CN102660245A - Pre-coated film propping agent, preparation method of the pre-coated film propping agent and sand prevention method adopting the pre-coated film propping agent - Google Patents
Pre-coated film propping agent, preparation method of the pre-coated film propping agent and sand prevention method adopting the pre-coated film propping agent Download PDFInfo
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Abstract
The invention relates to a pre-coated film propping agent, a preparation method of the pre-coated film propping agent and a sand prevention method adopting the pre-coated film propping agent. The pre-coated film propping agent comprises propping agents, one or more pre-coated resins, one or more pre-coating curing agents, a coupling agent and a lubricating agent. The one or more pre-coated resins comprise bisphenol-A epoxy resin, bisphenol-F epoxy resin and/or novolac epoxy resin. The one or more pre-coating curing agents are selected from alicyclic polyamines, aromatic polyamines, modified alicyclic polyamines and/or modified aromatic polyamines. The coupling agent is an organosilane coupling agent.
Description
Technical field
The present invention relates to crude oil, Natural gas extraction sand control field, particularly a kind of pre-coated film propping agent, its preparation method and the anti-sand method that uses it.
Background technology
In the discharge opeing or oil recovery production process thereafter after the waterfrac treatment construction finishes, propping agent usually occurs and return Tuhe formation sand production phenomenon.The propping agent and the reservoir sand that take ground to can both corrode oil nozzle, valve and miscellaneous equipment; The row of returning and another potential hazard that shakes out are that supporting crack length and width reduce, and cause the flow conductivity of propping agent to descend.In order to prevent that propping agent from returning the Tuhe formation sand production; Curable resin overlay film propping agent has been made in researcher research, and curable resin overlay film propping agent is meant at matrix (like silica sand, haydite, glass sphere and nutshell etc.) goes up cold overlay film or hot overlay film one deck solid thermoset resin, and is injected in the formation fracture; Under the effect of reservoir stress, temperature and acvator; Resin on the aggregate is softening, and bonding each other and curing forms a filtering net; Or liquid thermosetting resin directly injected on the propping agent of formation fracture, resin solidification is with filtering net of the bonding one-tenth of propping agent.This filtering net can prevent that formation sand production, propping agent from returning the Tuhe and reducing the proppant embedment stratum.Mainly divide two big types by the resin kind of overlay film: one type is the coating phenolic resin propping agent, and another kind of is epoxy resin overlay film propping agent.
The external many bibliographical informations of chemical sand control condition of cure and the construction technology when adopting resol to make sticker.USP 4413931 has been studied the coating technique of resol, and the insoluble parameter of the resol that has proposed to use is greater than 1, and dipolymer ratio in ortho position is many more in the resin, help improving consolidation strength.USP 4336842 adds pure and mild tensio-active agent in the washing fluid when construction, improves consolidation strength through the softening temperature that reduces resol.USP 5218038 with of the fracturing fluid reaction and water-soluble, when synthetic resins, carries out modification with alkylphenol and aryl phenol to thermoplasticity and heat-reactive phenolic resin for fear of resol; To the silica sand overlay film time, carry out overlay film with the mixture of thermoset and novolac resin, do not use the hexamethylenetetramine solidifying agent; During overlay film, the level of response of resin is by overlay film time and temperature control; Confirmed the water miscible testing method of overlay film propping agent.USP 4597991 has been studied coating technique: the coupling agent that will add water is sprayed onto on the silica sand of heat, stirs 5～60 seconds; With hot blast heating silica sand to 120～176 ℃, remove in the silica sand moisture content with blow away the dust in the sand; Resol (account for silica sand weight 1～8%) with containing stearate adds in the silica sand, also can add polyvinyl butyral and improve resin toughness, stirs 30 seconds to 5 minutes; The aqueous solution hardening by cooling resin that adds hexamethylenetetramine (accounting for resin quality 13～17%); Add cooling liqs and blowing.
Domestic chemical sand control is main with resol, and resol has that raw material is easy to get, cheap, advantage such as acid resistance is strong.But there is the defective of two aspects in it: fragility is big on the one hand, and toughness is low, and when temperature was lower than 50 ℃, set time was long, fixed ultimate compression strength is low, need to add strong acid and could promote solidification rate and improve consolidation strength between sand grains, but strong acid is serious to tube corrosion; Resol has certain acidity owing to have a large amount of phenolic hydroxyl groups in the self structure on the other hand, makes its alkali resistance variation, and sand grains is difficult to fixed under the ternary composite driving condition.
CN1139730A relates to a kind of low temperature and is coated with the stuccoing technical recipe, is characterized in being applicable to sand control in reservoir temperature 40-100 ℃ the oil and water well, and easy construction, and the sand control expense is low.CN1168407A relates to a kind of high temperature resistant foamed resin preventing and fixing sand of oil well technical recipe that is used for; This kind sand prevention sand-fixing agent is a kind of black mucus; By modified phenolic resins, heat resistance accessory, the thinner alcohols dissolves each other; Ketone or lipid, coupling agent, whipping agent, curing agent component mix according to a certain percentage, and agitation and dilution is prepared from.CN116250C discloses oil-water well composite sand prevention material and preparation method thereof, comprises expansion-resisting agent in the oil recovery auxiliary agent, tensio-active agent, composite pore-forming and as the precoated sand of compaction material.Be mixed with spearhead and sand-carrying agent with expansion-resisting agent, tensio-active agent and clear water.Be mixed and made into liquid composite pore-forming with tensio-active agent, hydrochloric acid and methylolphenol.Be coated on the quartz sand surface of pickling with resin and additive, through oven dry, broken and form the precoated sand of single particle.To be that solidification value is minimum reach 40 ℃ to major advantage, is applicable to out oil, the well of the various degree of depth of carse, medium and small sand grains, and the construction success ratio is high, and validity period is long.
People such as Huang Qimao (oilfield chemistry, 2011,28 (1) 1～3) research epoxy resin sand control agent, resin demand accounts for 4% of sand weight, 60 ℃ of solidification values, consolidation strength is than higher, but resin demand is many, and solidification value is also than higher.People such as Li Huaiwen (oil drilling technology, 2011,39 (4) 99～102) use the epoxy resin sand control, make A material and B material, use inconvenience, and AB material difficulty mixes.
Above document uses the solid phenolic resin overlay film on propping agents such as silica sand or haydite and since the solidification value of resol than higher, set time long, fixed ultimate compression strength is low, resin demand is many, causes perviousness bad; Use epoxy resin overlay film propping agent, resin demand is many, and construction is inconvenient, and perviousness is bad.These disadvantages affect oil-gas field fracturings prevent formation sand production, prevent that propping agent from returning tells and prevents the proppant embedment stratum and influence perviousness.
Summary of the invention
The problem that invention will solve
The present invention is high in order to solve the curable propping agent solidification value that exists in the above-mentioned prior art, can not use when temperature is lower than 40 ℃; Set time is long, consolidation strength is low, and sand controlling result is poor; And resin demand is many, influences perviousness, develop a kind of can ambient cure, the high adhesive composition of consolidation strength and can make pre-coated film propping agent that resin coated propping agent realizes that intensity is high and preparation method thereof.
The scheme that is used to deal with problems
In order to realize the object of the invention, the invention provides a kind of pre-coated film propping agent, this pre-coated film propping agent comprises propping agent, pre-coated film resin, pre-coated film solidifying agent, coupling agent and lubricant; Said pre-coated film resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin and/or novolac epoxy; Said pre-coated film solidifying agent is alicyclic polyamine, modification alicyclic polyamine, aromatic polyamine and/or modified aromatic polyamine; Said coupling agent is an organo silane coupling agent.
Pre-coated film propping agent of the present invention; The content of wherein said pre-coated film resin is 0.1～1.5 quality % of said pre-coated film propping agent quality; The content of said pre-coated film solidifying agent is 10～40 quality % of said pre-coated film resin quality; The content of said coupling agent is 0.1～2 quality % of pre-coated film resin quality, and the content of said lubricant is 1～10 quality % of pre-coated film resin quality.
Pre-coated film propping agent of the present invention, wherein said propping agent is selected from natural siliceous sand and artificial porcelain granule.
Pre-coated film propping agent of the present invention, wherein said alicyclic polyamine are selected from one or more in isophorone diamine, amine ethyl piperazidine, two aminocyclohexane, diamino-dicyclohexyl methane, adjacent diamines methylcyclopentane and the Meng alkane diamines; Said aromatic polyamine is selected from one or more in m-xylene diamine, diaminodiphenyl-methane, the mphenylenediamine; Said modification alicyclic polyamine and said modified aromatic family polyamines product for reacting with at least a and the above-mentioned alicyclic polyamine and the above-mentioned aromatic polyamine that are selected from phenyl glycidyl ether, cresylglycidylether and the vinyl cyanide.
Pre-coated film propping agent of the present invention, wherein said lubricant is a stearate.
The present invention also provides a kind of preparation method of pre-coated film propping agent, and it comprises: with said propping agent heating, under agitation add said coupling agent and said pre-coated film resin, on said propping agent, form overlay film; Add said pre-coated film solidifying agent and stirring then; When material is about to conglomeration, add said lubricant, continue to stir and disperse fully until material.
Preparation in accordance with the present invention, the Heating temperature of wherein said propping agent are 180～250 ℃.
The present invention also provides a kind of sand-proof method for oil-gas well; Wherein the pre-coated film propping agent described in the claim 1-5 is mixed with epoxy resin and underwater curing agent; Inject the oil gas well through sand-carrying agent and carry out sand control, wherein said epoxy resin is liquid bisphenol A type epoxy resin and/or liquid bisphenol f type epoxy resin.
Sand-proof method for oil-gas well of the present invention, the mass ratio of wherein said epoxy resin and pre-coated film propping agent is 1～3: 100, the content of described underwater curing agent is 20～80 quality % of epoxy resin quality.
The effect of invention
According to pre-coated film propping agent provided by the invention; Can make the sand control system of processing by this pre-coated film propping agent have that the anti-breaking capacity of consolidation strength height, propping agent self improves, water conservancy diversion is good and the characteristic of realization ambient cure, and said sand control construction technology is simple, cost is low.
Embodiment
Pre-coated film propping agent provided by the invention comprises propping agent, pre-coated film resin, pre-coated film solidifying agent, coupling agent and lubricant; Said pre-coated film resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin and/or novolac epoxy, and said pre-coated film solidifying agent is alicyclic polyamine, modification alicyclic polyamine, aromatic polyamine and/or modified aromatic polyamine.
Said propping agent can be this area propping agent commonly used, as long as it meets set quota among the SY/T5108-2006 " fracturing propping agents performance test recommend method ".Propping agent among the present invention preferably uses natural siliceous sand and haydite.
The content of said pre-coated film resin is preferably 0.1～1.5 quality % of said propping agent quality, 0.3～1 quality % more preferably; Said pre-coated film resin is preferably bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy, for example can be selected to be purchased among the E-56 that can get, E-54, E-51, E-44, E-14, E-13, the E-10 one or more.
Said pre-coated film solidifying agent is alicyclic polyamine, modification alicyclic polyamine, aromatic polyamine and/or modified aromatic family polyamines.Wherein, said alicyclic polyamine is preferably selected from one or more in isophorone diamine, amine ethyl piperazidine, two aminocyclohexane, diamino-dicyclohexyl methane, adjacent diamines methylcyclopentane and the Meng alkane diamines.Said aromatic polyamine is preferably selected from one or more in m-xylene diamine, diaminodiphenyl-methane, the mphenylenediamine.Said modification alicyclic polyamine and modified aromatic family polyamines be preferably be selected from phenyl glycidyl ether, cresylglycidylether and the vinyl cyanide at least a respectively with the product of above-mentioned alicyclic polyamine and above-mentioned aromatic polyamine reaction, for example 1mol polyamines and 0.1～0.5mol's is selected from least a reaction product under 40～90 ℃ in phenyl glycidyl ether, cresylglycidylether and the vinyl cyanide.The consumption of said pre-coated film solidifying agent is preferably 10～40 quality % of pre-coated film resin quality.
Said coupling agent can be selected from various coupling agent well known by persons skilled in the art; In order to improve the bonding strength of pre-coated film resin and propping agent; Preferred said coupling agent is a silane coupling agent; The instance of silane coupling agent is preferably γ-An Bingjisanyiyangjiguiwan, N, two (the beta-hydroxyethyl)-gamma-amino propyl group trimethoxy silane of N-, anilino methylene triethoxyl silane, γ-glycidyl ether propyl trimethoxy silicane etc.The content of said coupling agent is preferably 0.1～2 quality % of pre-coated film resin quality, more preferably 0.5～1 quality %.
Said lubricant can be selected any various lubricants well known by persons skilled in the art for use; In order to be separated from each other between the propping agent that in solidification process, makes pre-coated film; Guarantee the integrity of propping agent overlay film; The preferred stearate that uses, for example calcium stearate, Zinic stearas and Magnesium Stearate etc., can be from Gaomi City new big auxiliary agent ltd buys.The content of said lubricant be preferably 1～10 quality % of pre-coated film resin, more preferably 2～5 quality %,
The preparation method of pre-coated film propping agent provided by the invention comprises: propping agent is heated to 180～250 ℃, under agitation adds coupling agent and pre-coated film resin, the time of stirring is preferably 60 ± 20 seconds, makes pre-coated film resin and coupling agent overlay film on propping agent; Add solidifying agent and stirring; When material is about to conglomeration, add lubricant, continue to stir and disperse fully until material; Material is cooled to envrionment temperature.
Epoxy resin binder provided by the invention, described epoxy resin are liquid bisphenol A type epoxy resin or bisphenol f type epoxy resin, and for example bisphenol A type epoxy resin can be selected from and be purchased E-56, E-54, E-51, the E-44 that can get; Bisphenol f type epoxy resin can be selected from the trade mark 6458 resins that are purchased the Xinhua Resin Factory, Shanghai that can get, the trade mark CYDF-170 and the CYDF-180 resin of epoxy resin factory of Yueyang general petrochemicals factory.Consumption accounts for 1～4% of propping agent quality.Described solidifying agent is the underwater curing agent that can buy on the market; 810 type solidifying agent like the Changsha chemical institute; The JA-1S type solidifying agent of Sichuan Province's Pujiang Fine Chemical Works, biochemical technology ltd solidifying agent 1085 etc. is illuminated in Changsha, and consumption accounts for 20～80% of epoxy resin quality.
Oil gas well sand control site construction technology of the present invention is for selecting for use continuous resin sand mulling (like Qingdao Tianheng Machinery Co., Ltd.; Strand, Qingdao gold becomes foundry machinery ltd; Hangzhou Taiyang Casting Engineering Tech. Co., Ltd. etc.); At first liquid resin and underwater curing agent are covered silica sand or haydite surface at pre-coated film, then silica sand or the haydite with overlay film carries out sand control through sand-carrying agent injection oil gas well.
Adopt the mode of embodiment that the present invention is explained in further detail below.
Embodiment 1
1, the preparation of pre-coated film silica sand
(particle diameter 0.425～0.85mm) is poured in the sand mill after being heated to 210 ℃, and (trade mark: E-51) 50 grams and γ-glycidyl ether propyl trimethoxy silicane 1 gram stirred 40 seconds to add bisphenol A epoxide resin with 10 kilograms natural siliceous sands; Add diaminodiphenyl-methane solidifying agent 15 grams and stir, the calcium stearate that when material begins conglomeration, adds 2 grams stirs and solidified 200 seconds, cools off, sieves, and can obtain pre-coated film silica sand.
2, oil gas well sand control capability test
Get above-mentioned pre-coated film silica sand 250 grams, E-51 bisphenol A epoxide resin 5 grams of laminated quartz sand weight 2% and JA-1S type solidifying agent 2 grams of this weight resin 40% are mixed in the pre-coated film silica sand of back adding, stir.Take by weighing this sand 50 grams, put into diameter and be 25 millimeters, an end and seal and manage the steel pipe that scribbles releasing agent with plug, add 30 gram water; This pipe was put into 30 ℃ of water bath with thermostatic control constant temperature 10 minutes; Take out the back and load 4,000 Ns power 20 seconds at WHY-300 type microcomputer control full-automatic pressure trier, the water bath with thermostatic control insulation that continues to put into 30 ℃ was taken out from steel pipe after 24 hours; Surveying its fixed ultimate compression strength is 7.1MPa, 40MPa rate of permeation 120.5 μ m
2
Comparative example 1
Get silica sand 250 gram of the not overlay film of above-mentioned same particle diameter, the JA-1S type solidifying agent 2.5 of E-51 bisphenol A epoxide resin 6.25 grams of the silica sand weight 2.5% of overlay film not and weight resin 40% is restrained in the silica sand that adds overlay film not after mixing, stir.Surveying its fixed ultimate compression strength by embodiment 1 sample preparation is 3.0MPa, rate of permeation 65.8 μ m
2
Comparative example 2
(particle diameter 0.425～0.85mm) is poured in the sand mill after being heated to 150 ℃ with 10 kilograms natural siliceous sands; The resol (trade mark: 1901, Shandong Shengquan Chemical Industry Co., Ltd.) that adds silica sand weight 4% stirred 30 seconds with γ-An Bingjisanyiyangjiguiwan 4 grams for 0.4 kilogram; The aqueous solution 180 grams (hexamethylenetetramine is 1: 2 with the mass ratio of water) that add hexamethylenetetramine when adding water for cooling to 110 ℃; The calcium stearate that when material begins conglomeration, adds 20 grams is stirred to conglomeration to be disperseed, cool off, sieves, and can obtain universal sand control laminated quartz sand propping agent.
Take by weighing this sand 50 grams, press embodiment 1 sample preparation, 30 ℃ of insulations were surveyed its fixed ultimate compression strength in 72 hours and are had only 0.2MPa, rate of permeation 42.7 μ m
2
Embodiment 2
1, the preparation of pre-coated film haydite
(particle diameter 0.425～0.85mm) is poured in the sand mill after being heated to 230 ℃, and (trade mark: E-54) 100 grams and γ-glycidyl ether propyl trimethoxy silicane 1 gram stirred 50 seconds to add bisphenol A epoxide resin with 10 kilograms haydites; Add diaminodiphenyl-methane solidifying agent 30 grams and stir, the calcium stearate that when material begins conglomeration, adds 5 grams stirs and solidified 220 seconds, cools off, sieves, and can obtain pre-coated film haydite.
2, oil gas well sand control capability test
Get above-mentioned pre-coated film haydite 250 grams, E-51 bisphenol A epoxide resin 5 grams of film-coated ceramisite weight 2% and 810 type solidifying agent, 2 grams of weight resin 40% are mixed in the pre-coated film haydite of back adding, stir.Press embodiment 1 sample preparation, 25 ℃ of water bath heat preservations 24 hours, surveying its fixed ultimate compression strength was 9.5MPa, 60MPa rate of permeation 145.6 μ m
2
Comparative example 3
Get haydite 250 gram of the not overlay film of above-mentioned same particle diameter, 810 type solidifying agent 3.0 of E-51 bisphenol A epoxide resin 7.5 grams of the haydite weight 3.0% of overlay film not and weight resin 40% are restrained in the haydite that adds overlay film not after mixing, stir.Press embodiment 1 sample preparation, 25 ℃ of water bath heat preservations 24 hours, surveying its fixed ultimate compression strength was 4.5MPa, 60MPa rate of permeation 102.7 μ m
2
Embodiment 3
25 ℃ of consolidation times are confirmed
Table 1 set time is to the influence of fixed ultimate compression strength
| Time, h | 4 | 8 | 12 | 24 |
| Fixed ultimate compression strength, MPa | 3.5 | 7.2 | 9.8 | 11.9 |
Get the foregoing description 2 pre-coated film haydites, the E-51 bisphenol A epoxide resin of film-coated ceramisite weight 3% and 810 type solidifying agent of weight resin 40% are mixed in the pre-coated film haydite of back adding, stir.Press embodiment 1 sample preparation, survey its fixed ultimate compression strength (seeing table 1) at different time.From table 1,25 ℃ of heat preservation solidification 24 hours, ultimate compression strength has arrived peak.
Claims (9)
1. pre-coated film propping agent, it comprises propping agent, pre-coated film resin, pre-coated film solidifying agent, coupling agent and lubricant; Said pre-coated film resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin and/or novolac epoxy; Said pre-coated film solidifying agent is alicyclic polyamine, modification alicyclic polyamine, aromatic polyamine and/or modified aromatic polyamine; Said coupling agent is an organo silane coupling agent.
2. pre-coated film propping agent according to claim 1; The content of wherein said pre-coated film resin is 0.1～1.5 quality % of said pre-coated film propping agent quality; The content of said pre-coated film solidifying agent is 10～40 quality % of said pre-coated film resin quality; The content of said coupling agent is 0.1～2 quality % of pre-coated film resin quality, and the content of said lubricant is 1～10 quality % of pre-coated film resin quality.
3. pre-coated film propping agent according to claim 1 and 2, wherein said propping agent is selected from natural siliceous sand and haydite.
4. pre-coated film propping agent according to claim 1 and 2, wherein said alicyclic polyamine are selected from one or more in isophorone diamine, amine ethyl piperazidine, two aminocyclohexane, diamino-dicyclohexyl methane, adjacent diamines methylcyclopentane and the Meng alkane diamines; Said aromatic polyamine is selected from one or more in m-xylene diamine, diaminodiphenyl-methane, the mphenylenediamine; Said modification alicyclic polyamine and said modified aromatic family polyamines product for reacting with at least a and the above-mentioned alicyclic polyamine and the above-mentioned aromatic polyamine that are selected from phenyl glycidyl ether, cresylglycidylether and the vinyl cyanide.
5. pre-coated film propping agent according to claim 1 and 2, wherein said lubricant is a stearate.
6. the preparation method of pre-coated film propping agent described in the claim 1-5, it comprises: with said propping agent heating, under agitation add said coupling agent and said pre-coated film resin, on said propping agent, form overlay film; Add said pre-coated film solidifying agent and stirring then; When material is about to conglomeration, add said lubricant, continue to stir and disperse fully until material.
7. preparation method according to claim 6, the Heating temperature of wherein said propping agent are 180～250 ℃.
8. sand-proof method for oil-gas well; Wherein the pre-coated film propping agent described in the claim 1-5 is mixed with epoxy resin and underwater curing agent; Inject the oil gas well through sand-carrying agent and carry out sand control, wherein said epoxy resin is liquid bisphenol A type epoxy resin and/or liquid bisphenol f type epoxy resin.
9. sand-proof method for oil-gas well according to claim 8, the mass ratio of wherein said epoxy resin and pre-coated film propping agent is 1～3: 100, the content of described underwater curing agent is 20～80 quality % of epoxy resin quality.
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Application publication date: 20120912 Assignee: BEIJING QISINTAL NEW MATERIAL CO., LTD. Assignor: Beijing qixiangda science and technology limited company|Yangquan Changqing oil fracturing proppant Co. Ltd. Contract record no.: 2015990000089 Denomination of invention: Pre-coated film propping agent, preparation method of the pre-coated film propping agent and sand prevention method adopting the pre-coated film propping agent Granted publication date: 20140514 License type: Exclusive License Record date: 20150304 |
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