CN108467719A - A kind of preparation with sterilization and the water filling clay expansion-resisting agent of anti-scaling action - Google Patents
A kind of preparation with sterilization and the water filling clay expansion-resisting agent of anti-scaling action Download PDFInfo
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- CN108467719A CN108467719A CN201810398177.XA CN201810398177A CN108467719A CN 108467719 A CN108467719 A CN 108467719A CN 201810398177 A CN201810398177 A CN 201810398177A CN 108467719 A CN108467719 A CN 108467719A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/584—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific surfactants
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating
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Abstract
The present invention provides a kind of preparation of the water filling clay expansion-resisting agent with sterilization and anti-scaling action, disclosing the cationic surfactant independently synthesized has the migration for preferably preventing clay swelling, clay particle, and has outstanding erosion resistibility and good sterilizing ability；The phosphino- maleic acrylic copolymer scale preventative independently synthesized, the ability for the anti-calcium scale having had slow down the blocking of dirt；The clay expansion-resisting agent with sterilization and anti-scaling action is obtained after being compounded with urea, dodecyl benzyl dimethyl ammonium chloride, ammonium chloride and potassium chloride.The clay expansion-resisting agent for water injection work that the present invention is developed, with good inhibition clay hydration swelling and erosion resistibility, the ability of excellent anti-calcium sulfate and calcium carbonate scale, effectively sulfate reducing bacteria, saprophytic bacteria and iron bacteria can be sterilized, and the of low cost, agent is the exemplary role that innovation has been made in the one multi-functional water filling of exploitation with clay expansion-resisting agent, is had broad application prospects.
Description
Technical field
When the present invention relates to suitable for oil-field flooding operation it is a kind of there is sterilization and anti-scaling action prevent clay swelling
The preparation of clay expansion-resisting agent.
Background technology
With the continuous development of China's water flooding technology, water drive is applied to production development by more and more oil fields
In, waterflooding extraction has become the development scheme in most of oil fields.But with the continuous progress of water flooding, due to external
Fluid and the incompatibility of reservoir rock mineral and the incompatibility of outside fluid and reservoir fluid often cause the stifled of stratum
Plug, makes reservoir permeability reduce, water injection pressure constantly increases, especially for low permeability reservoir, it is easier to be damaged, cause
Injection pressure rapid increase shorts the problems such as being on the rise, to reduce the production capacity and rate of oil production in oil field.
Injection water is damaged caused by being incompatible with reservoir and is mainly shown as：Sensibility is damaged；The intrusion of solid phase particles with it is stifled
Plug；Water blocking damage etc. caused by chemisorption and wettability modification.Damage caused by injection water is incompatible with reservoir fluid is main
It shows as：Formation damage caused by inorganic scale；Formation damage caused by organic deposition；Emulsion plugging；Damage caused by microorganism
With the influence of free gas etc..
In order to prevent and overcome these injuries, protects reservoir, it is solid to reduce in addition to strictly controlling injection water suspension content
The intrusion of phase particle is outer with blocking, and various inorganic agents are usually added in Water Injection Engineering.
Injection water is contacted with the clay mineral in stratum, leads to clay mineral hydration swelling, dispersion and migration, to block
The throat of formation void structure, causes in-place permeability to reduce, and generates damage, this injury is the most serious, prevents using clay swollen
Agent is to solve the problems, such as this unique method.
The bacteriums such as a certain amount of sulfate reducing bacteria (SRB), saprophytic bacteria (TGB) and the iron bacteria (FB) contained in injection water,
They grow and breed in ground installation, waterflood-transmission line, oil pipe, underground injection device and reservoir, and sulfate reducing bacteria can be with
Sulfate ion in water is reduced into sulfidion, while also producing by-product H2S.Therefore, cause than other bacteriums
More serious corrosion.The activity of sulfate reducing bacteria will produce sticky substance, and result in blockage, this is also that reservoir is caused to be hindered
The reason that evil, water injection pressure rise, must be added fungicide in water filling thus.
Injection water is mixed with water flooding, if be incompatible, scale formation can occur.Domestic onshore oil field injects water simultaneously
It is all made of re-injection after sewage disposal, these re-injection water salinities are high, the chemically and thermally mechanical balance state hair of mineral aqueous solution
When life changes and becomes supersaturation, inorganic scale is then therefrom precipitated out.Inorganic scaling can be happened in oil pipe, may also occur at
In stratum near injection-production well eye, the common dirt in oil field mainly has calcium carbonate scale and calcium sulfate scale.These dirt precipitations block water filling
Channel causes water injection pressure to rise, and to solve the problems, such as this, just needs that scale preventative is added in water filling.
It is injured caused by injury and fouling caused by order to reduce clay mineral hydration swelling, bacterium, it is most effective at present
Method is to be continuously added to clay expansion-resisting agent, fungicide and scale preventative in injecting water.
Water filling clay expansion-resisting agent used at present only there is single clay to prevent swollen performance, if it is possible to make this glutinous
Native expansion-resisting agent is not only able to prevent clay swelling, can also solve bacterium and scale problems, and imparting clay expansion-resisting agent is also had and is killed
The function of bacterium and antiscale plays the role of one multiple-effect, and the process of sterilization and antiscale can be reduced in water injection work, reduces medicament
Usage amount reduces cost.
Clay expansion-resisting agent can be divided into inorganic salts, inorganic polymeric species, cationic surface according to the difference of chemical composition
Activating agent class and organic cation small molecular weight polymer class.Electrodeless salt and inorganic polymeric species are cheap, have well
Prevent the ability of clay swelling.Organic cationic surfactant and organic cationic polymer be on strand with tertiary amine or
The molecule of quaternary ammonium positive charge group, there are very strong active forces between clay mineral for it, can effectively prevent clay mineral
Hydration swelling and dispersion are migrated, and have long-term effect.
The difference of fungicide according to chemical composition is divided into inorganic fungicide and organic bactericide two major classes.Inorganic fungicide includes
Chlorine, chlorine dioxide and sodium hypochlorite etc..Organic bactericide includes quaternary ammonium salt, chlorophenols and organic sulfur class and chloramines class etc..It presses
The bactericidal mechanism of fungicide is divided into oxidized form and non-oxidative bactericide.Such as chlorine, sodium hypochlorite and chloramines etc. are that oxidized form kills
Microbial inoculum；Quaternary ammonium salt, chlorophenols and dithiocyano-methane etc. are non-oxidative bactericides.
The difference of the common chemical scale inhibition agent in oil field according to chemical composition is divided into inorganic phosphate salt, organic phospho acid and its salt
Class, polymerization species etc..Inorganic phosphate mainly has tertiary sodium phosphate, tetrasodium pyrophosphate, sodium tripolyphosphate and calgon.It is organic
Phosphonic acids and its esters mainly have aminotrimethylenephosphonic acid（ATMP）, ethylene diamine tetra methylene phosphonic acid（EDTMPA）, 1-hydroxy ethylene-1,1-diphosphonic
Sour sodium（HEDP）Deng.Polymer mainly has Sodium Polyacrylate（PAAS）, poly amic acid（PMA）, poly-maleic anhydride
（HPMA）Deng.
The clay expansion-resisting agent that the present invention develops not only prevents the expansion of clay, migration, also can be to sulfate reducing bacteria
(SRB), saprophytic bacteria (TGB) and iron bacteria (FB) are effectively sterilized, it is therefore prevented that the waterflood path caused by the breeding of bacterium
It blocks；It can also prevent calcium sulfate and calcium carbonate scale from being formed, reduce fouling and form caused blocking, protect reservoir well, reach
To the effect of one multiple-effect.The present invention has following innovative point：
1. the clay expansion-resisting agent has the triple effects for preventing clay swelling, sterilization and antiscale；
2. cationic surfactant has the ability for preventing clay swelling well, while also having the fortune for preventing clay particle
The ability of shifting has outstanding erosion resistibility, has long-term effect；
3. cationic surfactant is in addition to clay swelling effect is prevented, also certain bactericidal effect, with dodecyl
Dimethyl benzyl ammonium chloride is used in mixed way, and bactericidal effect is more preferable；
4. the phosphino-maleic acid-acrylate copolymer scale preventative of synthesis, it has extraordinary anti-calcium scale（Calcium sulfate, calcium carbonate）
Ability, reduce the dirt that injection water and water flooding are formed due to being incompatible, slow down the blocking of dirt, eliminate and be individually added into antiscale
The operation of agent；
It is individually added into fungicide operation in oil-field flooding 5. eliminating, reduces construction intensity, saved fungicide medicament；
6. playing the role of one multiple-effect.
Invention content
It is an object of the invention to：The clay expansion-resisting agent provided, can play prevents clay swelling, migrates, prevents calcium scale
(calcium sulfate, calcium carbonate) fouling, sterilization comprehensive function, play the role of one multiple-effect, reduce injury of the water filling to reservoir
Comprehensive production effect, in Oil-production Enterprises water filling it is energy saving, lower consumption, reduce cost strong science and technology support is provided.
The object of the present invention is achieved like this：A kind of preparation with sterilization and the clay expansion-resisting agent of anti-scaling action.
Raw material is by A：Cationic surfactant, B：Phosphino-maleic acid-acrylate copolymer scale preventative, C：Urea, D：Ten
Dialkyl dimethyl benzyl ammonium chloride, E：Ammonium chloride and F：Potassium chloride forms, and is obtained after mixing with sterilization and anti-scaling action
Clay expansion-resisting agent G.
The wherein synthesis of A cationic surfactants：
1）The trimethylamine 179.1kg of 33wt% mass concentrations is added into the reaction kettle equipped with condensing unit, is warming up to 20-30 DEG C,
It is stirred under 1000 revs/min, for use；
2）The benzyl chloride that 126.6kg contents are 99% or more is added in Agitation Tank, is then added drop-wise to 1）It is loaded with the reaction of trimethylamine
In kettle, time 10-15min is added dropwise；Stirring is warming up to 50-60 DEG C under 1000 revs/min, reacts 30-60min, obtains anti-
Answer object；
3) by 2）Reactant in reaction kettle stirs under 1000 revs/min, closes condensing unit, is warming up to 95-120 DEG C, waits anti-
Answering in object has that a large amount of crystal generate and when liquid retrogradation multiplies heat and releases liquid and then cooling, it is cooling after by product be put into it is long ×
In wide × a height of cm × 6 of 50cm × 30 cm stainless steel discs, it is then placed in baking oven.6h is dried at 90 DEG C, and Xinxiang is used after cooling
The MGD350 bulk material machines of auspicious rich bulk material equipment Co., Ltd of city production be ground into can cross the powder of 40 mesh screens to get to
Solid cationic surfactant A.
Wherein B phosphino-maleic acid-acrylate copolymers scale preventative synthesizes：
1）4kg ammonium persulfates are dissolved in 20kg deionized waters or distilled water water, in room temperature, 1000 revs/min of lower stirring and dissolvings,
Obtain initiator；
2）70kg deionized waters or distilled water are added into reaction kettle, 9kg maleic anhydrides are then added, 1000 turns/
Stirring under point.After maleic anhydride is completely dissolved, the sodium phosphite of 10kg is added, is stirred under 1000 revs/min, the time
10-15min rises temperature to 50-55 DEG C.It waits for that sodium hypophosphite is completely dissolved, is warming up to 75-80 DEG C, stirred at 1000 revs/min
Under, respectively with 2 feed pots, while 27.0kg acrylic acid and 1 is added dropwise）Initiator, time 50-60min, control acrylic acid and
Initiator adds simultaneously, is warming up to 85-95 DEG C, the reaction was continued 2-3h, obtains faint yellow viscous solution, it is calculated with the amount of monomer
Effective concentration is 33.8wt%；
3）By 2）In the faint yellow viscous solution that is prepared to be put into length × width × height be the cm stainless steel discs of cm × 6 of 50cm × 30
In, it is then placed in baking oven, is dried at 90 DEG C for 24 hours, is used after cooling with the auspicious rich bulk material equipment Co., Ltd production in Xinxiang City
MGD350 bulk material machines are ground into the solid anti-scaling agent B that can cross the powder of 40 mesh screens to get nitrogen yellow.
Homemade raw material A and B are mixed with C, D, E and F phase, are uniformly mixed the G for being made described.
The mechanism of the present invention and effect：The cationic surfactant that the present invention synthesizes have prevent clay particle well
Expansion and migration, there is outstanding erosion resistibility, have long-term effect.Simultaneously because organoammonium cations, have certain kill
The ability for having well and preventing clay particle hydration swelling is used in combination with urea, with dodecyl dimethyl benzyl in bacterium property
Ammonium chloride is used in mixed way, and bactericidal effect is more preferable.
Sulphur in water filling can be effectively prevented after being mixed with the phosphino-maleic acid-acrylate copolymer scale preventative that the present invention synthesizes
The formation of sour calcium, calcium carbonate scale.The dirt to be formed that is incompatible for reducing injection water and water flooding slows down the blocking of fouling formation.
The technical scheme is that clay expansion-resisting agent and preparation method with sterilization and anti-scaling action, feature exist
In：Present invention self-control is compounded using raw material A, B and with C, D, E and F, and G, which is made, has the clay expansion-resisting agent of sterilization and anti-scaling action,
Each material quality ratio is：A:B:C:D:E:F=15%~25%:1%~5%:20%~30%:0%~15%:15%~25%:15%~25%.At this
Under mass ratio, A, B, C, D, E and F are uniformly mixed, G, which is made, has the clay expansion-resisting agent of sterilization and anti-scaling action, to make this
Invention clay expansion-resisting agent has the triple effects for preventing clay swelling, sterilization and antiscale, plays the role of one multiple-effect；Wherein G
Under each mass ratio, be dissolved separately in tap water, be made into mass concentration be respectively 0.3wt%, 0.5wt%, 0.8wt% and
The solution of 1.0wt% under room temperature (25 DEG C), compares at 0.3wt% with tap water, centrifugal process measures clay anti-dilative and is more than or equal to
81.1%, anti-rate of washing is more than or equal to 81.5%, and anti-calcium sulfate scale antiscaling rate is more than or equal to 97.2%, and anti-calcium carbonate scale antiscaling rate is more than
Equal to 73.2%；Clay anti-dilative is more than or equal to 86.5% at 0.5wt%, and anti-rate of washing is more than or equal to 84.7%, and anti-calcium sulfate scale is anti-
Dirty rate is more than or equal to 98.0%, and anti-calcium carbonate scale antiscaling rate is more than or equal to 75.4%；Clay anti-dilative is more than or equal at 0.8wt%
91.0%, anti-rate of washing is more than or equal to 87.6%, and anti-calcium sulfate scale antiscaling rate is more than or equal to 98.6%, and anti-calcium carbonate scale antiscaling rate is more than
Equal to 78.3%；Clay anti-dilative is more than or equal to 94.2% at 1.0wt%, and anti-rate of washing is more than or equal to 91.7%, and anti-calcium sulfate scale is anti-
Dirty rate is more than or equal to 99%, and anti-calcium carbonate scale antiscaling rate is more than or equal to 79.7%；With sulfate reducing bacteria (SRB) number be 6 ×
102A/ml, saprophytic bacteria (TGB) number are 6 × 103A/ml and iron bacteria (FB) number are 2.5 × 102The Xinjiang Oil Regions of a/ml
21 wellblock Sewage Disposal of field branch company Luliang Oil Field, junggar Basin operation area heath treated reinjected water is according to " SY/T 5329-2012 are broken
Consider shale oil to be worth doing and hide injection water quality index and analysis method " evaluation.In G dosages 0.3wt% or more, iron bacteria (FB) number is small
In equal to 40/mL, in G dosages 0.5wt% or more, sulfate reducing bacteria (SRB) number, which is respectively less than, is equal to 9.5/mL,
Saprophytic bacteria (TGB) number, which is respectively less than, is equal to 95/mL, reaches the index request in the standard.Wherein mass ratio：A:B:C:D:E:
F=20%:4%:26%:15%:15%:20% G, in concentration 0.5wt% or more, clay anti-dilative is all higher than equal to 90.4%, is resisted
The rate of washing is all higher than equal to 90.2%, and anti-calcium sulfate scale antiscaling rate is more than or equal to 99.4%, and anti-calcium carbonate scale antiscaling rate, which is all higher than, to be equal to
82.1%, sulfate reducing bacteria (SRB) number, which is respectively less than, after sterilization is equal to 4/mL, and saprophytic bacteria (TGB) number, which is respectively less than, to be equal to
65/mL, iron bacteria (FB) number, which is respectively less than, is equal to 7.5/mL, reaches the index request in standard.
The clay expansion-resisting agent developed of the present invention has the ability of good inhibition clay hydration swelling and with preventing clay
The ability of particle migration has outstanding erosion resistibility；It is good with the compounding effects such as inorganic salts and urea, not only increase system
Anti-dilative also reduce the dosage of cationic surfactant clay expansion-resisting agent especially with cheap urea；Than
Existing frequently-used clay expansion-resisting agent is cheap, stablizes the long-term effect of clay with washing method evaluation clay expansion-resisting agent, has excellent performance, together
When with excellent bactericidal property and anti-scaling property so that clay expansion-resisting agent removes, and there is excellent clay to prevent swollen, particle migration, anti-
Outside performance of flushing, performance, good bactericidal property also with outstanding anti-calcium sulfate scale and calcium carbonate scale make clay expansion-resisting agent
Impart three kinds of functions.
The agent is clay swelling, reduction pharmaceutical use and process, reduction water drive cost, the one multiple-effect prevented in water filling
Innovative demonstration effect has been made, has shown technological progress.
Specific implementation method：
Embodiment 1：A, B raw material will be made by oneself, the clay expansion-resisting agent G with sterilization and anti-scaling action is made with C, D, E and F compounding,
In each material quality ratio be：A:B:C:D:E:F=15%:1%:30%:15%:20%:19%.
G is dissolved separately in tap water, it is respectively 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% to be made into mass concentration
Solution, under room temperature (25 DEG C), anti-dilative under various concentration anti-wash rate, anti-scaling property and bactericidal property and is：
1）Concentration is respectively that the anti-dilative of 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% are：81.1%, 86.5%, 91% and
94.2%, the anti-rate of washing is：83.4%, 86.3%, 89.5% and 91.7%；
2）Concentration is respectively that 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% are to the antiscaling rate of calcium sulfate：97.2%、98%、
98.6% and 99%, the antiscaling rate to calcium carbonate is：73.2%, 75.4%, 78.3% and 79.7%；
3）Concentration is respectively 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt%, and sulfate reducing bacteria (SRB) number is after sterilization：
7.5/mL, 6/mL, 0/mL and 0/mL, saprophytic bacteria (TGB) number is：95/mL, 70/mL, 45/mL and 20
A/mL, iron bacteria (FB) number are：20/mL, 9.5/mL, 4.5/mL and 0/mL.
Compare centrifugal process with tap water in concentration 0.3wt% and measure clay anti-dilative 81.1%, resists and wash rate 83.4%, prevent
Calcium sulfate scale antiscaling rate 97.2%, anti-calcium carbonate scale antiscaling rate 73.2%, sulfate reducing bacteria (SRB) is 7.5/mL after sterilization,
Saprophytic bacteria (TGB) number is：95/mL, iron bacteria (FB) number is：20/mL, reach the index request in standard.
In concentration 0.8wt% or more, clay anti-dilative is all higher than equal to 91.0%, and the anti-rate of washing is all higher than equal to 89.5%,
Anti- calcium sulfate scale antiscaling rate is all higher than equal to 98.6%, and anti-calcium carbonate scale antiscaling rate is all higher than equal to 78.3%, and not only clay is prevented swollen
Rate and it is anti-wash that rate is good, and anti-calcium sulfate scale and calcium carbonate scale performance are also excellent, to sulfate reducing bacteria (SRB), saprophytic bacteria (TGB) and
The bactericidal property of iron bacteria (FB) also reaches the index request in standard.
Embodiment 2：A, B raw material will be made by oneself, the clay expansion-resisting agent with sterilization and anti-scaling action is made with C, D, E and F compounding
G, wherein each material quality ratio is：A:B:C:D:E:F=20%:2%:25%:10%:20%:23%.
G is dissolved separately in tap water, it is respectively 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% to be made into mass concentration
Solution, under room temperature (25 DEG C), anti-dilative under various concentration anti-wash rate, anti-scaling property and bactericidal property and is：
1）Concentration is respectively that the anti-dilative of 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% are：83.7%, 87.2%, 91.1% and
94.4%, the anti-rate of washing is：84.2%, 86.6%, 90.1% and 92.5%；
2）Concentration is respectively that 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% are to the antiscaling rate of calcium sulfate：98.1%、99%、
99.3% and 99.4%, the antiscaling rate to calcium carbonate is：76.7%, 79.6%, 80.5% and 81.3%；
3）Concentration is respectively 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt%, and sulfate reducing bacteria (SRB) number is after sterilization：
7.5/mL, 6.5/mL, 1.5/mL and 0/mL, saprophytic bacteria (TGB) number is：95/mL, 75/mL, 65/mL
With 45/mL, iron bacteria (FB) number is：25/mL, 11.5/mL, 7.5/mL and 4/mL.
Compare centrifugal process with tap water in concentration 0.3wt% and measure clay anti-dilative 83.7%, resists and wash rate 84.2%, prevent
Calcium sulfate scale antiscaling rate 98.1%, anti-calcium carbonate scale antiscaling rate 76.7%, after sterilization sulfate reducing bacteria (SRB) number be 7.5/
ML, saprophytic bacteria (TGB) number are：95/mL, iron bacteria (FB) number is：25/mL, reach the index request in standard.
In concentration 0.8wt% or more, clay anti-dilative is all higher than equal to 91.1%, and the anti-rate of washing is all higher than equal to 90.1%,
Anti- calcium sulfate scale antiscaling rate is all higher than equal to 99.3%, and anti-calcium carbonate scale antiscaling rate is all higher than equal to 80.5%, and not only clay is prevented swollen
Rate and it is anti-wash that rate is good, and anti-calcium sulfate scale and calcium carbonate scale performance are also excellent, to sulfate reducing bacteria (SRB), saprophytic bacteria (TGB) and
The bactericidal property of iron bacteria (FB) also reaches the index request in standard.
Embodiment 3：A, B raw material will be made by oneself, the clay expansion-resisting agent with sterilization and anti-scaling action is made with C, D, E and F compounding
G, wherein each material quality ratio is：A:B:C:D:E:F=20%:4%:26%:15%:15%:20%.
G is dissolved separately in tap water, it is respectively 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% to be made into mass concentration
Solution, under room temperature (25 DEG C), anti-dilative under various concentration anti-wash rate, anti-scaling property and bactericidal property and is：
1）Concentration is respectively that the anti-dilative of 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% are：86.6%, 90.4%, 92.1% and
95.7%, the anti-rate of washing is：85.3%, 90.2%, 91.3% and 93.8%；
2）Concentration is respectively that 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% are to the antiscaling rate of calcium sulfate：99.2%、99.4%、
99.9% and 99.9%, the antiscaling rate to calcium carbonate is：80.6%, 82.1%, 83.9% and 84.8%；
3）Concentration is respectively 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt%, and sulfate reducing bacteria (SRB) number is after sterilization：6
A/mL, 4/mL, 0/mL and 0/mL, saprophytic bacteria (TGB) number is：95/mL, 65/mL, 45/mL and 15/
ML, iron bacteria (FB) number are：15/mL, 7.5/mL, 0/mL and 0/mL.
Compare centrifugal process with tap water in concentration 0.3wt% and measure clay anti-dilative 86.6%, resists and wash rate 85.3%, prevent
Calcium sulfate scale antiscaling rate 99.2%, anti-calcium carbonate scale antiscaling rate 80.6%, after sterilization sulfate reducing bacteria (SRB) number be 6/
ML, saprophytic bacteria (TGB) number are：95/mL, iron bacteria (FB) number is：15/mL, reach the index request in standard.
In concentration 0.5wt% or more, clay anti-dilative is all higher than equal to 90.4%, and the anti-rate of washing is all higher than equal to 90.2%,
Anti- calcium sulfate scale antiscaling rate is all higher than equal to 99.4%, and anti-calcium carbonate scale antiscaling rate is all higher than equal to 82.1%, and not only clay is prevented swollen
Rate and the anti-rate of washing are had excellent performance, and anti-calcium sulfate scale and calcium carbonate scale performance are also excellent, to sulfate reducing bacteria (SRB), saprophytic bacteria
(TGB) and the bactericidal property of iron bacteria (FB) reaches the index request in standard.
The G best performances of the quality proportioning.
Embodiment 4：A, B raw material will be made by oneself, the clay expansion-resisting agent with sterilization and anti-scaling action is made with C, D, E and F compounding
G, wherein each material quality ratio is：A:B:C:D:E:F=25%:3%:20%:5%:22%:25%.
G is dissolved separately in tap water, it is respectively 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% to be made into mass concentration
Solution, under room temperature (25 DEG C), anti-dilative under various concentration anti-wash rate, antiscale property and bactericidal property and is：
1）Concentration is respectively that the anti-dilative of 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% are：84.2%, 88.3%, 91.6% and
94.7%, the anti-rate of washing is：84.8%, 87.4%, 90.5% and 93.1%；
2）Concentration is respectively that 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% are to the antiscaling rate of calcium sulfate：98.8%、99.3%、
99.5% and 99.7%, the antiscaling rate to calcium carbonate is：78.9%, 79.8%, 82.3% and 83.7%；
3）Concentration is respectively 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt%, and sulfate reducing bacteria (SRB) number is after sterilization：
9.5/mL, 7/mL, 2/mL and 0/mL, saprophytic bacteria (TGB) number is：160/mL, 95/mL, 70/mL and 65
A/mL, iron bacteria (FB) number are：30/mL, 15/mL, 11.5/mL and 6.5/mL.
Compare centrifugal process with tap water in concentration 0.3wt% and measure clay anti-dilative 84.2%, resists and wash rate 84.8%, prevent
Calcium sulfate scale antiscaling rate 98.8%, anti-calcium carbonate scale antiscaling rate 78.9%, after sterilization sulfate reducing bacteria (SRB) number be 9.5/
ML, iron bacteria (FB) number are 30/mL, reach the index request in standard.
In concentration 0.5wt% or more, clay anti-dilative is all higher than equal to 88.3%, and the anti-rate of washing is all higher than equal to 87.4%,
Anti- calcium sulfate scale antiscaling rate is all higher than equal to 99.3%, and anti-calcium carbonate scale antiscaling rate is all higher than equal to 79.8%, saprophytic bacteria after sterilization
(TGB) number is less than or equal to 95/mL, reaches the index request in standard.
In concentration 0.8wt% or more, anti-dilative is more than or equal to 91.6%, and anti-rate of washing is more than or equal to 90.5%, anti-calcium sulfate
Dirty antiscaling rate is all higher than equal to 99.6%, and anti-calcium carbonate scale antiscaling rate is all higher than equal to 82.3%, and not only clay anti-dilative is washed with anti-
Rate is good, and anti-calcium sulfate scale and calcium carbonate scale performance are also excellent, to the bactericidal properties of sulfate reducing bacteria (SRB) and saprophytic bacteria (TGB)
The index request in standard can be reached.
Embodiment 5：A, B raw material will be made by oneself, the clay expansion-resisting agent with sterilization and anti-scaling action is made with C, D, E and F compounding
G, wherein each material quality ratio is：A:B:C:D:E:F=25%:5%:30%:0%:25%:15%.
G is dissolved separately in tap water, it is respectively the molten of 0.3wt%, 0.5wt%, 0.8wt%, 1.0wt% to be made into mass concentration
Liquid, under room temperature (25 DEG C), anti-dilative under various concentration anti-wash rate, anti-scaling property and bactericidal property and is：
1）Concentration is respectively that the anti-dilative of 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% are：85.1%, 88.8%, 92% and
95.1%, the anti-rate of washing is：81.5%, 84.7%, 87.6% and 90.6%；
2）Concentration is respectively that 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt% are to the antiscaling rate of calcium sulfate：99.3%、99.7%、
99.9% and 99.9%, the antiscaling rate to calcium carbonate is：80.2%, 83.4%, 85.3% and 86.1%；
3）Concentration is respectively 0.3wt%, 0.5wt%, 0.8wt% and 1.0wt%, and sulfate reducing bacteria (SRB) number is after sterilization：15
A/mL, 9.5/mL, 4.5/mL and 1.1/mL；Saprophytic bacteria (TGB) number is：200/mL, 95/mL, 75/mL
With 70/mL；Iron bacteria (FB) number is：40/mL, 20/mL, 15/mL and 7.5/mL.
Compare centrifugal process with tap water in concentration 0.3wt% and measure clay anti-dilative 85.1%, resists and wash rate 81.5%, prevent
Calcium sulfate scale antiscaling rate 99.3%, anti-calcium carbonate scale antiscaling rate 80.2%, iron bacteria (FB) number is 40/mL after sterilization, is reached
Index request in standard.
In concentration 0.5wt% or more, clay anti-dilative is all higher than equal to 88.8%, and the anti-rate of washing is all higher than equal to 84.7%,
Anti- calcium sulfate scale antiscaling rate is all higher than equal to 99.7%, and anti-calcium carbonate scale antiscaling rate is all higher than equal to 83.4%, sulfate after sterilization
Reducing bacteria (SRB) number, which is respectively less than, is equal to 9.5/mL, and saprophytic bacteria (TGB) number, which is respectively less than, is equal to 95/mL, reaches standard
In index request；The mass ratio of D is 0% in the G systems, only homemade A is leaned on to sterilize, but in G concentration 0.5wt% or more
When, the finger in standard is still reached to the bactericidal property of sulfate reducing bacteria (SRB), saprophytic bacteria (TGB) and iron bacteria (FB)
Mark requires.
In concentration 0.8wt% or more, anti-dilative is more than or equal to 92.0%, and anti-rate of washing is more than or equal to 87.6%, anti-calcium sulfate
Dirty antiscaling rate is equal to 99.9%, and anti-calcium carbonate scale antiscaling rate is more than or equal to 85.3%, and not only clay anti-dilative and anti-rate of washing are good, anti-sulphur
Sour calcium scale and calcium carbonate scale performance are also excellent, reach mark to the bactericidal property of sulfate reducing bacteria (SRB) and saprophytic bacteria (TGB)
Index request in standard.
Raw material of the present invention includes homemade cationic surfactant A, self-control phosphino- maleic-acrylic acid copolymerization
The raw material benzyl chloride that object scale preventative B is selected is produced by Shandong Pan Ze Chemical Industry Science Co., Ltd；Trimethylamine is by Nantong 95
Chemical Company produces；Acrylic acid is produced by Dongfang Chemical Plant, Beijing, The East Chemical Plant,Beijing；Ammonium persulfate, sodium hypophosphite, maleic acid
Acid anhydride, ammonium chloride, potassium chloride are that analysis is pure to be produced by Chengdu Ke Long chemical reagents factory；Dodecyl benzyl dimethyl ammonium chloride,
Purity 99% is produced by the Xi'an bio tech ltd Jia Boying；Urea is industrial urea to be had by Shaanxi Shan Hua coal chemical industries group
Limit company produces.
The test evaluation of product of the present invention is carried out according to following national standard：People's Republic of China's oil and gas industry
Standard " SY/T 5971-2016 oil-gas field fracturings are acidified and water filling clay stabilizer method of evaluating performance "；The Chinese people are total
With state's oil and gas industry standard " SY/T 5673-1993 scale inhibitor for oilfield method of evaluating performance "；The People's Republic of China (PRC)
Oil and gas industry standard " SY/T 5329-2012 clastic rock reservoir water water quality index and analysis method ".
Claims (4)
1. the technical scheme is that a kind of water filling preparation of clay expansion-resisting agent with sterilization and anti-scaling action, feature
It is：It will self-control cationic surfactant, self-control phosphino-maleic acid-acrylate copolymer scale preventative, urea, dodecyl two
Methylbenzyl ammonium chloride, ammonium chloride and potassium chloride are by mass percentage： 15%~25%:1%~5%:20%~30%:0%~15%:15%~
25%:The water filling clay expansion-resisting agent with sterilization and anti-scaling action is made in 15% ~ 25% ratio after mixing；
The synthesis step of the self-control cationic surfactant：
1）The trimethylamine 179.1kg of 33wt% mass concentrations is added into the reaction kettle equipped with condensing unit, is warming up to 20-30 DEG C,
It is stirred under 1000 revs/min, for use；
2）The benzyl chloride that 126.6kg contents are 99% or more is added in Agitation Tank, the benzyl chloride is then added drop-wise to step 1）
It is loaded in the reaction kettle of trimethylamine；Stirring is warming up to 50-60 DEG C under 1000 revs/min, reacts 30-60min, obtains reactant；
3) by step 2）In reactant obtained stirred under 1000 revs/min, close condensing unit, be warming up to 95-120 DEG C, etc.
Multiply heat when having a large amount of crystal generations and liquid retrogradation in reactant and release liquid and then cooling, product is put into baking after cooling
Case, dries 6h at 90 DEG C, crushes to be made after cooling and reached the powder of 40 mesh screens to get to solid cation surface activating
Agent；
The synthesis step of the self-control phosphino-maleic acid-acrylate copolymer scale preventative：
4）4kg ammonium persulfates are dissolved in 20kg deionized waters or distilled water water, in room temperature, 1000 revs/min of lower stirring and dissolvings,
Obtain initiator；
5）70kg deionized waters or distilled water are added into reaction kettle, 9kg maleic anhydrides are then added, 1000 turns/
Stirring, after maleic anhydride is completely dissolved, adds the sodium phosphite of 10.0kg, is stirred under 1000 revs/min under point, when
Between 10-15min, rise temperature to 50-55 DEG C, wait for that sodium hypophosphite is completely dissolved, be warming up to 75-80 DEG C, stirred under 1000 revs/min
50-60min is mixed, while 27kg acrylic acid and step 4 is added dropwise）In initiator obtained, 85-95 DEG C to be warming up to, the reaction was continued
2-3h obtains faint yellow viscous solution；
6）By step 5）In the faint yellow viscous solution that is prepared be put into baking oven, dry at 90 DEG C for 24 hours, be ground into after cooling
The powder of 40 mesh screens can be crossed to get the solid anti-scaling agent B of nitrogen yellow.
2. a kind of preparation with sterilization and the water filling clay expansion-resisting agent of anti-scaling action according to claim 1, special
Sign is：In the step 2）In, the benzyl chloride is added drop-wise to step 1）In be loaded with the time used in the reaction kettle of trimethylamine
10-15min。
3. a kind of preparation with sterilization and the water filling clay expansion-resisting agent of anti-scaling action according to claim 1, special
Sign is：In the step 5）In, it controls the acrylic acid and initiator while dripping.
4. a kind of preparation with sterilization and the water filling clay expansion-resisting agent of anti-scaling action according to claim 1, special
Sign is：In the step 5）Or 6）In, the faint yellow viscous solution calculates its mass concentration with the amount of monomer and is
33.8wt%。
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| CN111647394A (en) * | 2020-06-22 | 2020-09-11 | 保定市三拓化工产品有限公司 | Preparation method of small cation shale inhibitor |
| CN111849444A (en) * | 2020-06-24 | 2020-10-30 | 中国石油天然气股份有限公司 | Ultra-low permeability oil reservoir pressure-reducing and injection-increasing system and preparation method thereof |
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