immersed and supported, the porous ceramsite proppant is placed in a constant-temperature water bath at 40 ℃ for fully absorbing for 12 hours, the absorbed scale inhibitor proppant is taken out, the porous ceramsite proppant loaded by the ATMP is dried, the prepared porous ceramsite proppant loaded by the ATMP is soaked in clean water according to a method of experiment I, and then scale inhibition yield test is carried out, wherein the test result is shown in Table 3.
Comparative example 3
This comparative example differs from example 1 in the type of dendrimer scale inhibitor, which is specifically as follows:
and placing 20g of the prepared porous ceramsite propping agent into a conical flask, adding 30% of aminotrimethylene phosphate (ATMP) scale inhibitor into the conical flask until the solution is completely immersed and supported, placing the porous ceramsite propping agent into a constant-temperature water bath kettle at 40 ℃ for fully absorbing for 12 hours, taking out the absorbed scale inhibitor, drying to obtain the ATMP-loaded scale inhibitor, blowing the prepared ATMP scale inhibitor into a fluidized bed, spraying 20% of glycol aqueous solution onto the surface of the propping agent, and drying the blown air at 100 ℃ to obtain the ATMP film-coated porous ceramsite scale inhibitor. The prepared ATMP coated porous ceramsite propping agent is soaked in clear water according to the method of the first experiment, and then is subjected to a sufficient rate test, and the test result is shown in Table 3.
TABLE 3 relation between days of soaking and scale inhibition rate of organophosphate scale inhibition proppants
| Soaking time (Tian) | 30 | 50 | 100 | 150 | 200 |
| Comparative example 1 scale inhibition% | 50 | 22 | 0 | 0 | 0 |
| Comparative example 2 scale inhibition% | 52 | 23 | 0 | 0 | 0 |
| Comparative example 3 scale inhibition% | 60 | 23 | 0 | 0 | 0 |
As can be seen from Table 3, the scale inhibition propping agent prepared on the organic phosphoric acid supported porous ceramsite has the scale inhibition rate lower than 70% in 30 days, the scale inhibition effect is obviously reduced in 50 days, and the scale inhibition effect is basically lost even after the film coating treatment is carried out for 100 days, which indicates that the drug effect period of the organic phosphoric acid scale inhibition propping agent is short.
Experiment three, determination of tectorial membrane dissolution time
The prepared porous ceramsite scale inhibition propping agent coated with the film in example 1 is 1.65g/cm produced by Shanghai Starfish month energy science and technology Co., ltd 3 The conventional ceramsite is mixed according to a ratio of 1:10, and then the mixture is put into clear water to observe the membrane swelling and dissolving process of the coated porous propping agent. Until complete dissolution of the film was observed in water after 5 days, the surface produced an aqueous solution of a certain viscosity. The method can be used for preventing the scale inhibitor from being degraded due to the fact that the method can be used for preventing a large amount of fracturing fluid from flowing back in the initial stage of fracturing fluid flowing back and dissolving the scale inhibitor.
The foregoing detailed description is directed to one of the possible embodiments of the present invention, which is not intended to limit the scope of the invention, but is to be accorded the full scope of all such equivalents and modifications so as not to depart from the scope of the invention.
Claims (16)
1. The coated long-acting porous ceramsite scale inhibition propping agent is characterized in that the raw materials of the scale inhibition propping agent comprise porous ceramsite, dendritic polymer scale inhibition agent and water-soluble high polymer material.
2. The scale inhibiting proppant of claim 1, wherein the water soluble polymeric material is at least one of gelatin, polyacrylamide, and polyethylene glycol.
3. The scale inhibiting proppant of claim 1, wherein the water soluble polymeric material is polyethylene glycol.
4. The scale inhibiting proppant of claim 1, wherein the porous ceramsite is prepared by mixing an organic foam with a ceramic slurry, burning the organic foam at a temperature of 200-500 ℃, and then heating to sinter the porous ceramsite.
5. The scale inhibiting proppant of claim 4, wherein the ceramic slurry is at least one of bauxite, clay, sludge, shale powder, gangue powder, and fly ash.
6. The scale inhibiting proppant of claim 4, wherein the organic foam is at least one of polystyrene foam, polyethylene foam, and phenolic resin foam.
7. The scale inhibiting proppant of claim 4, wherein the organic foam comprises 10-30% by volume of the whole system, the time of combustion is 2-5 hours, the temperature is raised to 1000-1200 ℃, and the time of sintering is 2-5 hours.
8. The scale inhibiting proppant of claim 1, wherein the method of preparing the dendrimer scale inhibitor comprises the steps of:
(1) Mixing ethylenediamine and methanol, adding methyl acrylate, and reacting to obtain a product G0.5;
(2) Mixing the product G0.5 with methanol, and adding ethylenediamine to react to obtain a product G1.0;
(3) Mixing the product G1.0 with methanol, adding methyl acrylate, and reacting to obtain a product G1.5;
(4) Mixing the product G1.5 methanol, and adding ethylenediamine to react to obtain a product G2.0;
(5) And adding the product G2.0 into NaOH aqueous solution for hydrolysis to obtain the dendrimer scale inhibitor.
9. The scale inhibiting proppant of claim 8, wherein the molar ratio of ethylenediamine or product G1.0 to methanol in step (1) or (3) is in the range of 1:8-20; the molar ratio of ethylenediamine or product G1.0 to methyl acrylate in step (1) or (3) is in the range of 1:1.1 to 1:5; the mixing is carried out in an ice water bath at 0 ℃ and is stirred and mixed uniformly under the protection of nitrogen; the reaction temperature is 20-30 ℃, the reaction time is 20-28h, and the purification is needed after the reaction, wherein the purification operation is reduced pressure distillation to remove excessive methanol and methyl acrylate.
10. The scale inhibiting proppant of claim 8, wherein the molar ratio of G0.5 or G1.5 to methanol in steps (2) and (4) is from 1:15 to 25; the temperature of the reaction is 20-30 ℃, and the reaction time is 20-28h; and after the reaction, the reaction needs to be purified, and the purification operation is reduced pressure distillation to remove excessive methanol and ethylenediamine.
11. The scale inhibiting proppant of claim 8, wherein the mass to volume ratio of the product G2.0 to NaOH aqueous solution in step (5) is 1:4, the NaOH aqueous solution has a mass concentration of 10%, and the hydrolysis temperature is 45-55 ℃.
12. A method of preparing a scale inhibiting proppant as set forth in any one of claims 1-11 comprising the steps of:
(1) Preparing an aqueous solution of the dendrimer scale inhibitor, mixing with the porous ceramsite, and stirring to obtain adsorbed ceramsite;
(2) Drying the adsorbed ceramsite, and obtaining a porous ceramsite scale inhibition propping agent;
(3) And (3) dissolving the water-soluble polymer material in water, spraying the water-soluble polymer material on the porous ceramsite scale inhibition propping agent, and drying to obtain the porous ceramsite scale inhibition propping agent.
13. The method according to claim 12, wherein the concentration of the scale inhibitor in the aqueous solution in the step (1) is 3-30%, the stirring is performed in a water bath at 40-60 ℃, and the stirring time is 10-14h.
14. The method according to claim 12, wherein the drying temperature in step (2) is 90 to 100 ℃ and the drying time is 10 to 14 hours.
15. The method according to claim 12, wherein the concentration of the water-soluble polymer material after being dissolved in water in the step (3) is 10% -30%, the drying temperature is 80-100 ℃, and the drying time is 6-12 hours.
16. Use of a scale inhibiting proppant as set forth in any one of claims 1-11 in a fracturing operation after mixing the scale inhibiting proppant with a proppant of the same particle size in a volume ratio of 1:9-1:99.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211159667.7A CN117736718A (en) | 2022-09-22 | 2022-09-22 | Tectorial membrane long-acting porous ceramsite scale inhibition propping agent, preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211159667.7A CN117736718A (en) | 2022-09-22 | 2022-09-22 | Tectorial membrane long-acting porous ceramsite scale inhibition propping agent, preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117736718A true CN117736718A (en) | 2024-03-22 |
Family
ID=90276374
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211159667.7A Pending CN117736718A (en) | 2022-09-22 | 2022-09-22 | Tectorial membrane long-acting porous ceramsite scale inhibition propping agent, preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117736718A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117567109A (en) * | 2023-12-02 | 2024-02-20 | 浙江荣圣新材料科技有限公司 | Nano-porous ALC-containing flame-retardant fireproof material for fireproof door |
-
2022
- 2022-09-22 CN CN202211159667.7A patent/CN117736718A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117567109A (en) * | 2023-12-02 | 2024-02-20 | 浙江荣圣新材料科技有限公司 | Nano-porous ALC-containing flame-retardant fireproof material for fireproof door |
| CN117567109B (en) * | 2023-12-02 | 2024-06-04 | 浙江德星新材料科技有限公司 | Nano-porous ALC-containing flame-retardant fireproof material for fireproof door |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| AU2006203483B2 (en) | Delayed tackifying compositions and associated methods involving controlling particulate migration | |
| CA2763357C (en) | Tackifying agent pre-coated particulates | |
| US7595280B2 (en) | Delayed tackifying compositions and associated methods involving controlling particulate migration | |
| CA2438288C (en) | Methods and compositions for consolidating proppant in subterranean fractures | |
| US6209646B1 (en) | Controlling the release of chemical additives in well treating fluids | |
| CA2552049C (en) | Orthoester compositions and methods of use in subterranean applications | |
| US8082994B2 (en) | Methods for enhancing fracture conductivity in subterranean formations | |
| EP2630214B1 (en) | Wellbore cementing compositions and methods of making and using same | |
| CN107880869B (en) | Microcapsule coated acid for oil field and preparation method thereof | |
| CN117736718A (en) | Tectorial membrane long-acting porous ceramsite scale inhibition propping agent, preparation method and application | |
| CN112980410B (en) | Temporary plugging agent for oil field and preparation method thereof | |
| CN109679598B (en) | Strong-wall anti-collapse water-based drilling fluid and preparation method thereof | |
| CN111876138B (en) | Carbon-based tackifier and preparation method and application thereof | |
| CN113150755B (en) | Preparation method of filtrate reducer, drilling fluid and preparation method of drilling fluid | |
| CN106753319B (en) | A kind of method of modifying of antisludging agent to ceramsite propping agent | |
| CN108251096B (en) | Residue-free fracturing fluid loss agent and fluid loss method for fractured reservoir | |
| CN117946644B (en) | Degradable resin plugging agent and preparation method and application thereof | |
| CN115838589B (en) | High-strength particle temporary plugging agent for fracturing diversion and preparation method and application thereof | |
| CN117447976A (en) | Composite multifunctional temporary plugging particle suspension and preparation method and application thereof | |
| CN115926771B (en) | Self-breaking modified soap kernel glue fracturing fluid and use method thereof | |
| CN116410716B (en) | Supermolecule gel temporary plugging agent and preparation method thereof | |
| CN117965144B (en) | Resin mortar plugging system suitable for fracture-cavity stratum, and preparation and application thereof | |
| CN114539994A (en) | Reservoir drilling fluid system and preparation method thereof | |
| CN117025190A (en) | Adjustable temporary plugging agent, preparation method and application | |
| CN117757460A (en) | Sustained-release propping agent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |